data_carlfrancisite _audit_creation_method SHELXL-2014 _chemical_name_systematic manganese magnesium silicate arsenite arsenate hydrate ; ? ; _chemical_name_common carlfrancisite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As42 H252 Mg61 Mn179 O576 Si40 Zn30' _chemical_formula_weight 27018.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 167 _space_group_name_H-M_alt 'R -3 c :H' _space_group_name_Hall '-R 3 2"c' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 8.2238(2) _cell_length_b 8.2238(2) _cell_length_c 205.113(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 12013.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.735 _exptl_crystal_F_000 12913 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 80 microns _exptl_crystal_size_mid 60 microns _exptl_crystal_size_min 10 microns _exptl_absorpt_coefficient_mu 9.181 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30274 _diffrn_reflns_av_unetI/netI 0.0125 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -287 _diffrn_reflns_limit_l_max 288 _diffrn_reflns_theta_min 2.383 _diffrn_reflns_theta_max 30.028 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 3947 _reflns_number_gt 3837 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+130.6129P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3947 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.3333 0.6667 0.01445(2) 0.01488(12) Uani 1 3 d S T P . . As2 As 0.0000 0.0000 0.03838(2) 0.01293(12) Uani 1 3 d S T P . . As3 As 0.6667 0.3333 0.02398(2) 0.0133(2) Uani 0.812(3) 3 d S T . . . Z1 Mn 0.0000 0.25789(8) 0.2500 0.0186(2) Uani 1.009(4) 2 d S T . . . Z2 Zn 0.4716(6) 0.0861(5) 0.02384(2) 0.0199(13) Uani 0.096(2) 1 d . . . . . M1 Mn 0.68709(6) 0.10960(6) 0.06004(2) 0.01361(16) Uani 0.967(3) 1 d . . P . . M2 Mn 0.21486(7) 0.25881(7) 0.02367(2) 0.01760(17) Uani 0.968(3) 1 d . . P . . M3 Mn 0.64649(8) 0.55508(8) 0.03530(2) 0.01460(18) Uani 0.822(3) 1 d . . P . . M4 Mn 0.0000 0.0000 0.05968(2) 0.0155(4) Uani 0.659(5) 3 d S T . . . M5 Mn 0.10709(6) 0.40024(6) 0.07178(2) 0.01444(12) Uani 1 1 d . . . . . M6 Mn 0.0000 0.0000 0.01029(2) 0.0195(3) Uani 0.898(5) 3 d S T . . . M7 Mn 0.11707(6) 0.41594(6) 0.04879(2) 0.01480(12) Uani 1 1 d . . . . . M8 Mg 0.3333 0.6667 0.03497(2) 0.0148(5) Uani 1.173(10) 3 d S T . . . M9 Mg 0.13869(12) 0.42033(12) 0.00011(2) 0.0133(3) Uani 1.107(6) 1 d . . P . . T1A As 0.6667 0.3333 0.07322(2) 0.0107(4) Uani 0.023(5) 3 d S T P . . T1S Si 0.6667 0.3333 0.07322(2) 0.0107(4) Uani 0.977(5) 3 d S T P . . T2A As 0.6667 0.3333 0.04910(2) 0.0151(4) Uani 0.182(6) 3 d S T P . . T2S Si 0.6667 0.3333 0.04910(2) 0.0151(4) Uani 0.818(6) 3 d S T P . . T3A As 0.3333 0.6667 0.06197(2) 0.0108(4) Uani 0.008(5) 3 d S T P . . T3S Si 0.3333 0.6667 0.06197(2) 0.0108(4) Uani 0.992(5) 3 d S T P . . T4A As 0.0000 0.0000 0.08053(2) 0.0113(3) Uani 0.443(5) 3 d S T P . . T4S Si 0.0000 0.0000 0.08053(2) 0.0113(3) Uani 0.557(5) 3 d S T P . . O1 O 0.3333 0.6667 0.00608(2) 0.0157(7) Uani 1 3 d S T P . . O2 O 0.1357(3) 0.6302(3) 0.06513(2) 0.0138(4) Uani 1 1 d . . . . . O3 O 0.3802(3) 0.4809(3) -0.00480(2) 0.0181(4) Uani 1 1 d . . . . . O4 O 0.4667(3) 0.3072(3) 0.02861(2) 0.0188(4) Uani 1 1 d . . . . . O5 O 0.5176(3) 0.1279(3) 0.07632(2) 0.0148(4) Uani 1 1 d . . . . . O6 O 0.2150(3) 0.0535(3) 0.04126(2) 0.0175(4) Uani 1 1 d . . . . . O7 O 0.1489(3) 0.4350(3) 0.02948(2) 0.0168(4) Uani 1 1 d . . . . . O8 O 0.3955(3) 0.5056(3) 0.04157(2) 0.0192(4) Uani 1 1 d . . . . . O9 O 0.2140(3) 0.0406(3) 0.01800(2) 0.0173(4) Uani 1 1 d . . . . . O10 O 0.6667 0.3333 0.04143(2) 0.0228(8) Uani 1 3 d S T P . . O11 O 0.1837(3) 0.2310(3) 0.05357(2) 0.0152(4) Uani 1 1 d . . . . . O12 O 0.3874(3) 0.5042(3) 0.01706(2) 0.0194(4) Uani 1 1 d . . . . . O13 O 0.6667 0.3333 0.06525(2) 0.0126(6) Uani 1 3 d S T P . . O14 O 0.2361(3) 0.0728(3) 0.06569(2) 0.0148(4) Uani 1 1 d . . . . . O15 O 0.3333 0.6667 0.07806(2) 0.0163(7) Uani 1 3 d S T P . . O16 O 0.2033(3) 0.2537(3) 0.00570(2) 0.0185(4) Uani 1 1 d . . . . . O17 O 0.6382(3) 0.4995(3) 0.05278(2) 0.0135(4) Uani 1 1 d . . . . . O18 O 0.3333 0.6667 0.05398(2) 0.0123(6) Uani 1 3 d S T P . . O19 O 0.1602(3) 0.2078(3) 0.07772(2) 0.0145(4) Uani 1 1 d . . . . . O20 O 0.0000 0.0000 0.03011(2) 0.0163(7) Uani 1 3 d S T P . . LP O 0.6667 0.3333 0.01822(11) 0.048(7) Uiso 0.29(2) 3 d S . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.01227(16) 0.01227(16) 0.0201(3) 0.000 0.000 0.00614(8) As2 0.01027(15) 0.01027(15) 0.0182(2) 0.000 0.000 0.00514(8) As3 0.0115(2) 0.0115(2) 0.0170(3) 0.000 0.000 0.00573(12) Z1 0.0212(4) 0.0139(3) 0.0230(4) -0.00343(12) -0.0069(2) 0.01060(18) Z2 0.0164(19) 0.0158(19) 0.028(2) 0.0005(14) 0.0001(14) 0.0082(15) M1 0.0112(2) 0.0100(2) 0.0201(3) 0.00034(15) -0.00018(16) 0.00568(17) M2 0.0181(3) 0.0142(2) 0.0223(3) -0.00315(17) -0.00341(17) 0.00939(19) M3 0.0117(3) 0.0116(3) 0.0214(3) -0.00146(18) -0.00027(19) 0.0065(2) M4 0.0119(4) 0.0119(4) 0.0226(7) 0.000 0.000 0.0059(2) M5 0.0107(2) 0.0118(2) 0.0210(2) 0.00199(15) 0.00203(15) 0.00582(16) M6 0.0194(4) 0.0194(4) 0.0199(5) 0.000 0.000 0.00968(18) M7 0.0110(2) 0.0112(2) 0.0228(2) 0.00191(15) 0.00005(15) 0.00599(16) M8 0.0128(6) 0.0128(6) 0.0189(8) 0.000 0.000 0.0064(3) M9 0.0086(4) 0.0100(4) 0.0220(5) 0.0006(3) -0.0005(3) 0.0050(3) T1A 0.0084(5) 0.0084(5) 0.0152(7) 0.000 0.000 0.0042(2) T1S 0.0084(5) 0.0084(5) 0.0152(7) 0.000 0.000 0.0042(2) T2A 0.0095(4) 0.0095(4) 0.0263(6) 0.000 0.000 0.0047(2) T2S 0.0095(4) 0.0095(4) 0.0263(6) 0.000 0.000 0.0047(2) T3A 0.0084(5) 0.0084(5) 0.0157(7) 0.000 0.000 0.0042(2) T3S 0.0084(5) 0.0084(5) 0.0157(7) 0.000 0.000 0.0042(2) T4A 0.0085(3) 0.0085(3) 0.0167(4) 0.000 0.000 0.00426(14) T4S 0.0085(3) 0.0085(3) 0.0167(4) 0.000 0.000 0.00426(14) O1 0.0172(11) 0.0172(11) 0.0126(15) 0.000 0.000 0.0086(5) O2 0.0098(8) 0.0135(9) 0.0187(9) 0.0005(7) 0.0000(7) 0.0064(7) O3 0.0143(9) 0.0147(10) 0.0241(11) 0.0000(8) 0.0001(8) 0.0063(8) O4 0.0227(11) 0.0159(10) 0.0206(10) -0.0011(8) -0.0021(8) 0.0118(9) O5 0.0113(9) 0.0093(8) 0.0199(9) 0.0017(7) -0.0023(7) 0.0022(7) O6 0.0110(9) 0.0217(10) 0.0201(10) -0.0006(8) -0.0010(8) 0.0085(8) O7 0.0145(9) 0.0165(10) 0.0213(10) -0.0031(8) -0.0014(8) 0.0092(8) O8 0.0213(10) 0.0129(9) 0.0239(11) -0.0010(8) -0.0052(8) 0.0087(9) O9 0.0180(10) 0.0130(9) 0.0212(10) 0.0007(8) 0.0021(8) 0.0080(8) O10 0.0217(12) 0.0217(12) 0.025(2) 0.000 0.000 0.0108(6) O11 0.0140(9) 0.0124(9) 0.0207(10) -0.0005(7) -0.0023(7) 0.0077(8) O12 0.0192(10) 0.0165(10) 0.0252(11) 0.0016(8) -0.0005(8) 0.0109(9) O13 0.0120(9) 0.0120(9) 0.0136(15) 0.000 0.000 0.0060(5) O14 0.0126(9) 0.0126(9) 0.0197(9) 0.0017(7) 0.0007(7) 0.0067(8) O15 0.0169(11) 0.0169(11) 0.0151(16) 0.000 0.000 0.0084(5) O16 0.0168(10) 0.0147(9) 0.0227(11) 0.0004(8) 0.0000(8) 0.0070(8) O17 0.0136(9) 0.0097(8) 0.0189(9) 0.0011(7) 0.0006(7) 0.0071(7) O18 0.0122(9) 0.0122(9) 0.0125(15) 0.000 0.000 0.0061(5) O19 0.0118(9) 0.0113(9) 0.0190(9) 0.0013(7) -0.0010(7) 0.0049(7) O20 0.0181(11) 0.0181(11) 0.0127(15) 0.000 0.000 0.0090(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O12 1.692(2) . ? As1 O12 1.692(2) 3_565 ? As1 O12 1.692(2) 2_665 ? As1 O1 1.716(4) . ? As2 O20 1.697(4) . ? As2 O6 1.700(2) . ? As2 O6 1.700(2) 3 ? As2 O6 1.700(2) 2 ? As3 LP 1.18(2) . ? As3 O4 1.817(2) 2_655 ? As3 O4 1.817(2) . ? As3 O4 1.817(2) 3_665 ? As3 Z2 1.857(4) 2_655 ? As3 Z2 1.857(4) . ? As3 Z2 1.857(4) 3_665 ? As3 M3 3.0080(8) 2_655 ? As3 M3 3.0080(8) 3_665 ? As3 M3 3.0083(8) . ? Z1 O5 2.070(2) 25 ? Z1 O5 2.070(2) 36_445 ? Z1 O19 2.112(2) 34 ? Z1 O19 2.112(2) 26_455 ? Z1 T1S 2.9660(10) 34 ? Z1 T1A 2.9660(10) 34 ? Z1 T1S 2.9660(10) 25 ? Z1 T1A 2.9660(10) 25 ? Z2 O4 1.879(5) 2_655 ? Z2 O4 2.083(4) . ? Z2 O7 2.109(5) 3 ? Z2 LP 2.185(13) . ? Z2 O12 2.256(5) 2_655 ? Z2 O9 2.296(5) . ? Z2 M3 2.363(4) 2_655 ? Z2 M2 2.904(4) 2_655 ? Z2 M2 3.078(4) . ? Z2 M2 3.129(4) 3 ? M1 O2 2.115(2) 3 ? M1 O14 2.137(2) 2_655 ? M1 O11 2.178(2) 2_655 ? M1 O13 2.2064(18) . ? M1 O17 2.235(2) 2_655 ? M1 O17 2.366(2) 3_665 ? M1 T2A 2.9593(11) . ? M1 M4 3.1240(5) 1_655 ? M2 O9 2.136(2) . ? M2 O7 2.145(2) . ? M2 O4 2.156(2) . ? M2 O9 2.188(2) 2 ? M2 O12 2.251(2) . ? M2 O20 2.373(2) . ? M2 Z2 2.904(4) 3_665 ? M2 Z2 3.129(4) 2 ? M3 O7 2.111(2) 2_665 ? M3 O6 2.139(2) 3_665 ? M3 O4 2.179(2) 3_665 ? M3 O4 2.283(2) . ? M3 O10 2.288(2) . ? M3 O8 2.289(2) . ? M3 Z2 2.363(4) 3_665 ? M3 M8 3.1373(5) . ? M3 M7 3.1584(8) 2_665 ? M4 O14 2.118(2) . ? M4 O14 2.118(2) 2 ? M4 O14 2.118(2) 3 ? M4 O11 2.142(2) 2 ? M4 O11 2.142(2) 3 ? M4 O11 2.143(2) . ? M4 M1 3.1239(5) 3_665 ? M4 M1 3.1239(5) 2_545 ? M4 M1 3.1239(5) 1_455 ? M5 O5 2.108(2) 2 ? M5 O14 2.160(2) 2 ? M5 O19 2.207(2) . ? M5 O2 2.246(2) . ? M5 O2 2.325(2) 2_665 ? M5 O15 2.418(2) . ? M5 T3A 2.8697(10) . ? M6 O16 2.133(2) 2 ? M6 O16 2.133(2) 3 ? M6 O16 2.133(2) . ? M6 O9 2.262(2) 3 ? M6 O9 2.262(2) 2 ? M6 O9 2.263(2) . ? M7 O17 2.087(2) 3_565 ? M7 O11 2.100(2) . ? M7 O8 2.166(2) 3_565 ? M7 O18 2.2092(18) . ? M7 O6 2.408(2) 2 ? M7 O8 2.508(2) . ? M7 M3 3.1591(8) 3_565 ? M7 M8 3.4333(14) . ? M8 O7 2.075(2) . ? M8 O7 2.075(2) 3_565 ? M8 O7 2.075(2) 2_665 ? M8 O8 2.128(2) 3_565 ? M8 O8 2.128(2) 2_665 ? M8 O8 2.128(2) . ? M8 M3 3.1372(5) 2_665 ? M8 M3 3.1373(5) 3_565 ? M8 M7 3.4330(14) 3_565 ? M8 M7 3.4330(14) 2_665 ? M9 O16 2.050(2) . ? M9 O3 2.054(2) . ? M9 O16 2.061(2) 21 ? M9 O3 2.065(2) 21 ? M9 O3 2.078(2) 3_565 ? M9 O1 2.219(2) . ? M9 M9 3.0511(9) 21 ? M9 M9 3.0511(9) 20 ? M9 M9 3.1483(17) 19_565 ? M9 M9 3.2048(15) 3_565 ? M9 M9 3.2048(15) 2_665 ? T1A O13 1.635(4) . ? T1A O5 1.640(2) . ? T1A O5 1.640(2) 2_655 ? T1A O5 1.640(2) 3_665 ? T1A Z1 2.9664(10) 25 ? T1A Z1 2.9664(10) 26 ? T1A Z1 2.9665(10) 27 ? T2A O10 1.572(5) . ? T2A O17 1.677(2) . ? T2A O17 1.677(2) 3_665 ? T2A O17 1.677(2) 2_655 ? T2A M1 2.9592(11) 2_655 ? T2A M1 2.9592(11) 3_665 ? T3A O2 1.633(2) 3_565 ? T3A O2 1.633(2) 2_665 ? T3A O2 1.633(2) . ? T3A O18 1.638(4) . ? T3A M5 2.8697(11) 3_565 ? T3A M5 2.8697(11) 2_665 ? T4A O19 1.654(2) 2 ? T4A O19 1.654(2) 3 ? T4A O19 1.655(2) . ? T4A O15 1.657(4) 16_444 ? O1 M9 2.219(2) 3_565 ? O1 M9 2.219(2) 2_665 ? O2 M1 2.116(2) 2 ? O2 M5 2.325(2) 3_565 ? O3 M9 2.065(2) 20 ? O3 M9 2.077(2) 2_665 ? O4 Z2 1.879(5) 3_665 ? O4 M3 2.179(2) 2_655 ? O5 Z1 2.070(2) 25 ? O5 M5 2.108(2) 3 ? O6 M3 2.139(2) 2_655 ? O6 M7 2.408(2) 3 ? O7 Z2 2.110(5) 2 ? O7 M3 2.111(2) 3_565 ? O8 M7 2.165(2) 2_665 ? O9 M2 2.188(2) 3 ? O10 M3 2.288(2) 2_655 ? O10 M3 2.288(2) 3_665 ? O11 M1 2.178(2) 3_665 ? O12 Z2 2.257(5) 3_665 ? O13 M1 2.2065(18) 2_655 ? O13 M1 2.2065(18) 3_665 ? O14 M1 2.137(2) 3_665 ? O14 M5 2.160(2) 3 ? O15 T4S 1.657(4) 16_554 ? O15 T4A 1.657(4) 16_554 ? O15 M5 2.418(2) 3_565 ? O15 M5 2.418(2) 2_665 ? O16 M9 2.061(2) 20 ? O17 M7 2.087(2) 2_665 ? O17 M1 2.235(2) 3_665 ? O17 M1 2.366(2) 2_655 ? O18 M7 2.2093(18) 3_565 ? O18 M7 2.2094(18) 2_665 ? O19 Z1 2.112(2) 27 ? O20 M2 2.373(2) 2 ? O20 M2 2.373(2) 3 ? LP Z2 2.185(13) 2_655 ? LP Z2 2.185(13) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 As1 O12 110.47(8) . 3_565 ? O12 As1 O12 110.47(8) . 2_665 ? O12 As1 O12 110.47(8) 3_565 2_665 ? O12 As1 O1 108.44(8) . . ? O12 As1 O1 108.46(8) 3_565 . ? O12 As1 O1 108.46(8) 2_665 . ? O20 As2 O6 110.32(8) . . ? O20 As2 O6 110.34(8) . 3 ? O6 As2 O6 108.60(8) . 3 ? O20 As2 O6 110.34(8) . 2 ? O6 As2 O6 108.60(8) . 2 ? O6 As2 O6 108.59(8) 3 2 ? LP As3 O4 121.52(7) . 2_655 ? LP As3 O4 121.52(7) . . ? O4 As3 O4 95.17(10) 2_655 . ? LP As3 O4 121.52(8) . 3_665 ? O4 As3 O4 95.17(10) 2_655 3_665 ? O4 As3 O4 95.17(10) . 3_665 ? LP As3 Z2 89.13(14) . 2_655 ? O4 As3 Z2 69.09(14) 2_655 2_655 ? O4 As3 Z2 149.04(16) . 2_655 ? O4 As3 Z2 61.53(14) 3_665 2_655 ? LP As3 Z2 89.13(14) . . ? O4 As3 Z2 61.53(14) 2_655 . ? O4 As3 Z2 69.08(14) . . ? O4 As3 Z2 149.04(16) 3_665 . ? Z2 As3 Z2 119.978(9) 2_655 . ? LP As3 Z2 89.13(14) . 3_665 ? O4 As3 Z2 149.04(16) 2_655 3_665 ? O4 As3 Z2 61.53(14) . 3_665 ? O4 As3 Z2 69.09(14) 3_665 3_665 ? Z2 As3 Z2 119.977(10) 2_655 3_665 ? Z2 As3 Z2 119.977(9) . 3_665 ? LP As3 M3 140.534(14) . 2_655 ? O4 As3 M3 49.23(7) 2_655 2_655 ? O4 As3 M3 45.94(7) . 2_655 ? O4 As3 M3 97.92(8) 3_665 2_655 ? Z2 As3 M3 113.35(13) 2_655 2_655 ? Z2 As3 M3 51.77(13) . 2_655 ? Z2 As3 M3 104.93(13) 3_665 2_655 ? LP As3 M3 140.533(13) . 3_665 ? O4 As3 M3 45.94(7) 2_655 3_665 ? O4 As3 M3 97.92(8) . 3_665 ? O4 As3 M3 49.23(7) 3_665 3_665 ? Z2 As3 M3 51.78(13) 2_655 3_665 ? Z2 As3 M3 104.93(13) . 3_665 ? Z2 As3 M3 113.35(13) 3_665 3_665 ? M3 As3 M3 66.80(2) 2_655 3_665 ? LP As3 M3 140.539(13) . . ? O4 As3 M3 97.91(8) 2_655 . ? O4 As3 M3 49.23(7) . . ? O4 As3 M3 45.94(7) 3_665 . ? Z2 As3 M3 104.93(13) 2_655 . ? Z2 As3 M3 113.34(13) . . ? Z2 As3 M3 51.78(13) 3_665 . ? M3 As3 M3 66.79(2) 2_655 . ? M3 As3 M3 66.79(2) 3_665 . ? O5 Z1 O5 119.42(12) 25 36_445 ? O5 Z1 O19 121.79(8) 25 34 ? O5 Z1 O19 101.71(8) 36_445 34 ? O5 Z1 O19 101.71(8) 25 26_455 ? O5 Z1 O19 121.79(8) 36_445 26_455 ? O19 Z1 O19 87.31(12) 34 26_455 ? O5 Z1 T1S 97.19(7) 25 34 ? O5 Z1 T1S 32.18(6) 36_445 34 ? O19 Z1 T1S 97.82(6) 34 34 ? O19 Z1 T1S 153.97(6) 26_455 34 ? O5 Z1 T1A 97.19(7) 25 34 ? O5 Z1 T1A 32.18(6) 36_445 34 ? O19 Z1 T1A 97.82(6) 34 34 ? O19 Z1 T1A 153.97(6) 26_455 34 ? T1S Z1 T1A 0.00(4) 34 34 ? O5 Z1 T1S 32.18(6) 25 25 ? O5 Z1 T1S 97.19(7) 36_445 25 ? O19 Z1 T1S 153.97(6) 34 25 ? O19 Z1 T1S 97.82(6) 26_455 25 ? T1S Z1 T1S 88.71(4) 34 25 ? T1A Z1 T1S 88.71(4) 34 25 ? O5 Z1 T1A 32.18(6) 25 25 ? O5 Z1 T1A 97.19(7) 36_445 25 ? O19 Z1 T1A 153.97(6) 34 25 ? O19 Z1 T1A 97.82(6) 26_455 25 ? T1S Z1 T1A 88.71(4) 34 25 ? T1A Z1 T1A 88.71(4) 34 25 ? T1S Z1 T1A 0.00(4) 25 25 ? As3 Z2 O4 58.18(14) . 2_655 ? As3 Z2 O4 54.55(13) . . ? O4 Z2 O4 85.0(2) 2_655 . ? As3 Z2 O7 145.9(2) . 3 ? O4 Z2 O7 98.6(2) 2_655 3 ? O4 Z2 O7 102.8(2) . 3 ? As3 Z2 LP 32.7(5) . . ? O4 Z2 LP 80.4(4) 2_655 . ? O4 Z2 LP 76.2(4) . . ? O7 Z2 LP 178.6(6) 3 . ? As3 Z2 O12 118.2(2) . 2_655 ? O4 Z2 O12 97.43(19) 2_655 2_655 ? O4 Z2 O12 169.2(2) . 2_655 ? O7 Z2 O12 87.21(16) 3 2_655 ? LP Z2 O12 93.9(4) . 2_655 ? As3 Z2 O9 114.07(19) . . ? O4 Z2 O9 171.9(2) 2_655 . ? O4 Z2 O9 88.16(16) . . ? O7 Z2 O9 87.21(16) 3 . ? LP Z2 O9 93.7(4) . . ? O12 Z2 O9 88.46(17) 2_655 . ? As3 Z2 M3 90.11(17) . 2_655 ? O4 Z2 M3 63.93(15) 2_655 2_655 ? O4 Z2 M3 58.29(13) . 2_655 ? O7 Z2 M3 55.98(12) 3 2_655 ? LP Z2 M3 122.6(5) . 2_655 ? O12 Z2 M3 132.10(19) 2_655 2_655 ? O9 Z2 M3 115.81(18) . 2_655 ? As3 Z2 M2 90.16(15) . 2_655 ? O4 Z2 M2 47.91(11) 2_655 2_655 ? O4 Z2 M2 132.76(19) . 2_655 ? O7 Z2 M2 90.27(14) 3 2_655 ? LP Z2 M2 89.76(13) . 2_655 ? O12 Z2 M2 49.80(10) 2_655 2_655 ? O9 Z2 M2 138.26(18) . 2_655 ? M3 Z2 M2 96.53(13) 2_655 2_655 ? As3 Z2 M2 84.90(13) . . ? O4 Z2 M2 129.41(19) 2_655 . ? O4 Z2 M2 44.37(10) . . ? O7 Z2 M2 94.60(15) 3 . ? LP Z2 M2 85.32(12) . . ? O12 Z2 M2 131.96(18) 2_655 . ? O9 Z2 M2 43.89(9) . . ? M3 Z2 M2 84.91(12) 2_655 . ? M2 Z2 M2 174.86(16) 2_655 . ? As3 Z2 M2 151.69(19) . 3 ? O4 Z2 M2 141.7(2) 2_655 3 ? O4 Z2 M2 101.01(16) . 3 ? O7 Z2 M2 43.08(9) 3 3 ? LP Z2 M2 137.9(4) . 3 ? O12 Z2 M2 83.57(13) 2_655 3 ? O9 Z2 M2 44.34(9) . 3 ? M3 Z2 M2 87.00(12) 2_655 3 ? M2 Z2 M2 118.15(13) 2_655 3 ? M2 Z2 M2 66.79(8) . 3 ? O2 M1 O14 95.89(8) 3 2_655 ? O2 M1 O11 92.40(8) 3 2_655 ? O14 M1 O11 85.70(8) 2_655 2_655 ? O2 M1 O13 102.86(8) 3 . ? O14 M1 O13 90.71(8) 2_655 . ? O11 M1 O13 164.61(8) 2_655 . ? O2 M1 O17 101.80(8) 3 2_655 ? O14 M1 O17 162.22(8) 2_655 2_655 ? O11 M1 O17 95.19(8) 2_655 2_655 ? O13 M1 O17 83.74(9) . 2_655 ? O2 M1 O17 169.47(8) 3 3_665 ? O14 M1 O17 93.93(8) 2_655 3_665 ? O11 M1 O17 84.57(8) 2_655 3_665 ? O13 M1 O17 80.75(9) . 3_665 ? O17 M1 O17 68.54(10) 2_655 3_665 ? O2 M1 T2A 136.00(6) 3 . ? O14 M1 T2A 128.09(6) 2_655 . ? O11 M1 T2A 92.14(6) 2_655 . ? O13 M1 T2A 78.33(8) . . ? O17 M1 T2A 34.20(5) 2_655 . ? O17 M1 T2A 34.48(5) 3_665 . ? O2 M1 M4 93.93(6) 3 1_655 ? O14 M1 M4 42.52(6) 2_655 1_655 ? O11 M1 M4 43.23(6) 2_655 1_655 ? O13 M1 M4 132.00(4) . 1_655 ? O17 M1 M4 136.39(6) 2_655 1_655 ? O17 M1 M4 90.75(5) 3_665 1_655 ? T2A M1 M4 118.20(3) . 1_655 ? O9 M2 O7 167.07(9) . . ? O9 M2 O4 90.60(9) . . ? O7 M2 O4 99.12(9) . . ? O9 M2 O9 80.84(12) . 2 ? O7 M2 O9 89.20(9) . 2 ? O4 M2 O9 171.38(9) . 2 ? O9 M2 O12 99.24(9) . . ? O7 M2 O12 89.33(9) . . ? O4 M2 O12 90.05(9) . . ? O9 M2 O12 92.34(8) 2 . ? O9 M2 O20 82.02(8) . . ? O7 M2 O20 88.32(8) . . ? O4 M2 O20 96.91(8) . . ? O9 M2 O20 80.97(8) 2 . ? O12 M2 O20 172.93(8) . . ? O9 M2 Z2 100.09(10) . 3_665 ? O7 M2 Z2 92.84(10) . 3_665 ? O4 M2 Z2 40.31(10) . 3_665 ? O9 M2 Z2 142.19(10) 2 3_665 ? O12 M2 Z2 49.98(10) . 3_665 ? O20 M2 Z2 136.81(10) . 3_665 ? O9 M2 Z2 48.19(10) . . ? O7 M2 Z2 140.27(10) . . ? O4 M2 Z2 42.50(10) . . ? O9 M2 Z2 128.88(10) 2 . ? O12 M2 Z2 98.64(10) . . ? O20 M2 Z2 87.40(8) . . ? Z2 M2 Z2 64.96(15) 3_665 . ? O9 M2 Z2 127.94(10) . 2 ? O7 M2 Z2 42.23(10) . 2 ? O4 M2 Z2 141.26(10) . 2 ? O9 M2 Z2 47.19(10) 2 2 ? O12 M2 Z2 87.54(9) . 2 ? O20 M2 Z2 86.24(8) . 2 ? Z2 M2 Z2 121.82(13) 3_665 2 ? Z2 M2 Z2 173.09(9) . 2 ? O7 M3 O6 95.66(9) 2_665 3_665 ? O7 M3 O4 99.58(9) 2_665 3_665 ? O6 M3 O4 100.67(9) 3_665 3_665 ? O7 M3 O4 87.01(8) 2_665 . ? O6 M3 O4 174.28(9) 3_665 . ? O4 M3 O4 73.85(13) 3_665 . ? O7 M3 O10 167.37(7) 2_665 . ? O6 M3 O10 94.31(9) 3_665 . ? O4 M3 O10 86.15(10) 3_665 . ? O4 M3 O10 83.78(9) . . ? O7 M3 O8 83.73(8) 2_665 . ? O6 M3 O8 92.16(9) 3_665 . ? O4 M3 O8 166.31(9) 3_665 . ? O4 M3 O8 93.16(9) . . ? O10 M3 O8 88.16(9) . . ? O7 M3 Z2 55.91(11) 2_665 3_665 ? O6 M3 Z2 130.45(12) 3_665 3_665 ? O4 M3 Z2 54.40(11) 3_665 3_665 ? O4 M3 Z2 47.67(11) . 3_665 ? O10 M3 Z2 121.44(13) . 3_665 ? O8 M3 Z2 119.58(11) . 3_665 ? O7 M3 As3 93.96(6) 2_665 . ? O6 M3 As3 137.46(7) 3_665 . ? O4 M3 As3 36.80(7) 3_665 . ? O4 M3 As3 37.05(6) . . ? O10 M3 As3 83.86(9) . . ? O8 M3 As3 130.10(6) . . ? Z2 M3 As3 38.11(10) 3_665 . ? O7 M3 M8 41.03(6) 2_665 . ? O6 M3 M8 96.03(7) 3_665 . ? O4 M3 M8 138.77(7) 3_665 . ? O4 M3 M8 89.31(6) . . ? O10 M3 M8 129.97(6) . . ? O8 M3 M8 42.71(6) . . ? Z2 M3 M8 86.31(10) 3_665 . ? As3 M3 M8 117.55(3) . . ? O7 M3 M7 95.63(6) 2_665 2_665 ? O6 M3 M7 49.61(6) 3_665 2_665 ? O4 M3 M7 147.99(7) 3_665 2_665 ? O4 M3 M7 135.26(6) . 2_665 ? O10 M3 M7 84.96(9) . 2_665 ? O8 M3 M7 43.28(6) . 2_665 ? Z2 M3 M7 151.01(10) 3_665 2_665 ? As3 M3 M7 167.28(2) . 2_665 ? M8 M3 M7 66.09(3) . 2_665 ? O14 M4 O14 89.52(9) . 2 ? O14 M4 O14 89.52(9) . 3 ? O14 M4 O14 89.52(9) 2 3 ? O14 M4 O11 174.82(8) . 2 ? O14 M4 O11 87.08(8) 2 2 ? O14 M4 O11 94.36(8) 3 2 ? O14 M4 O11 94.36(8) . 3 ? O14 M4 O11 174.82(8) 2 3 ? O14 M4 O11 87.08(8) 3 3 ? O11 M4 O11 89.28(9) 2 3 ? O14 M4 O11 87.09(8) . . ? O14 M4 O11 94.36(8) 2 . ? O14 M4 O11 174.82(8) 3 . ? O11 M4 O11 89.27(9) 2 . ? O11 M4 O11 89.27(9) 3 . ? O14 M4 M1 43.00(6) . 3_665 ? O14 M4 M1 90.85(6) 2 3_665 ? O14 M4 M1 132.50(7) 3 3_665 ? O11 M4 M1 133.10(7) 2 3_665 ? O11 M4 M1 94.33(6) 3 3_665 ? O11 M4 M1 44.15(6) . 3_665 ? O14 M4 M1 90.85(6) . 2_545 ? O14 M4 M1 132.50(7) 2 2_545 ? O14 M4 M1 43.00(6) 3 2_545 ? O11 M4 M1 94.33(6) 2 2_545 ? O11 M4 M1 44.14(6) 3 2_545 ? O11 M4 M1 133.09(7) . 2_545 ? M1 M4 M1 119.946(3) 3_665 2_545 ? O14 M4 M1 132.50(7) . 1_455 ? O14 M4 M1 43.00(6) 2 1_455 ? O14 M4 M1 90.85(6) 3 1_455 ? O11 M4 M1 44.14(6) 2 1_455 ? O11 M4 M1 133.10(7) 3 1_455 ? O11 M4 M1 94.33(6) . 1_455 ? M1 M4 M1 119.945(3) 3_665 1_455 ? M1 M4 M1 119.945(3) 2_545 1_455 ? O5 M5 O14 91.06(8) 2 2 ? O5 M5 O19 103.44(8) 2 . ? O14 M5 O19 87.94(8) 2 . ? O5 M5 O2 90.62(8) 2 . ? O14 M5 O2 98.34(8) 2 . ? O19 M5 O2 164.54(8) . . ? O5 M5 O2 159.51(8) 2 2_665 ? O14 M5 O2 94.98(8) 2 2_665 ? O19 M5 O2 96.34(8) . 2_665 ? O2 M5 O2 69.16(10) . 2_665 ? O5 M5 O15 94.34(7) 2 . ? O14 M5 O15 174.60(8) 2 . ? O19 M5 O15 90.98(8) . . ? O2 M5 O15 81.44(8) . . ? O2 M5 O15 79.87(8) 2_665 . ? O5 M5 T3A 124.92(6) 2 . ? O14 M5 T3A 100.00(6) 2 . ? O19 M5 T3A 130.50(6) . . ? O2 M5 T3A 34.58(5) . . ? O2 M5 T3A 34.67(5) 2_665 . ? O15 M5 T3A 76.73(8) . . ? O16 M6 O16 101.96(8) 2 3 ? O16 M6 O16 101.96(8) 2 . ? O16 M6 O16 101.96(8) 3 . ? O16 M6 O9 89.00(8) 2 3 ? O16 M6 O9 89.59(8) 3 3 ? O16 M6 O9 161.90(9) . 3 ? O16 M6 O9 89.59(8) 2 2 ? O16 M6 O9 161.90(9) 3 2 ? O16 M6 O9 89.00(8) . 2 ? O9 M6 O9 76.58(9) 3 2 ? O16 M6 O9 161.89(9) 2 . ? O16 M6 O9 89.01(8) 3 . ? O16 M6 O9 89.60(8) . . ? O9 M6 O9 76.57(9) 3 . ? O9 M6 O9 76.57(9) 2 . ? O17 M7 O11 105.24(9) 3_565 . ? O17 M7 O8 92.07(8) 3_565 3_565 ? O11 M7 O8 161.42(9) . 3_565 ? O17 M7 O18 105.40(8) 3_565 . ? O11 M7 O18 94.09(8) . . ? O8 M7 O18 87.61(9) 3_565 . ? O17 M7 O6 88.80(8) 3_565 2 ? O11 M7 O6 85.39(8) . 2 ? O8 M7 O6 88.34(9) 3_565 2 ? O18 M7 O6 165.36(9) . 2 ? O17 M7 O8 165.63(8) 3_565 . ? O11 M7 O8 87.59(8) . . ? O8 M7 O8 74.51(11) 3_565 . ? O18 M7 O8 79.60(8) . . ? O6 M7 O8 85.76(8) 2 . ? O17 M7 M3 84.34(6) 3_565 3_565 ? O11 M7 M3 127.46(6) . 3_565 ? O8 M7 M3 46.44(7) 3_565 3_565 ? O18 M7 M3 133.78(7) . 3_565 ? O6 M7 M3 42.58(5) 2 3_565 ? O8 M7 M3 82.65(5) . 3_565 ? O17 M7 M8 128.02(6) 3_565 . ? O11 M7 M8 125.18(6) . . ? O8 M7 M8 36.52(6) 3_565 . ? O18 M7 M8 84.48(8) . . ? O6 M7 M8 83.90(6) 2 . ? O8 M7 M8 38.12(5) . . ? M3 M7 M8 56.651(19) 3_565 . ? O7 M8 O7 93.38(10) . 3_565 ? O7 M8 O7 93.38(10) . 2_665 ? O7 M8 O7 93.37(10) 3_565 2_665 ? O7 M8 O8 88.73(9) . 3_565 ? O7 M8 O8 93.82(9) 3_565 3_565 ? O7 M8 O8 172.38(11) 2_665 3_565 ? O7 M8 O8 172.36(11) . 2_665 ? O7 M8 O8 88.74(9) 3_565 2_665 ? O7 M8 O8 93.82(9) 2_665 2_665 ? O8 M8 O8 83.81(11) 3_565 2_665 ? O7 M8 O8 93.81(9) . . ? O7 M8 O8 172.37(11) 3_565 . ? O7 M8 O8 88.74(9) 2_665 . ? O8 M8 O8 83.80(11) 3_565 . ? O8 M8 O8 83.80(11) 2_665 . ? O7 M8 M3 134.96(7) . 2_665 ? O7 M8 M3 41.89(6) 3_565 2_665 ? O7 M8 M3 94.21(6) 2_665 2_665 ? O8 M8 M3 89.46(7) 3_565 2_665 ? O8 M8 M3 46.86(7) 2_665 2_665 ? O8 M8 M3 130.66(8) . 2_665 ? O7 M8 M3 41.88(6) . 3_565 ? O7 M8 M3 94.21(6) 3_565 3_565 ? O7 M8 M3 134.95(8) 2_665 3_565 ? O8 M8 M3 46.86(7) 3_565 3_565 ? O8 M8 M3 130.67(8) 2_665 3_565 ? O8 M8 M3 89.46(7) . 3_565 ? M3 M8 M3 119.954(3) 2_665 3_565 ? O7 M8 M3 94.21(6) . . ? O7 M8 M3 134.96(8) 3_565 . ? O7 M8 M3 41.90(6) 2_665 . ? O8 M8 M3 130.66(8) 3_565 . ? O8 M8 M3 89.45(7) 2_665 . ? O8 M8 M3 46.86(7) . . ? M3 M8 M3 119.952(3) 2_665 . ? M3 M8 M3 119.952(3) 3_565 . ? O7 M8 M7 135.36(7) . 3_565 ? O7 M8 M7 88.58(7) 3_565 3_565 ? O7 M8 M7 131.06(7) 2_665 3_565 ? O8 M8 M7 46.68(7) 3_565 3_565 ? O8 M8 M7 37.28(7) 2_665 3_565 ? O8 M8 M7 84.52(8) . 3_565 ? M3 M8 M7 57.26(2) 2_665 3_565 ? M3 M8 M7 93.49(3) 3_565 3_565 ? M3 M8 M7 115.21(4) . 3_565 ? O7 M8 M7 131.05(7) . 2_665 ? O7 M8 M7 135.37(7) 3_565 2_665 ? O7 M8 M7 88.58(7) 2_665 2_665 ? O8 M8 M7 84.52(8) 3_565 2_665 ? O8 M8 M7 46.68(7) 2_665 2_665 ? O8 M8 M7 37.28(7) . 2_665 ? M3 M8 M7 93.49(3) 2_665 2_665 ? M3 M8 M7 115.22(4) 3_565 2_665 ? M3 M8 M7 57.25(2) . 2_665 ? M7 M8 M7 58.46(3) 3_565 2_665 ? O7 M8 M7 88.57(7) . . ? O7 M8 M7 131.06(7) 3_565 . ? O7 M8 M7 135.37(7) 2_665 . ? O8 M8 M7 37.28(7) 3_565 . ? O8 M8 M7 84.52(8) 2_665 . ? O8 M8 M7 46.68(7) . . ? M3 M8 M7 115.21(4) 2_665 . ? M3 M8 M7 57.26(2) 3_565 . ? M3 M8 M7 93.48(3) . . ? M7 M8 M7 58.46(3) 3_565 . ? M7 M8 M7 58.46(3) 2_665 . ? O16 M9 O3 83.93(10) . . ? O16 M9 O16 94.60(13) . 21 ? O3 M9 O16 98.40(10) . 21 ? O16 M9 O3 100.21(10) . 21 ? O3 M9 O3 175.38(11) . 21 ? O16 M9 O3 83.39(9) 21 21 ? O16 M9 O3 172.13(10) . 3_565 ? O3 M9 O3 94.54(13) . 3_565 ? O16 M9 O3 93.27(10) 21 3_565 ? O3 M9 O3 81.08(10) 21 3_565 ? O16 M9 O1 89.52(9) . . ? O3 M9 O1 83.14(9) . . ? O16 M9 O1 175.73(9) 21 . ? O3 M9 O1 94.78(9) 21 . ? O3 M9 O1 82.62(9) 3_565 . ? O16 M9 M9 94.28(7) . 21 ? O3 M9 M9 140.19(8) . 21 ? O16 M9 M9 41.95(7) 21 21 ? O3 M9 M9 42.07(7) 21 21 ? O3 M9 M9 91.83(7) 3_565 21 ? O1 M9 M9 136.67(7) . 21 ? O16 M9 M9 42.22(7) . 20 ? O3 M9 M9 42.34(7) . 20 ? O16 M9 M9 93.05(7) 21 20 ? O3 M9 M9 142.04(8) 21 20 ? O3 M9 M9 136.88(8) 3_565 20 ? O1 M9 M9 90.76(4) . 20 ? M9 M9 M9 119.979(2) 21 20 ? O16 M9 M9 140.35(9) . 19_565 ? O3 M9 M9 134.92(8) . 19_565 ? O16 M9 M9 87.84(7) 21 19_565 ? O3 M9 M9 40.68(7) 21 19_565 ? O3 M9 M9 40.39(7) 3_565 19_565 ? O1 M9 M9 88.27(4) . 19_565 ? M9 M9 M9 62.23(4) 21 19_565 ? M9 M9 M9 177.23(6) 20 19_565 ? O16 M9 M9 133.26(7) . 3_565 ? O3 M9 M9 87.84(7) . 3_565 ? O16 M9 M9 132.13(7) 21 3_565 ? O3 M9 M9 87.82(7) 21 3_565 ? O3 M9 M9 38.87(7) 3_565 3_565 ? O1 M9 M9 43.78(6) . 3_565 ? M9 M9 M9 119.63(4) 21 3_565 ? M9 M9 M9 120.36(4) 20 3_565 ? M9 M9 M9 57.40(4) 19_565 3_565 ? O16 M9 M9 86.49(7) . 2_665 ? O3 M9 M9 39.39(7) . 2_665 ? O16 M9 M9 137.53(7) 21 2_665 ? O3 M9 M9 138.27(7) 21 2_665 ? O3 M9 M9 87.44(6) 3_565 2_665 ? O1 M9 M9 43.78(6) . 2_665 ? M9 M9 M9 179.08(4) 21 2_665 ? M9 M9 M9 60.37(4) 20 2_665 ? M9 M9 M9 117.39(4) 19_565 2_665 ? M9 M9 M9 60.0 3_565 2_665 ? O13 T1A O5 112.81(9) . . ? O13 T1A O5 112.81(9) . 2_655 ? O5 T1A O5 105.94(9) . 2_655 ? O13 T1A O5 112.81(9) . 3_665 ? O5 T1A O5 105.94(9) . 3_665 ? O5 T1A O5 105.94(9) 2_655 3_665 ? O13 T1A Z1 134.36(2) . 25 ? O5 T1A Z1 42.23(8) . 25 ? O5 T1A Z1 64.09(8) 2_655 25 ? O5 T1A Z1 111.36(9) 3_665 25 ? O13 T1A Z1 134.36(2) . 26 ? O5 T1A Z1 111.37(9) . 26 ? O5 T1A Z1 42.23(8) 2_655 26 ? O5 T1A Z1 64.09(8) 3_665 26 ? Z1 T1A Z1 76.51(3) 25 26 ? O13 T1A Z1 134.36(2) . 27 ? O5 T1A Z1 64.09(8) . 27 ? O5 T1A Z1 111.36(9) 2_655 27 ? O5 T1A Z1 42.23(8) 3_665 27 ? Z1 T1A Z1 76.51(3) 25 27 ? Z1 T1A Z1 76.51(3) 26 27 ? O10 T2A O17 116.78(8) . . ? O10 T2A O17 116.78(8) . 3_665 ? O17 T2A O17 101.27(10) . 3_665 ? O10 T2A O17 116.78(8) . 2_655 ? O17 T2A O17 101.27(10) . 2_655 ? O17 T2A O17 101.27(10) 3_665 2_655 ? O10 T2A M1 139.307(19) . 2_655 ? O17 T2A M1 53.00(8) . 2_655 ? O17 T2A M1 48.51(8) 3_665 2_655 ? O17 T2A M1 103.85(9) 2_655 2_655 ? O10 T2A M1 139.307(18) . 3_665 ? O17 T2A M1 48.51(8) . 3_665 ? O17 T2A M1 103.85(9) 3_665 3_665 ? O17 T2A M1 53.00(8) 2_655 3_665 ? M1 T2A M1 68.76(3) 2_655 3_665 ? O10 T2A M1 139.309(18) . . ? O17 T2A M1 103.85(9) . . ? O17 T2A M1 53.00(8) 3_665 . ? O17 T2A M1 48.51(8) 2_655 . ? M1 T2A M1 68.75(3) 2_655 . ? M1 T2A M1 68.75(3) 3_665 . ? O2 T3A O2 105.24(10) 3_565 2_665 ? O2 T3A O2 105.23(10) 3_565 . ? O2 T3A O2 105.23(10) 2_665 . ? O2 T3A O18 113.43(8) 3_565 . ? O2 T3A O18 113.43(8) 2_665 . ? O2 T3A O18 113.44(8) . . ? O2 T3A M5 51.32(8) 3_565 3_565 ? O2 T3A M5 112.02(10) 2_665 3_565 ? O2 T3A M5 54.09(8) . 3_565 ? O18 T3A M5 134.52(2) . 3_565 ? O2 T3A M5 54.10(8) 3_565 2_665 ? O2 T3A M5 51.32(8) 2_665 2_665 ? O2 T3A M5 112.01(10) . 2_665 ? O18 T3A M5 134.52(2) . 2_665 ? M5 T3A M5 76.26(3) 3_565 2_665 ? O2 T3A M5 112.02(10) 3_565 . ? O2 T3A M5 54.10(8) 2_665 . ? O2 T3A M5 51.31(8) . . ? O18 T3A M5 134.53(2) . . ? M5 T3A M5 76.26(3) 3_565 . ? M5 T3A M5 76.26(3) 2_665 . ? O19 T4A O19 108.54(8) 2 3 ? O19 T4A O19 108.53(8) 2 . ? O19 T4A O19 108.53(8) 3 . ? O19 T4A O15 110.39(8) 2 16_444 ? O19 T4A O15 110.39(8) 3 16_444 ? O19 T4A O15 110.40(8) . 16_444 ? As1 O1 M9 123.50(8) . . ? As1 O1 M9 123.51(8) . 3_565 ? M9 O1 M9 92.46(11) . 3_565 ? As1 O1 M9 123.51(8) . 2_665 ? M9 O1 M9 92.46(11) . 2_665 ? M9 O1 M9 92.45(11) 3_565 2_665 ? T3A O2 M1 126.91(12) . 2 ? T3A O2 M5 94.11(10) . . ? M1 O2 M5 116.10(9) 2 . ? T3A O2 M5 91.23(10) . 3_565 ? M1 O2 M5 120.73(9) 2 3_565 ? M5 O2 M5 101.66(8) . 3_565 ? M9 O3 M9 95.59(10) . 20 ? M9 O3 M9 101.75(11) . 2_665 ? M9 O3 M9 98.94(10) 20 2_665 ? As3 O4 Z2 60.29(14) . 3_665 ? As3 O4 Z2 56.37(13) . . ? Z2 O4 Z2 108.4(3) 3_665 . ? As3 O4 M2 120.38(12) . . ? Z2 O4 M2 91.78(15) 3_665 . ? Z2 O4 M2 93.13(14) . . ? As3 O4 M3 97.26(10) . 2_655 ? Z2 O4 M3 150.01(18) 3_665 2_655 ? Z2 O4 M3 67.29(14) . 2_655 ? M2 O4 M3 117.73(11) . 2_655 ? As3 O4 M3 93.72(10) . . ? Z2 O4 M3 68.41(15) 3_665 . ? Z2 O4 M3 140.82(16) . . ? M2 O4 M3 125.51(11) . . ? M3 O4 M3 95.80(9) 2_655 . ? T1A O5 Z1 105.59(11) . 25 ? T1A O5 M5 129.31(13) . 3 ? Z1 O5 M5 117.05(10) 25 3 ? As2 O6 M3 124.64(12) . 2_655 ? As2 O6 M7 129.49(12) . 3 ? M3 O6 M7 87.80(8) 2_655 3 ? M8 O7 Z2 130.76(15) . 2 ? M8 O7 M3 97.10(10) . 3_565 ? Z2 O7 M3 68.10(13) 2 3_565 ? M8 O7 M2 127.29(11) . . ? Z2 O7 M2 94.68(14) 2 . ? M3 O7 M2 127.78(11) 3_565 . ? M8 O8 M7 106.19(10) . 2_665 ? M8 O8 M3 90.43(9) . . ? M7 O8 M3 90.27(9) 2_665 . ? M8 O8 M7 95.21(9) . . ? M7 O8 M7 91.39(9) 2_665 . ? M3 O8 M7 173.43(11) . . ? M2 O9 M2 104.43(10) . 3 ? M2 O9 M6 100.40(9) . . ? M2 O9 M6 98.83(9) 3 . ? M2 O9 Z2 87.92(13) . . ? M2 O9 Z2 88.47(13) 3 . ? M6 O9 Z2 167.12(15) . . ? T2A O10 M3 123.33(9) . . ? T2A O10 M3 123.33(9) . 2_655 ? M3 O10 M3 92.70(13) . 2_655 ? T2A O10 M3 123.33(9) . 3_665 ? M3 O10 M3 92.70(13) . 3_665 ? M3 O10 M3 92.70(13) 2_655 3_665 ? M7 O11 M4 126.25(10) . . ? M7 O11 M1 125.56(10) . 3_665 ? M4 O11 M1 92.60(9) . 3_665 ? As1 O12 M2 127.01(12) . . ? As1 O12 Z2 131.16(16) . 3_665 ? M2 O12 Z2 80.21(13) . 3_665 ? T1A O13 M1 119.02(8) . . ? T1A O13 M1 119.02(8) . 2_655 ? M1 O13 M1 98.45(11) . 2_655 ? T1A O13 M1 119.02(8) . 3_665 ? M1 O13 M1 98.45(11) . 3_665 ? M1 O13 M1 98.45(11) 2_655 3_665 ? M4 O14 M1 94.48(9) . 3_665 ? M4 O14 M5 128.71(10) . 3 ? M1 O14 M5 130.20(10) 3_665 3 ? T4S O15 T4A 0.0 16_554 16_554 ? T4S O15 M5 122.20(8) 16_554 . ? T4A O15 M5 122.20(8) 16_554 . ? T4S O15 M5 122.20(8) 16_554 3_565 ? T4A O15 M5 122.20(8) 16_554 3_565 ? M5 O15 M5 94.25(10) . 3_565 ? T4S O15 M5 122.20(8) 16_554 2_665 ? T4A O15 M5 122.20(8) 16_554 2_665 ? M5 O15 M5 94.25(10) . 2_665 ? M5 O15 M5 94.25(10) 3_565 2_665 ? M9 O16 M9 95.84(10) . 20 ? M9 O16 M6 124.24(11) . . ? M9 O16 M6 125.16(11) 20 . ? T2A O17 M7 130.01(13) . 2_665 ? T2A O17 M1 97.29(10) . 3_665 ? M7 O17 M1 113.26(9) 2_665 3_665 ? T2A O17 M1 92.52(9) . 2_655 ? M7 O17 M1 122.51(10) 2_665 2_655 ? M1 O17 M1 93.13(8) 3_665 2_655 ? T3A O18 M7 118.80(8) . . ? T3A O18 M7 118.81(8) . 3_565 ? M7 O18 M7 98.73(11) . 3_565 ? T3A O18 M7 118.81(8) . 2_665 ? M7 O18 M7 98.73(11) . 2_665 ? M7 O18 M7 98.72(11) 3_565 2_665 ? T4A O19 Z1 113.01(11) . 27 ? T4A O19 M5 126.32(11) . . ? Z1 O19 M5 116.16(9) 27 . ? As2 O20 M2 123.78(8) . 2 ? As2 O20 M2 123.78(8) . . ? M2 O20 M2 92.08(10) 2 . ? As2 O20 M2 123.78(8) . 3 ? M2 O20 M2 92.08(10) 2 3 ? M2 O20 M2 92.08(10) . 3 ? As3 LP Z2 58.2(5) . 2_655 ? As3 LP Z2 58.2(5) . 3_665 ? Z2 LP Z2 94.7(7) 2_655 3_665 ? As3 LP Z2 58.2(5) . . ? Z2 LP Z2 94.7(7) 2_655 . ? Z2 LP Z2 94.7(7) 3_665 . ? _refine_diff_density_max 2.437 _refine_diff_density_min -1.177 _refine_diff_density_rms 0.187 _shelxl_version_number 2014-3 _shelx_res_file ; TITL Carlfrancisite in R-3c CELL 0.71073 8.2238 8.2238 205.113 90.00 90.00 120.00 ZERR 1.00 0.0002 0.0002 0.006 0.00 0.00 0.00 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM Y, X, .5-Z SYMM X-Y, -Y, .5-Z SYMM -X, -X+Y, .5-Z SFAC O H MG SI MN ZN AS UNIT 576 252 61 40 179 30 42 OMIT 0 0 6 OMIT 0 0 -6 OMIT 0 0 12 OMIT 0 0 -12 OMIT 0 0 18 OMIT 0 0 -18 L.S. 10 BOND 1 FMAP 2 PLAN 20 ACTA WGHT 0.056200 130.612900 FVAR 0.02873 0.96652 0.96761 0.82213 1.10666 0.02292 0.18246 FVAR 0.00780 0.44272 AS1 7 0.333333 0.666667 0.014447 10.33333 0.01227 0.01227 = 0.02010 0.00000 0.00000 0.00614 AS2 7 0.000000 0.000000 0.038379 10.33333 0.01027 0.01027 = 0.01824 0.00000 0.00000 0.00514 AS3 7 0.666667 0.333333 0.023980 0.27074 0.01147 0.01147 = 0.01698 0.00000 0.00000 0.00573 Z1 5 0.000000 0.257891 0.250000 0.50443 0.02119 0.01395 = 0.02300 -0.00343 -0.00685 0.01060 Z2 6 0.471581 0.086062 0.023843 0.09595 0.01644 0.01582 = 0.02778 0.00050 0.00011 0.00821 M1 5 0.687090 0.109599 0.060036 21.00000 0.01123 0.01001 = 0.02008 0.00034 -0.00018 0.00568 M2 5 0.214855 0.258813 0.023674 31.00000 0.01811 0.01416 = 0.02228 -0.00315 -0.00341 0.00939 M3 5 0.646492 0.555080 0.035303 41.00000 0.01169 0.01165 = 0.02142 -0.00146 -0.00027 0.00654 M4 5 0.000000 0.000000 0.059679 0.21981 0.01187 0.01187 = 0.02265 0.00000 0.00000 0.00593 M5 5 0.107086 0.400242 0.071778 11.00000 0.01073 0.01179 = 0.02104 0.00199 0.00203 0.00582 M6 5 0.000000 0.000000 0.010293 0.29931 0.01937 0.01937 = 0.01989 0.00000 0.00000 0.00968 M7 5 0.117065 0.415936 0.048793 11.00000 0.01098 0.01123 = 0.02277 0.00191 0.00005 0.00599 M8 3 0.333333 0.666667 0.034968 0.39110 0.01277 0.01277 = 0.01886 0.00000 0.00000 0.00639 M9 3 0.138686 0.420327 0.000109 51.00000 0.00855 0.00995 = 0.02195 0.00056 -0.00046 0.00503 T1A 7 0.666667 0.333333 0.073224 60.33333 0.00844 0.00844 = 0.01519 0.00000 0.00000 0.00422 T1S 4 0.666667 0.333333 0.073224 -60.33333 0.00844 0.00844 = 0.01519 0.00000 0.00000 0.00422 T2A 7 0.666667 0.333333 0.049096 70.33333 0.00946 0.00946 = 0.02632 0.00000 0.00000 0.00473 T2S 4 0.666667 0.333333 0.049096 -70.33333 0.00946 0.00946 = 0.02632 0.00000 0.00000 0.00473 T3A 7 0.333333 0.666667 0.061967 80.33333 0.00836 0.00836 = 0.01569 0.00000 0.00000 0.00418 T3S 4 0.333333 0.666667 0.061967 -80.33333 0.00836 0.00836 = 0.01569 0.00000 0.00000 0.00418 T4A 7 0.000000 0.000000 0.080530 90.33333 0.00852 0.00852 = 0.01673 0.00000 0.00000 0.00426 T4S 4 0.000000 0.000000 0.080530 -90.33333 0.00852 0.00852 = 0.01673 0.00000 0.00000 0.00426 O1 1 0.333333 0.666667 0.006080 10.33333 0.01721 0.01721 = 0.01258 0.00000 0.00000 0.00861 O2 1 0.135662 0.630155 0.065134 11.00000 0.00984 0.01354 = 0.01873 0.00049 0.00002 0.00642 O3 1 0.380201 0.480921 -0.004804 11.00000 0.01425 0.01475 = 0.02409 0.00004 0.00005 0.00635 O4 1 0.466669 0.307221 0.028610 11.00000 0.02267 0.01590 = 0.02064 -0.00108 -0.00208 0.01178 O5 1 0.517647 0.127875 0.076324 11.00000 0.01128 0.00929 = 0.01990 0.00173 -0.00230 0.00219 O6 1 0.214991 0.053480 0.041258 11.00000 0.01100 0.02173 = 0.02010 -0.00065 -0.00101 0.00850 O7 1 0.148893 0.435004 0.029483 11.00000 0.01452 0.01655 = 0.02126 -0.00306 -0.00136 0.00917 O8 1 0.395497 0.505602 0.041574 11.00000 0.02127 0.01286 = 0.02388 -0.00097 -0.00518 0.00874 O9 1 0.213963 0.040619 0.018001 11.00000 0.01796 0.01305 = 0.02122 0.00068 0.00213 0.00797 O10 1 0.666667 0.333333 0.041432 10.33333 0.02167 0.02167 = 0.02509 0.00000 0.00000 0.01083 O11 1 0.183731 0.230968 0.053571 11.00000 0.01405 0.01239 = 0.02069 -0.00046 -0.00229 0.00772 O12 1 0.387414 0.504233 0.017057 11.00000 0.01923 0.01655 = 0.02515 0.00157 -0.00055 0.01094 O13 1 0.666667 0.333333 0.065254 10.33333 0.01203 0.01203 = 0.01364 0.00000 0.00000 0.00602 O14 1 0.236059 0.072838 0.065689 11.00000 0.01262 0.01264 = 0.01972 0.00174 0.00074 0.00668 O15 1 0.333333 0.666667 0.078059 10.33333 0.01687 0.01687 = 0.01511 0.00000 0.00000 0.00844 O16 1 0.203295 0.253741 0.005699 11.00000 0.01676 0.01468 = 0.02273 0.00039 0.00004 0.00698 O17 1 0.638227 0.499458 0.052779 11.00000 0.01362 0.00972 = 0.01890 0.00106 0.00058 0.00707 O18 1 0.333333 0.666667 0.053982 10.33333 0.01219 0.01219 = 0.01254 0.00000 0.00000 0.00610 O19 1 0.160193 0.207817 0.077719 11.00000 0.01176 0.01133 = 0.01904 0.00131 -0.00097 0.00485 O20 1 0.000000 0.000000 0.030107 10.33333 0.01806 0.01806 = 0.01267 0.00000 0.00000 0.00903 LP 1 0.666667 0.333333 0.018222 0.09540 0.04813 EXYZ T1A T1S EADP T1A T1S EXYZ T2A T2S EADP T2A T2S EXYZ T3A T3S EADP T3A T3S EXYZ T4A T4S EADP T4A T4S HKLF 4 REM Carlfrancisite in R-3c REM R1 = 0.0337 for 3837 Fo > 4sig(Fo) and 0.0343 for all 3947 data REM 260 parameters refined using 0 restraints END WGHT 0.0562 130.4464 REM Highest difference peak 2.437, deepest hole -1.177, 1-sigma level 0.187 Q1 1 0.3333 0.6667 0.0104 10.33333 0.05 2.44 Q2 1 0.0000 0.0000 0.0344 10.33333 0.05 2.38 Q3 1 0.0000 0.0000 0.0421 10.33333 0.05 2.13 Q4 1 0.0000 0.0000 0.0846 10.33333 0.05 1.81 Q5 1 0.1049 0.3986 0.0752 11.00000 0.05 1.79 Q6 1 0.1185 0.4153 0.0454 11.00000 0.05 1.73 Q7 1 0.6667 0.3333 0.0275 10.33333 0.05 1.70 Q8 1 0.3333 0.6667 0.0182 10.33333 0.05 1.68 Q9 1 0.1046 0.3976 0.0683 11.00000 0.05 1.68 Q10 1 0.0019 0.2614 0.2535 11.00000 0.05 1.56 Q11 1 0.1143 0.4153 0.0523 11.00000 0.05 1.53 Q12 1 0.6858 0.1072 0.0564 11.00000 0.05 1.53 Q13 1 0.6847 0.1069 0.0636 11.00000 0.05 1.50 Q14 1 0.2119 0.2566 0.0203 11.00000 0.05 1.48 Q15 1 0.2173 0.2650 0.0273 11.00000 0.05 1.38 Q16 1 0.6667 0.3333 0.0457 10.33333 0.05 1.37 Q17 1 0.6454 0.5585 0.0316 11.00000 0.05 1.33 Q18 1 0.6667 0.3333 0.0695 10.33333 0.05 1.32 Q19 1 0.3333 0.6667 0.0577 10.33333 0.05 1.22 Q20 1 0.6484 0.5616 0.0389 11.00000 0.05 1.19 ; _shelx_res_checksum 92838 _shelx_hkl_file ; -1 -1 0 1324.46 44.32 2 -1 0 1376.68 41.22 -2 1 0 1377.07 25.94 1 1 0 1348.89 23.47 -1 2 0 1309.14 26.68 3 -3 0 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