data_FERRI-OBERTIITE _publ_contact_author ; Roberta Oberti ; _publ_contact_author_email ; oberti@crystal.unipv.it ; loop_ _publ_author_name _publ_author_address 'Oberti R.' 'CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Hawthorne F.C.' 'Dep. Geological Sciences, University of Manitoba, Winnipeg, Canada' 'Ball N.A.' 'Dep. Geological Sciences, University of Manitoba, Winnipeg, Canada' 'Blass G.' '4Merzbachstrasse 6, 52246 Eschweiler-St-Joris, Germany' _publ_section_title ; ? ; _audit_creation_method 'manually entered' _chemical_name_systematic ? _chemical_name_mineral ; FERRI-OBERTIITE ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_analytical ; Al0.06 Ca0.35 F0.55 Fe3+0.62 H0.19 K0.22 Mg3.58 Mn0.15 Na2.37 Ni0.01 O23.45 Si7.82 Ti0.78 Zn0.01 ; _chemical_formula_sum 'Ca0.30 F0.60 Fe0.89 K0.47 Mg3.24 Na2.03 O23.40 Si8.00 Ti0.86' _chemical_formula_weight 857.46 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' 'O2-' 'O2-' 0.0080 0.0060 'Hovesteydt, 1982' 'O-' 'O-' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F-' 'F-' 0.0140 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.082 0.0710 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si4+' 'Si4+' 0.082 0.0710 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti4+' 'Ti4+' 0.2780 0.4460 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe3+' 'Fe3+' 0.3460 0.8450 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg2+' 'Mg2+' 0.0490 0.0360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe2+' 'Fe2+' 0.3460 0.8450 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na+' 'Na+' 0.0360 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca2+' 'Ca2+' 0.2260 0.3060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K+' 'K+' 0.1790 0.2500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 9.7901(7) _cell_length_b 17.9354(13) _cell_length_c 5.2892(4) _cell_angle_alpha 90 _cell_angle_beta 104.142(2) _cell_angle_gamma 90 _cell_volume 900.58(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2268 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'acicular' _exptl_crystal_colour 'pink orange' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.162 _exptl_crystal_F_000 845.8 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 2.143 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _diffrn_radiation_probe 'x-ray' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Axs Smart-Apex CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6970 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.271 _diffrn_reflns_theta_max 30.010 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1365 _reflns_number_gt 1138 _reflns_threshold_expression 'I > 3\s(I)' _computing_data_collection 'SMART (Bruker-Axs Inc)' _computing_cell_refinement 'SAINT (Bruker-Axs Inc)' _computing_data_reduction 'SAINT (Bruker-Axs Inc)' _computing_structure_refinement 'ORFLS (Busing et al., 1962), modified' _refine_special_details ; Refinement of F against reflections with F > 3sigma(F). The threshold expression (_gt) of F > 3sigma(F) corresponds to the cutoff used to discriminate between observed and unobserved reflections for refinement. The use of unitary weigth produces unusual values for the calculated weighted wR-factor (similar to R). ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme UNIT _refine_ls_extinction_method NONE _refine_ls_number_reflns 1138 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0295 _refine_ls_wR_factor_gt 0.0265 _refine_ls_restrained_S_all 1.47 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 O1A O 0.11351(16) 0.08588(9) 0.21916(31) 0.0099(4) Uani 0.23(13) 1 d . . P . . O1B O2- 0.11351(16) 0.08588(9) 0.21916(31) 0.0099(4) Uani 0.77(13) 1 d . . P . . O2A O 0.11684(17) 0.16561(9) 0.72383(32) 0.0118(5) Uani 0.29(13) 1 d . . P . . O2B O2- 0.11684(17) 0.16561(9) 0.72383(32) 0.0118(5) Uani 0.71(13) 1 d . . P . . O3A O- 0.10417(24) 0.0000 0.70598(45) 0.0147(7) Uani 0.70(5) 2 d S T P . . O3B F- 0.10417(24) 0.0000 0.70598(45) 0.0147(7) Uani 0.30(5) 2 d S T P . . O4A O 0.35831(18) 0.25044(10) 0.79933(34) 0.0150(5) Uani 0.45(12) 1 d . . P . . O4B O2- 0.35831(18) 0.25044(10) 0.79933(34) 0.0150(5) Uani 0.55(12) 1 d . . P . . O5A O 0.34938(17) 0.12815(10) 0.08317(33) 0.0137(5) Uani 0.43(13) 1 d . . P . . O5B O2- 0.34938(17) 0.12815(10) 0.08317(33) 0.0137(5) Uani 0.57(13) 1 d . . P . . O6A O 0.34658(17) 0.11993(10) 0.58350(32) 0.0136(5) Uani 0.37(13) 1 d . . P . . O6B O2- 0.34658(17) 0.11993(10) 0.58350(32) 0.0136(5) Uani 0.63(13) 1 d . . P . . O7A O 0.34265(25) 0.0000 0.29968(50) 0.0144(7) Uani 0.38(9) 2 d S T P . . O7B O2- 0.34265(25) 0.0000 0.29968(50) 0.0144(7) Uani 0.62(9) 2 d S T P . . T1A Si 0.28353(6) 0.08522(3) 0.29551(12) 0.0090(2) Uani 0.76(10) 1 d . . P . . T1B Si4+ 0.28353(6) 0.08522(3) 0.29551(12) 0.0090(2) Uani 0.24(10) 1 d . . P . . T2A Si 0.28740(6) 0.17101(3) 0.79937(12) 0.0085(2) Uani 0.73(10) 1 d . . P . . T2B Si4+ 0.28740(6) 0.17101(3) 0.79937(12) 0.0085(2) Uani 0.27(10) 1 d . . P . . M1A Ti4+ 0.0000 0.08059(4) 0.5000 0.0136(3) Uani 0.265(6) 2 d S T P . . M1B Fe3+ 0.0000 0.08059(4) 0.5000 0.0136(3) Uani 0.265(6) 2 d S T P . . M1C Mg2+ 0.0000 0.08059(4) 0.5000 0.0136(3) Uani 0.470(6) 2 d S T P . . M2A Ti4+ 0.0000 0.18114(5) 0.0000 0.0109(3) Uani 0.166(6) 2 d S T P . . M2B Fe3+ 0.0000 0.18114(5) 0.0000 0.0109(3) Uani 0.167(6) 2 d S T P . . M2C Mg2+ 0.0000 0.18114(5) 0.0000 0.0109(3) Uani 0.667(6) 2 d S T P . . M3A Fe2+ 0.0000 0.0000 0.0000 0.0102(5) Uani 0.034(3) 4 d S T P . . M3B Mg2+ 0.0000 0.0000 0.0000 0.0102(5) Uani 0.966(3) 4 d S T P . . M4A Na+ 0.0000 0.27393(7) 0.5000 0.0198(5) Uani 0.850(10) 2 d S T P . . M4B Ca2+ 0.0000 0.27393(7) 0.5000 0.0198(5) Uani 0.150(10) 2 d S T P . . A Na+ 0.0000 0.5000 0.0000 0.0308(25) Uani 0.325(3) 4 d S T P . . AM K+ 0.0436(5) 0.5000 0.0920(8) 0.0350(13) Uani 0.233(3) 2 d S T P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1A 0.0092(7) 0.0108(7) 0.0096(7) -0.0006(5) 0.0023(6) -0.0011(6) O1B 0.0092(7) 0.0108(7) 0.0096(7) -0.0006(5) 0.0023(6) -0.0011(6) O2A 0.0113(7) 0.0129(8) 0.0114(7) -0.0003(6) 0.0033(6) 0.0001(6) O2B 0.0113(7) 0.0129(8) 0.0114(7) -0.0003(6) 0.0033(6) 0.0001(6) O3A 0.0141(11) 0.0174(11) 0.0123(11) 0.0000 0.0024(8) 0.0000 O3B 0.0141(11) 0.0174(11) 0.0123(11) 0.0000 0.0024(8) 0.0000 O4A 0.0196(8) 0.0121(8) 0.0128(8) -0.0031(6) 0.0032(6) 0.0000(6) O4B 0.0196(8) 0.0121(8) 0.0128(8) -0.0031(6) 0.0032(6) 0.0000(6) O5A 0.0118(7) 0.0174(8) 0.0126(8) -0.0004(6) 0.0044(6) 0.0042(6) O5B 0.0118(7) 0.0174(8) 0.0126(8) -0.0004(6) 0.0044(6) 0.0042(6) O6A 0.0124(7) 0.0176(8) 0.0107(7) 0.0000(6) 0.0025(6) -0.0039(7) O6B 0.0124(7) 0.0176(8) 0.0107(7) 0.0000(6) 0.0025(6) -0.0039(7) O7A 0.0118(11) 0.0098(10) 0.0205(12) 0.0000 0.0021(9) 0.0000 O7B 0.0118(11) 0.0098(10) 0.0205(12) 0.0000 0.0021(9) 0.0000 T1A 0.0095(3) 0.0090(3) 0.0087(3) -0.0003(2) 0.0025(2) -0.0004(2) T1B 0.0095(3) 0.0090(3) 0.0087(3) -0.0003(2) 0.0025(2) -0.0004(2) T2A 0.0089(3) 0.0091(3) 0.0076(3) -0.0013(2) 0.0021(2) -0.0002(2) T2B 0.0089(3) 0.0091(3) 0.0076(3) -0.0013(2) 0.0021(2) -0.0002(2) M1A 0.0105(4) 0.0220(5) 0.0086(4) 0.0000 0.0032(2) 0.0000 M1B 0.0105(4) 0.0220(5) 0.0086(4) 0.0000 0.0032(2) 0.0000 M1C 0.0105(4) 0.0220(5) 0.0086(4) 0.0000 0.0032(2) 0.0000 M2A 0.0111(4) 0.0122(5) 0.0096(4) 0.0000 0.0032(3) 0.0000 M2B 0.0111(4) 0.0122(5) 0.0096(4) 0.0000 0.0032(3) 0.0000 M2B 0.0111(4) 0.0122(5) 0.0096(4) 0.0000 0.0032(3) 0.0000 M3A 0.0111(8) 0.0117(8) 0.0075(8) 0.0000 0.0019(5) 0.0000 M3B 0.0111(8) 0.0117(8) 0.0075(8) 0.0000 0.0019(5) 0.0000 M4A 0.0224(8) 0.0174(8) 0.0238(8) 0.0000 0.0139(5) 0.0000 M4B 0.0224(8) 0.0174(8) 0.0238(8) 0.0000 0.0139(5) 0.0000 A 0.0166(32) 0.0645(54) 0.0161(33) 0.0000 0.0130(27) 0.0000 AM 0.0342(21) 0.0438(20) 0.0324(21) 0.0000 0.0185(16) 0.0000 _geom_special_details ; Geometry data (distances and angles) are reported only for T, M and A sites flagged by the A suffix. All esds are estimated using the full covariance matrix. ; 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 T1A O1A 1.614(2) . ? T1A O5A 1.620(2) . ? T1A O6A 1.622(2) . ? T1A O7A 1.633(1) . ? T2A O4A 1.585(2) . ? T2A O2A 1.622(2) . ? T2A O5A 1.663(2) 1_556 ? T2A O6A 1.674(2) . ? M1A O3A 1.942(2) . ? M1A O3A 1.942(2) 5_556 ? M1A O1A 2.063(2) 6_556 ? M1A O1A 2.063(2) . ? M1A O2A 2.091(2) . ? M1A O2A 2.091(2) 6_556 ? M2A O4A 1.959(2) 7_556 ? M2A O4A 1.959(2) 4_454 ? M2A O2A 2.082(2) 6_556 ? M2A O2A 2.082(2) 1_554 ? M2A O1A 2.206(2) . ? M2A O1A 2.206(2) 6 ? M3A O3A 2.058(2) 5_556 ? M3A O3A 2.058(2) 1_554 ? M3A O1A 2.079(2) 5 ? M3A O1A 2.079(2) 2 ? M3A O1A 2.079(2) 6 ? M3A O1A 2.079(2) . ? M4A O4A 2.386(2) 4_455 ? M4A O4A 2.386(2) 7_556 ? M4A O2A 2.413(2) 6_556 ? M4A O2A 2.413(2) . ? M4A O6A 2.530(2) 7_556 ? M4A O6A 2.530(2) 4_455 ? M4A O5A 2.921(2) 7_556 ? M4A O5A 2.921(2) 4_455 ? A O7A 2.466(3) 7 ? A O7A 2.466(3) 3_455 ? A O5A 2.823(2) 8 ? A O5A 2.823(2) 4_455 ? A O5A 2.823(2) 3_455 ? A O5A 2.823(2) 7 ? A O6A 3.181(2) 8_556 ? A O6A 3.181(2) 4_454 ? A O6A 3.181(2) 3_454 ? A O6A 3.181(2) 7_556 ? AM O7A 2.477(5) 3_455 ? AM O7A 2.580(5) 7 ? AM O5A 2.777(3) 8 ? AM O5A 2.777(3) 7 ? AM O6A 2.798(5) 8_556 ? AM O6A 2.798(5) 7_556 ? AM O5A 2.976(4) 4_455 ? AM O5A 2.976(4) 3_455 ? AM O7A 3.137(8) 7_556 ? 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 O1A T1A O5A 112.6(1) . . ? O1A T1A O6A 111.4(1) . . ? O5A T1A O6A 110.1(1) . . ? O1A T1A O7A 110.5(1) . . ? O5A T1A O7A 104.7(1) . . ? O6A T1A O7A 107.1(1) . . ? O4A T2A O2A 118.6(1) . . ? O4A T2A O5A 110.6(1) . 1_556 ? O2A T2A O5A 108.7(1) . 1_556 ? O4A T2A O6A 105.5(1) . . ? O2A T2A O6A 107.8(1) . . ? O5A T2A O6A 104.6(1) 1_556 . ? O3A M1A O3A 83.8(1) . 5_556 ? O3A M1A O1A 86.1(1) . 6_556 ? O3A M1A O1A 97.9(1) 5_556 6_556 ? O3A M1A O1A 97.9(1) . . ? O3A M1A O1A 86.1(1) 5_556 . ? O1A M1A O1A 174.7(1) 6_556 . ? O3A M1A O2A 94.9(1) . . ? O3A M1A O2A 178.5(1) 5_556 . ? O1A M1A O2A 82.8(1) 6_556 . ? O1A M1A O2A 93.3(1) . . ? O3A M1A O2A 178.5(1) . 6_556 ? O3A M1A O2A 94.9(1) 5_556 6_556 ? O1A M1A O2A 93.3(1) 6_556 6_556 ? O1A M1A O2A 82.8(1) . 6_556 ? O2A M1A O2A 86.4(1) . 6_556 ? O4A M2A O4A 102.4(1) 7_556 4_454 ? O4A M2A O2A 98.1(1) 7_556 6_556 ? O4A M2A O2A 91.5(1) 4_454 6_556 ? O4A M2A O2A 91.5(1) 7_556 1_554 ? O4A M2A O2A 98.1(1) 4_454 1_554 ? O2A M2A O2A 164.6(1) 6_556 1_554 ? O4A M2A O1A 90.1(1) 7_556 . ? O4A M2A O1A 165.7(1) 4_454 . ? O2A M2A O1A 79.7(1) 6_556 . ? O2A M2A O1A 88.4(1) 1_554 . ? O4A M2A O1A 165.7(1) 7_556 6 ? O4A M2A O1A 90.1(1) 4_454 6 ? O2A M2A O1A 88.4(1) 6_556 6 ? O2A M2A O1A 79.7(1) 1_554 6 ? O1A M2A O1A 78.5(1) . 6 ? O3A M3A O3A 180.0 5_556 1_554 ? O3A M3A O1A 97.2(1) 5_556 5 ? O3A M3A O1A 82.8(1) 1_554 5 ? O3A M3A O1A 82.8(1) 5_556 2 ? O3A M3A O1A 97.2(1) 1_554 2 ? O1A M3A O1A 84.4(1) 5 2 ? O3A M3A O1A 97.2(1) 5_556 6 ? O3A M3A O1A 82.8(1) 1_554 6 ? O1A M3A O1A 95.6(1) 5 6 ? O1A M3A O1A 180.0 2 6 ? O3A M3A O1A 82.8(1) 5_556 . ? O3A M3A O1A 97.2(1) 1_554 . ? O1A M3A O1A 180.0 5 . ? O1A M3A O1A 95.6(1) 2 . ? O1A M3A O1A 84.4(1) 6 . ? O4A M4A O4A 158.9(1) 4_455 7_556 ? O4A M4A O2A 84.0(1) 4_455 6_556 ? O4A M4A O2A 79.0(1) 7_556 6_556 ? O4A M4A O2A 79.0(1) 4_455 . ? O4A M4A O2A 84.0(1) 7_556 . ? O2A M4A O2A 72.8(1) 6_556 . ? O4A M4A O6A 136.0(1) 4_455 7_556 ? O4A M4A O6A 63.6(1) 7_556 7_556 ? O2A M4A O6A 138.7(1) 6_556 7_556 ? O2A M4A O6A 117.5(1) . 7_556 ? O4A M4A O6A 63.6(1) 4_455 4_455 ? O4A M4A O6A 136.0(1) 7_556 4_455 ? O2A M4A O6A 117.5(1) 6_556 4_455 ? O2A M4A O6A 138.7(1) . 4_455 ? O6A M4A O6A 82.4(1) 7_556 4_455 ? O4A M4A O5A 83.0(1) 4_455 7_556 ? O4A M4A O5A 110.0(1) 7_556 7_556 ? O2A M4A O5A 161.1(1) 6_556 7_556 ? O2A M4A O5A 91.3(1) . 7_556 ? O6A M4A O5A 57.8(1) 7_556 7_556 ? O6A M4A O5A 68.1(1) 4_455 7_556 ? O4A M4A O5A 110.0(1) 4_455 4_455 ? O4A M4A O5A 83.0(1) 7_556 4_455 ? O2A M4A O5A 91.3(1) 6_556 4_455 ? O2A M4A O5A 161.1(1) . 4_455 ? O6A M4A O5A 68.1(1) 7_556 4_455 ? O6A M4A O5A 57.8(1) 4_455 4_455 ? O5A M4A O5A 106.1(1) 7_556 4_455 ? O7A A O7A 180.0 7 3_455 ? O7A A O5A 57.8(1) 7 8 ? O7A A O5A 122.2(1) 3_455 8 ? O7A A O5A 122.2(1) 7 4_455 ? O7A A O5A 57.8(1) 3_455 4_455 ? O5A A O5A 180.0 8 4_455 ? O7A A O5A 122.2(1) 7 3_455 ? O7A A O5A 57.8(1) 3_455 3_455 ? O5A A O5A 71.0(1) 8 3_455 ? O5A A O5A 109.0(1) 4_455 3_455 ? O7A A O5A 57.8(1) 7 7 ? O7A A O5A 122.2(1) 3_455 7 ? O5A A O5A 109.0(1) 8 7 ? O5A A O5A 71.0(1) 4_455 7 ? O5A A O5A 180.0 3_455 7 ? O7A A O6A 100.5(1) 7 8_556 ? O7A A O6A 79.5(1) 3_455 8_556 ? O5A A O6A 51.8(1) 8 8_556 ? O5A A O6A 128.2(1) 4_455 8_556 ? O5A A O6A 61.2(1) 3_455 8_556 ? O5A A O6A 118.8(1) 7 8_556 ? O7A A O6A 79.5(1) 7 4_454 ? O7A A O6A 100.5(1) 3_455 4_454 ? O5A A O6A 128.2(1) 8 4_454 ? O5A A O6A 51.8(1) 4_455 4_454 ? O5A A O6A 118.8(1) 3_455 4_454 ? O5A A O6A 61.2(1) 7 4_454 ? O6A A O6A 180.0 8_556 4_454 ? O7A A O6A 79.5(1) 7 3_454 ? O7A A O6A 100.5(1) 3_455 3_454 ? O5A A O6A 61.2(1) 8 3_454 ? O5A A O6A 118.8(1) 4_455 3_454 ? O5A A O6A 51.8(1) 3_455 3_454 ? O5A A O6A 128.2(1) 7 3_454 ? O6A A O6A 94.9(1) 8_556 3_454 ? O6A A O6A 85.1(1) 4_454 3_454 ? O7A A O6A 100.5(1) 7 7_556 ? O7A A O6A 79.5(1) 3_455 7_556 ? O5A A O6A 118.8(1) 8 7_556 ? O5A A O6A 61.2(1) 4_455 7_556 ? O5A A O6A 128.2(1) 3_455 7_556 ? O5A A O6A 51.8(1) 7 7_556 ? O6A A O6A 85.1(1) 8_556 7_556 ? O6A A O6A 94.9(1) 4_454 7_556 ? O6A A O6A 180.0 3_454 7_556 ? O7A AM O7A 154.4(1) 3_455 7 ? O7A AM O5A 123.6(1) 3_455 8 ? O7A AM O5A 57.3(1) 7 8 ? O7A AM O5A 123.6(1) 3_455 7 ? O7A AM O5A 57.3(1) 7 7 ? O5A AM O5A 111.7(1) 8 7 ? O7A AM O6A 87.5(1) 3_455 8_556 ? O7A AM O6A 108.4(1) 7 8_556 ? O5A AM O6A 56.5(1) 8 8_556 ? O5A AM O6A 136.2(1) 7 8_556 ? O7A AM O6A 87.5(1) 3_455 7_556 ? O7A AM O6A 108.4(1) 7 7_556 ? O5A AM O6A 136.2(1) 8 7_556 ? O5A AM O6A 56.5(1) 7 7_556 ? O6A AM O6A 100.5(1) 8_556 7_556 ? O7A AM O5A 55.5(1) 3_455 4_455 ? O7A AM O5A 112.8(1) 7 4_455 ? O5A AM O5A 157.8(1) 8 4_455 ? O5A AM O5A 69.3(1) 7 4_455 ? O6A AM O5A 138.7(1) 8_556 4_455 ? O6A AM O5A 64.2(1) 7_556 4_455 ? O7A AM O5A 55.5(1) 3_455 3_455 ? O7A AM O5A 112.8(1) 7 3_455 ? O5A AM O5A 69.3(1) 8 3_455 ? O5A AM O5A 157.8(1) 7 3_455 ? O6A AM O5A 64.2(1) 8_556 3_455 ? O6A AM O5A 138.7(1) 7_556 3_455 ? O5A AM O5A 101.1(1) 4_455 3_455 ? O7A AM O7A 70.5(1) 3_455 7_556 ? O7A AM O7A 135.1(1) 7 7_556 ? O5A AM O7A 105.9(1) 8 7_556 ? O5A AM O7A 105.9(1) 7 7_556 ? O6A AM O7A 52.0(1) 8_556 7_556 ? O6A AM O7A 52.0(1) 7_556 7_556 ? O5A AM O7A 94.7(1) 4_455 7_556 ? O5A AM O7A 94.7(1) 3_455 7_556 ? T1A O5A T2A 136.6(1) . 1_554 ? T1A O6A T2A 137.3(1) . . ? T1A O7A T1A 138.8(1) . 2 ? O6A O7A O6A 110.5(1) 2 . ? O5A O6A O5A 173.5(1) 1_556 . ? _refine_diff_density_max 1.3 _refine_diff_density_min -0.4 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 2 0 3.0 0.5 0 4 0 1277.6 9.4 0 6 0 -4.9 0.5 0 8 0 61.6 1.8 0 10 0 746.3 8.0 0 12 0 5990.8 40.6 0 14 0 5.2 0.8 0 16 0 41.3 2.6 0 18 0 1.7 0.8 0 20 0 575.8 14.9 0 22 0 391.0 11.8 0 24 0 1122.6 32.2 1 1 0 520.4 3.0 1 3 0 0.5 0.1 1 5 0 2.6 0.3 1 7 0 273.9 2.7 1 9 0 954.1 6.5 1 11 0 1721.8 10.5 1 13 0 83.7 2.1 1 15 0 2.7 0.4 1 17 0 21.8 1.3 1 19 0 29.2 2.0 1 21 0 20.7 1.9 -1 23 0 5.7 0.8 -1 25 0 7.7 2.0 2 0 0 13.4 0.8 2 2 0 16.4 0.5 2 4 0 1570.6 8.7 2 6 0 2.5 0.3 2 8 0 3.1 0.4 2 10 0 117.1 2.0 2 12 0 52.5 1.4 2 14 0 187.8 3.0 2 16 0 91.6 2.4 2 18 0 5.5 0.8 2 20 0 10.8 1.2 2 22 0 22.0 2.1 2 24 0 230.6 7.8 3 1 0 3590.0 16.8 3 3 0 946.2 6.1 3 5 0 530.6 4.3 3 7 0 102.3 1.7 3 9 0 34.1 1.1 3 11 0 1179.5 9.8 3 13 0 6.9 0.7 3 15 0 52.1 1.8 3 17 0 76.2 3.1 3 19 0 246.6 5.5 3 21 0 16.1 1.9 3 23 0 261.4 8.4 4 0 0 40.5 1.5 4 2 0 0.7 0.2 4 4 0 26.6 0.9 4 6 0 2.1 0.3 4 8 0 2104.3 11.8 4 10 0 314.7 3.6 4 12 0 545.7 5.3 4 14 0 6.5 0.8 4 16 0 102.9 3.7 4 18 0 1.8 0.8 4 20 0 243.6 6.7 4 22 0 232.5 6.7 4 24 0 7.6 3.0 5 1 0 819.4 6.0 5 3 0 395.7 3.8 5 5 0 0.3 0.2 5 7 0 2.4 0.5 5 9 0 5.0 0.5 5 11 0 103.2 3.8 5 13 0 446.0 6.3 5 15 0 490.0 7.7 5 17 0 2.7 0.8 5 19 0 9.1 3.0 5 21 0 48.6 7.7 5 23 0 240.5 7.2 6 0 0 2056.1 18.1 6 2 0 61.5 1.5 6 4 0 5.2 0.5 6 6 0 8.4 0.8 6 8 0 171.8 2.9 6 10 0 19.2 1.3 6 12 0 2.2 0.6 6 14 0 1.2 0.8 6 16 0 275.0 8.0 6 18 0 2.4 0.8 6 20 0 40.4 5.0 6 22 0 17.1 2.1 7 1 0 951.8 7.5 7 3 0 321.3 4.0 7 5 0 0.3 0.4 7 7 0 406.0 5.1 7 9 0 1177.2 11.1 -7 11 0 2535.0 27.9 7 13 0 360.1 8.8 7 15 0 239.2 6.6 7 17 0 31.0 2.8 7 19 0 144.0 5.5 7 21 0 8.3 1.4 8 0 0 1537.2 15.2 8 2 0 8.9 0.8 8 4 0 4.0 0.6 8 6 0 48.8 2.2 8 8 0 4.3 0.7 8 10 0 36.6 2.6 8 12 0 217.0 6.5 8 14 0 5.2 1.1 8 16 0 15.5 2.7 8 18 0 15.9 2.1 8 20 0 13.3 2.0 9 1 0 151.1 3.6 9 3 0 26.1 1.3 9 5 0 0.6 0.5 9 7 0 131.1 4.7 9 9 0 43.7 3.2 9 11 0 25.9 2.4 9 13 0 10.0 2.7 9 15 0 230.3 7.0 9 17 0 30.3 2.9 10 0 0 925.5 12.1 10 2 0 1.1 0.3 10 4 0 15.2 1.5 10 6 0 10.1 1.4 10 8 0 697.4 15.1 10 10 0 100.9 4.3 10 12 0 818.7 23.8 10 14 0 2.1 0.8 10 16 0 103.8 5.1 11 1 0 595.9 8.8 11 3 0 57.5 3.1 11 5 0 27.3 2.3 11 7 0 11.0 1.5 11 9 0 20.7 4.0 11 11 0 497.4 10.5 11 13 0 29.7 2.8 12 0 0 13.6 2.0 -12 2 0 5.8 1.8 12 4 0 68.4 3.2 12 6 0 2.4 0.9 12 8 0 63.6 3.7 12 10 0 21.7 2.3 -13 3 0 12.2 5.3 -13 5 0 22.9 3.0 0 0 1 4.4 0.4 0 2 1 234.7 2.9 0 4 1 59.8 1.3 0 6 1 2627.4 19.4 0 8 1 0.4 0.2 0 10 1 20.6 0.9 0 12 1 8.4 0.7 0 14 1 327.8 4.1 0 16 1 375.2 5.6 0 18 1 29.8 1.7 0 20 1 17.8 1.6 0 22 1 14.1 1.5 0 24 1 3.1 0.8 1 1 1 458.5 3.2 -1 1 1 80.6 1.9 1 3 1 2822.5 15.7 -1 3 1 411.0 6.1 1 5 1 5824.4 26.4 -1 5 1 365.2 4.8 1 7 1 1092.3 13.2 -1 7 1 1373.0 8.0 1 9 1 408.1 5.9 -1 9 1 1463.0 8.9 1 11 1 47.2 1.4 -1 11 1 11.1 0.7 1 13 1 406.2 4.4 -1 13 1 19.5 1.0 1 15 1 471.5 5.2 -1 15 1 71.9 2.1 1 17 1 1809.1 14.8 -1 17 1 193.0 3.7 1 19 1 174.2 6.4 -1 19 1 161.7 4.0 1 21 1 96.6 4.0 -1 21 1 465.0 11.0 1 23 1 2.4 1.1 -1 23 1 19.6 3.0 2 0 1 47.1 1.3 -2 0 1 1.1 0.4 2 2 1 1241.5 12.8 -2 2 1 153.3 1.8 2 4 1 5.1 0.5 -2 4 1 43.3 1.2 2 6 1 3964.2 25.5 -2 6 1 18.6 1.1 2 8 1 14.6 0.6 -2 8 1 3.4 0.6 2 10 1 552.1 4.8 -2 10 1 21.6 0.8 2 12 1 0.6 0.4 -2 12 1 10.4 0.9 2 14 1 50.2 3.2 -2 14 1 624.9 8.7 2 16 1 121.2 3.1 -2 16 1 288.3 4.5 2 18 1 16.2 1.5 -2 18 1 17.1 1.2 2 20 1 87.9 3.8 -2 20 1 43.6 3.3 2 22 1 104.1 5.1 -2 22 1 0.1 0.8 2 24 1 2.5 1.1 -2 24 1 4.3 1.9 3 1 1 2.5 0.3 -3 1 1 449.3 3.6 3 3 1 130.8 1.6 -3 3 1 1784.2 16.0 3 5 1 1237.5 8.2 -3 5 1 2383.7 18.5 3 7 1 102.2 2.8 -3 7 1 181.1 4.3 3 9 1 53.1 1.9 -3 9 1 264.3 3.4 3 11 1 5.5 0.6 -3 11 1 127.1 2.5 3 13 1 6.1 0.8 -3 13 1 266.3 4.0 3 15 1 0.5 0.3 -3 15 1 168.7 3.3 3 17 1 38.5 2.2 -3 17 1 812.1 9.3 3 19 1 1.4 0.6 -3 19 1 1.2 0.6 3 21 1 79.9 3.8 -3 21 1 6.6 0.9 3 23 1 11.5 1.9 -3 23 1 14.7 2.7 4 0 1 4.0 0.7 -4 0 1 91.8 2.1 4 2 1 645.3 5.0 -4 2 1 994.2 6.6 4 4 1 66.1 2.0 -4 4 1 2.0 0.3 4 6 1 5887.7 51.2 -4 6 1 625.1 5.3 4 8 1 13.2 1.0 -4 8 1 2.0 0.5 4 10 1 80.3 2.8 -4 10 1 647.3 6.5 4 12 1 1.2 0.6 -4 12 1 1.3 0.3 4 14 1 1076.0 10.6 -4 14 1 4.3 0.7 4 16 1 416.8 7.6 -4 16 1 82.1 3.7 4 18 1 967.0 20.3 -4 18 1 10.3 1.3 4 20 1 1.4 0.6 -4 20 1 89.6 3.9 4 22 1 36.0 3.4 -4 22 1 102.6 4.3 -4 24 1 4.3 1.9 5 1 1 3.0 0.4 -5 1 1 5.6 0.5 5 3 1 15.7 0.8 -5 3 1 128.3 1.9 5 5 1 1238.9 8.2 -5 5 1 136.4 2.2 5 7 1 184.4 3.0 -5 7 1 41.1 1.2 5 9 1 74.8 2.5 -5 9 1 109.5 2.2 5 11 1 1.0 0.4 -5 11 1 2.4 0.5 5 13 1 14.2 1.5 -5 13 1 9.1 1.0 5 15 1 1.8 1.0 -5 15 1 12.5 1.2 5 17 1 315.1 6.6 -5 17 1 1.3 0.6 5 19 1 3.1 0.9 -5 19 1 1.7 1.3 5 21 1 62.3 3.8 -5 21 1 39.8 4.5 -5 23 1 0.4 0.7 6 0 1 7.8 1.7 -6 0 1 3.0 0.7 6 2 1 102.8 2.0 -6 2 1 306.6 5.7 6 4 1 7.8 0.6 -6 4 1 18.9 1.3 6 6 1 807.5 7.4 -6 6 1 8346.0 87.3 6 8 1 24.4 1.4 -6 8 1 21.9 1.3 6 10 1 136.7 3.3 -6 10 1 112.1 3.9 6 12 1 2.3 0.5 -6 12 1 -0.1 0.3 6 14 1 3.5 0.7 -6 14 1 374.0 6.8 6 16 1 22.2 2.8 -6 16 1 320.8 8.0 6 18 1 803.3 13.4 -6 18 1 900.0 13.9 6 20 1 117.3 7.3 -6 20 1 2.7 0.8 -6 22 1 0.6 0.7 7 1 1 2.7 0.4 -7 1 1 5.4 0.6 7 3 1 129.1 2.7 -7 3 1 152.3 2.5 7 5 1 239.7 4.4 -7 5 1 2322.3 17.6 7 7 1 2.2 0.5 -7 7 1 538.2 6.8 7 9 1 2.8 1.0 -7 9 1 0.1 0.3 7 11 1 9.4 1.5 -7 11 1 -0.2 0.5 7 13 1 70.2 4.4 -7 13 1 33.6 2.1 7 15 1 48.1 3.3 -7 15 1 34.7 2.8 7 17 1 112.9 4.8 -7 17 1 711.2 12.2 7 19 1 0.2 0.7 -7 19 1 103.8 4.6 -7 21 1 1.2 1.2 8 0 1 29.2 1.9 -8 0 1 1.6 0.5 8 2 1 106.4 2.7 -8 2 1 52.5 1.8 8 4 1 0.7 0.3 -8 4 1 21.7 1.5 8 6 1 1709.4 14.6 -8 6 1 74.7 2.5 8 8 1 22.8 1.6 -8 8 1 65.4 2.4 8 10 1 6.4 1.0 -8 10 1 80.4 3.1 8 12 1 16.9 2.4 -8 12 1 4.5 0.9 8 14 1 197.6 6.3 -8 14 1 4.1 1.0 8 16 1 147.4 5.6 -8 16 1 54.8 5.7 8 18 1 180.3 6.4 -8 18 1 209.8 6.7 -8 20 1 115.6 5.8 9 1 1 2.7 0.4 -9 1 1 0.8 0.4 9 3 1 0.7 0.4 -9 3 1 64.9 2.9 9 5 1 3.8 0.6 -9 5 1 426.8 7.9 9 7 1 34.7 2.0 -9 7 1 37.8 3.0 9 9 1 56.0 3.5 -9 9 1 1.7 0.5 9 11 1 1.9 0.6 -9 11 1 -0.1 0.5 9 13 1 6.0 1.8 -9 13 1 3.6 0.9 9 15 1 2.0 0.8 -9 15 1 1.7 0.7 9 17 1 9.3 1.6 -9 17 1 82.7 7.7 -9 19 1 1.5 0.7 10 0 1 1.6 1.4 -10 0 1 8.9 2.7 10 2 1 11.8 2.3 -10 2 1 111.1 2.8 10 4 1 14.0 1.3 -10 4 1 26.3 2.5 10 6 1 73.2 3.6 -10 6 1 1019.3 20.1 10 8 1 4.9 1.0 -10 8 1 4.7 1.3 10 10 1 42.4 5.5 -10 10 1 0.6 0.6 10 12 1 1.4 0.7 -10 12 1 1.6 0.9 10 14 1 8.5 1.4 -10 14 1 321.6 8.4 -10 16 1 162.7 6.1 11 1 1 3.1 1.2 -11 1 1 3.0 0.8 11 3 1 243.1 6.7 -11 3 1 1.8 1.3 11 5 1 1246.0 19.3 -11 5 1 9.3 1.4 11 7 1 513.8 10.3 -11 7 1 85.7 3.3 11 9 1 87.3 4.3 -11 9 1 95.6 5.3 11 11 1 0.6 0.7 -11 11 1 1.2 0.7 -11 13 1 21.4 2.3 -11 15 1 3.3 1.3 12 0 1 14.2 3.7 -12 0 1 12.9 2.0 12 2 1 70.1 4.1 -12 2 1 71.5 3.5 12 4 1 33.2 3.7 -12 4 1 22.0 2.6 12 6 1 310.7 9.3 -12 6 1 0.1 0.9 12 8 1 4.1 1.7 -12 8 1 11.9 2.0 -12 10 1 84.3 4.2 -12 12 1 2.9 1.0 -13 1 1 2.7 3.2 -13 3 1 162.3 6.2 -13 5 1 513.8 12.2 -13 7 1 139.2 10.9 0 0 2 713.8 6.9 0 2 2 1.4 0.4 0 4 2 13.6 0.8 0 6 2 3.3 0.4 0 8 2 102.6 1.8 0 10 2 61.0 1.5 0 12 2 1683.3 14.3 0 14 2 103.3 2.7 0 16 2 236.6 5.2 0 18 2 4.6 1.4 0 20 2 23.3 1.9 0 22 2 7.6 1.3 0 24 2 382.8 10.9 1 1 2 41.6 1.0 -1 1 2 27.7 0.8 1 3 2 58.4 1.5 -1 3 2 1.2 0.2 1 5 2 187.5 4.7 -1 5 2 166.1 2.2 1 7 2 422.6 4.2 -1 7 2 16.4 0.8 1 9 2 1068.1 14.1 -1 9 2 2.6 0.4 1 11 2 2400.6 16.9 -1 11 2 37.7 1.5 1 13 2 143.5 4.6 -1 13 2 206.9 3.5 1 15 2 19.3 1.4 -1 15 2 272.8 5.3 1 17 2 3.4 1.6 -1 17 2 10.1 1.1 1 19 2 82.7 3.3 -1 19 2 59.1 3.3 1 21 2 4.7 1.9 -1 21 2 5.5 1.1 1 23 2 122.9 6.2 -1 23 2 8.7 1.5 2 0 2 3867.3 26.7 -2 0 2 9951.5 62.5 2 2 2 18.2 1.1 -2 2 2 24.4 0.8 2 4 2 579.4 7.9 -2 4 2 803.0 6.8 2 6 2 25.2 1.2 -2 6 2 2.9 0.5 2 8 2 205.1 3.6 -2 8 2 1457.0 10.7 2 10 2 211.1 3.8 -2 10 2 347.8 6.1 2 12 2 171.6 4.9 -2 12 2 6033.3 32.3 2 14 2 0.0 0.4 -2 14 2 0.7 0.3 2 16 2 2.2 0.9 -2 16 2 74.4 4.8 2 18 2 1.7 0.9 -2 18 2 2.4 1.5 2 20 2 392.6 8.9 -2 20 2 114.8 4.5 2 22 2 150.4 5.5 -2 22 2 329.0 8.2 -2 24 2 284.5 11.6 3 1 2 6.3 0.5 -3 1 2 2127.5 11.2 3 3 2 42.8 1.0 -3 3 2 901.9 6.6 3 5 2 26.5 1.3 -3 5 2 608.6 8.4 3 7 2 29.8 1.4 -3 7 2 5.1 0.8 3 9 2 3.2 1.0 -3 9 2 137.5 2.4 3 11 2 6.4 0.9 -3 11 2 665.4 6.4 3 13 2 182.0 4.0 -3 13 2 2.6 0.6 3 15 2 320.7 5.6 -3 15 2 25.3 1.6 3 17 2 5.4 0.9 -3 17 2 4.8 0.7 3 19 2 6.2 1.1 -3 19 2 150.7 4.4 3 21 2 16.5 3.3 -3 21 2 7.2 1.2 3 23 2 94.6 10.7 -3 23 2 50.6 3.9 4 0 2 2159.7 32.2 -4 0 2 2307.9 22.5 4 2 2 53.3 1.6 -4 2 2 5.5 0.5 4 4 2 688.9 6.0 -4 4 2 587.0 5.3 4 6 2 1.9 0.5 -4 6 2 -1.7 0.3 4 8 2 192.3 3.8 -4 8 2 279.5 4.4 4 10 2 28.2 1.8 -4 10 2 82.7 2.4 4 12 2 1446.2 13.0 -4 12 2 18.6 1.3 4 14 2 2.8 0.8 -4 14 2 119.5 3.7 4 16 2 -0.5 0.4 -4 16 2 186.8 6.3 4 18 2 1.0 0.6 -4 18 2 7.7 0.9 4 20 2 1.6 0.9 -4 20 2 23.2 1.7 4 22 2 49.8 3.6 -4 22 2 11.9 1.9 5 1 2 4107.6 25.6 -5 1 2 1187.4 7.7 5 3 2 1144.9 10.7 -5 3 2 16.7 0.9 5 5 2 209.9 4.5 -5 5 2 52.1 1.7 5 7 2 8.4 1.1 -5 7 2 163.3 3.3 5 9 2 291.3 5.0 -5 9 2 893.2 9.9 5 11 2 2401.7 18.3 -5 11 2 2939.4 20.6 5 13 2 269.3 5.2 -5 13 2 432.5 6.4 5 15 2 50.8 2.8 -5 15 2 41.5 2.2 5 17 2 7.7 1.2 -5 17 2 12.3 1.3 5 19 2 254.4 6.5 -5 19 2 30.7 4.0 5 21 2 45.1 7.7 -5 21 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7 290.6 10.9 -2 4 7 11.6 2.9 -2 6 7 1001.1 22.6 -2 8 7 2.5 1.0 -3 1 7 0.3 1.0 -3 3 7 3.1 3.4 -3 5 7 56.3 5.4 -3 7 7 2.9 1.0 -4 0 7 6.9 2.5 -4 2 7 28.7 3.7 -4 4 7 0.1 1.0 -4 6 7 158.6 14.3 -4 8 7 5.6 2.6 -5 1 7 13.9 4.3 -5 3 7 65.1 3.8 -5 5 7 197.0 7.5 -5 7 7 17.1 6.4 -6 0 7 9.8 4.3 -6 2 7 4.0 1.6 -6 4 7 0.3 0.8 -6 6 7 490.1 12.6 -7 1 7 1.9 1.0 -7 3 7 4.5 1.4