data_MAGNESIO-FERRI-FLUORO-HORNBLENDE _publ_contact_author ; Roberta Oberti ; _publ_contact_author_email ; oberti@crystal.unipv.it ; loop_ _publ_author_name _publ_author_address 'Oberti R.' 'CNR-IGG, UOS 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' 'Chiappino L.' 'via Palmanova 67, I-20132 Milano, Italy' _publ_section_title ; Magnesio-ferri-fluoro-hornblende from Portoscuso, Sardinia, Italy: description of a newly approved member of the amphibole supergroup ; _audit_creation_method 'manually entered' _chemical_name_systematic ; ? ; _chemical_name_mineral 'MAGNESIO-FERRI-FLUORO-HORNBLENDE' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al1 Ca1.62 F1.56 Fe2.56 H0.72 K0.30 Mg2.47 Na0.38 O22.44 Si7' _chemical_formula_analytical ; Al1.11 Ca1.66 Cl0.08 F1.55 Fe2+1.94 Fe3+0.72 H0.37 K0.22 Mg2.20 Mn0.10 Na0.40 O22.37 Si6.89 Ti0.13 Zn0.01 ; _chemical_formula_weight 901.05 _chemical_compound_source ; Portoscuso, Cagliari, Sardinia, Italy, sample code 1231 in the amphibole database of the CNR-IGG Pavia. Type material is deposited in the mineralogical collections of the Mineralogical Museum of the Dipartimento di Scienze della Terra e dell'Ambiente, Pavia, Italy, sample number 2014-01 ; 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-' 0.0106 0.0060 'Hovesteydt, 1982' 'F-' 'F-' 0.0140 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O-' 'O-' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' 'Al3+' 'Al3+' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si4+' 'Si4+' 0.0817 0.0704 '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' 'Fe3+' 'Fe3+' 0.3460 0.8450 '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' 'Na+' 'Na+' 0.0360 0.0250 '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' 'H' 'H' 0.0000 0.0000 '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_ _symmetry_equiv_pos_as_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 9.839(5) _cell_length_b 18.078(9) _cell_length_c 5.319(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.99(3) _cell_angle_gamma 90.00 _cell_volume 913.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 887.1 _exptl_absorpt_coefficient_mu 3.28 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.65 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_probe 'x-ray' _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'PHILIPS PW1100' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2715 _diffrn_reflns_av_R_equivalents 0.0270 _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 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.09 _reflns_number_total 1390 _reflns_number_gt 1013 _reflns_threshold_expression >3\s(I) _computing_data_collection 'local program' _computing_cell_refinement 'LAT routine of PW1100 diffractometer' _computing_data_reduction 'local program' _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 _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method 'secondary isotropic' _refine_ls_extinction_coef 0.0000025(7) _refine_ls_extinction_expression 'Zachariasen, 1967' _refine_ls_number_reflns 1013 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0360 _refine_ls_wR_factor_gt 0.0233 _refine_ls_restrained_S_all 1.496 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.11024(20) 0.08735(10) 0.21700(37) 0.0109(5) Uani 0.24(15) 1 d P . . O1B O2- 0.11024(20) 0.08735(10) 0.21700(37) 0.0109(5) Uani 0.76(15) 1 d P . . O2A O 0.11934(20) 0.17161(11) 0.72864(36) 0.0117(5) Uani 0.55(15) 1 d P . . O2B O2- 0.11934(20) 0.17161(11) 0.72864(36) 0.0117(5) Uani 0.45(15) 1 d P . . O3A F- 0.10456(27) 0.0000 0.71200(47) 0.0151(8) Uani 0.78(5) 2 d SP . . O3B O- 0.10456(27) 0.0000 0.71200(47) 0.0151(8) Uani 0.22(5) 2 d SP . . O4A O 0.36559(22) 0.24943(11) 0.79359(38) 0.0135(6) Uani 0.47(15) 1 d P . . O4B O2- 0.36559(22) 0.24943(11) 0.79359(38) 0.0135(6) Uani 0.53(15) 1 d P . . O5A O 0.34844(22) 0.13600(11) 0.10233(40) 0.0154(6) Uani 0.57(16) 1 d P . . O5B O2- 0.34844(22) 0.13600(11) 0.10233(40) 0.0154(6) Uani 0.43(16) 1 d P . . O6A O 0.34449(22) 0.12020(10) 0.59232(40) 0.0137(6) Uani 0.60(16) 1 d P . . O6B O2- 0.34449(22) 0.12020(10) 0.59232(40) 0.0137(6) Uani 0.40(16) 1 d P . . O7A O 0.33836(30) 0.0000 0.29549(57) 0.0150(8) Uani 0.46(11) 2 d SP . . O7B O2- 0.33836(30) 0.0000 0.29549(57) 0.0150(8) Uani 0.54(11) 2 d SP . . T1A Al 0.28243(8) 0.08463(4) 0.29971(14) 0.0075(2) Uani 0.10(13) 1 d P . . T1B Si 0.28243(8) 0.08463(4) 0.29971(14) 0.0075(2) Uani 0.31(13) 1 d P . . T1C Al3+ 0.28243(8) 0.08463(4) 0.29971(14) 0.0075(2) Uani 0.15(13) 1 d P . . T1D Si4+ 0.28243(8) 0.08463(4) 0.29971(14) 0.0075(2) Uani 0.44(13) 1 d P . . T2A Si 0.29098(7) 0.17101(4) 0.80847(13) 0.0075(2) Uani 0.62(11) 1 d P . . T2B Si4+ 0.29098(7) 0.17101(4) 0.80847(13) 0.0075(2) Uani 0.38(11) 1 d P . . M1A Mg2+ 0.0000 0.08863(5) 0.5000 0.0099(3) Uani 0.652(6) 2 d SP . . M1B Fe2+ 0.0000 0.08863(5) 0.5000 0.0099(3) Uani 0.348(6) 2 d SP . . M2A Mg2+ 0.0000 0.17867(3) 0.0000 0.0089(2) Uani 0.236(5) 2 d SP . . M2B Fe3+ 0.0000 0.17867(3) 0.0000 0.0089(2) Uani 0.764(5) 2 d SP . . M3A Mg2+ 0.0000 0.0000 0.0000 0.0080(4) Uani 0.692(4) 4 d SP . . M3B Fe2+ 0.0000 0.0000 0.0000 0.0080(4) Uani 0.308(4) 4 d SP . . M4A Ca2+ 0.0000 0.27894(4) 0.5000 0.0116(3) Uani 0.808(11) 2 d SP . . M4B Na+ 0.0000 0.27894(4) 0.5000 0.0116(3) Uani 0.192(11) 2 d SP . . AM K+ 0.0240(12) 0.5000 0.0590(18) 0.0424(41) Uani 0.148(3) 2 d SP . . H H 0.188(16) 0.0000 0.846(29) 0.013 Uiso 0.36(9) 2 d SP . . M42 Fe2+ 0.0000 0.2465(24) 0.5000 0.014(8) Uiso 0.013(2) 2 d SP . . 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 0.0108(9) 0.0119(8) 0.0096(9) -0.0023(7) 0.0020(7) -0.0008(7) O1B 0.0108(9) 0.0119(8) 0.0096(9) -0.0023(7) 0.0020(7) -0.0008(7) O2A 0.0111(9) 0.0136(8) 0.0099(9) -0.0003(7) 0.0015(7) -0.0004(7) O2B 0.0111(9) 0.0136(8) 0.0099(9) -0.0003(7) 0.0015(7) -0.0004(7) O3A 0.0212(14) 0.0137(12) 0.0100(12) 0.0000 0.0035(10) 0.0000 O3B 0.0212(14) 0.0137(12) 0.0100(12) 0.0000 0.0035(10) 0.0000 O4A 0.0169(9) 0.0114(8) 0.0122(9) -0.0030(7) 0.0039(7) -0.0004(7) O4B 0.0169(9) 0.0114(8) 0.0122(9) -0.0030(7) 0.0039(7) -0.0004(7) O5A 0.0138(9) 0.0179(10) 0.0139(10) 0.0014(8) 0.0024(7) 0.0051(8) O5B 0.0138(9) 0.0179(10) 0.0139(10) 0.0014(8) 0.0024(7) 0.0051(8) O6A 0.0127(9) 0.0147(8) 0.0134(10) 0.0003(7) 0.0029(7) -0.0024(7) O6B 0.0127(9) 0.0147(8) 0.0134(10) 0.0003(7) 0.0029(7) -0.0024(7) O7A 0.0144(13) 0.0124(12) 0.0184(14) 0.0000 0.0045(11) 0.0000 O7B 0.0144(13) 0.0124(12) 0.0184(14) 0.0000 0.0045(11) 0.0000 T1A 0.0083(3) 0.0068(3) 0.0064(3) -0.0004(3) 0.0003(2) -0.0002(2) T1B 0.0083(3) 0.0068(3) 0.0064(3) -0.0004(3) 0.0003(2) -0.0002(2) T1C 0.0083(3) 0.0068(3) 0.0064(3) -0.0004(3) 0.0003(2) -0.0002(2) T1D 0.0083(3) 0.0068(3) 0.0064(3) -0.0004(3) 0.0003(2) -0.0002(2) T2A 0.0084(3) 0.0076(3) 0.0061(3) -0.0010(3) 0.0014(2) 0.0001(2) T2B 0.0084(3) 0.0076(3) 0.0061(3) -0.0010(3) 0.0014(2) 0.0001(2) M1A 0.0103(5) 0.0132(5) 0.0064(5) 0.0000 0.0024(3) 0.0000 M1B 0.0103(5) 0.0132(5) 0.0064(5) 0.0000 0.0024(3) 0.0000 M2A 0.0093(3) 0.0083(3) 0.0088(3) 0.0000 0.0019(2) 0.0000 M2B 0.0093(3) 0.0083(3) 0.0088(3) 0.0000 0.0019(2) 0.0000 M3A 0.0108(6) 0.0063(7) 0.0057(7) 0.0000 0.0000(4) 0.0000 M3B 0.0108(6) 0.0063(7) 0.0057(7) 0.0000 0.0000(4) 0.0000 M4A 0.0146(5) 0.0104(5) 0.0121(5) 0.0000 0.0076(3) 0.0000 M4B 0.0146(5) 0.0104(5) 0.0121(5) 0.0000 0.0076(3) 0.0000 AM 0.0649(73) 0.0275(28) 0.0535(79) 0.0000 0.0487(67) 0.0000 _geom_special_details ; Geometry data (distances and angles) are reported only for T, M and A sites flagged by the A suffix and for the H atom. 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 O7A 1.628(1) . ? T1A O1A 1.637(2) . ? T1A O6A 1.648(2) . ? T1A O5A 1.655(2) . ? T2A O4A 1.608(2) . ? T2A O2A 1.631(2) . ? T2A O5A 1.645(2) 1_556 ? T2A O6A 1.660(2) . ? M1A O1A 2.071(2) 6_556 ? M1A O1A 2.071(2) . ? M1A O3A 2.073(2) 5_556 ? M1A O3A 2.073(2) . ? M1A O2A 2.090(2) . ? M1A O2A 2.090(2) 6_556 ? M2A O4A 1.973(2) 7_556 ? M2A O4A 1.973(2) 4_454 ? M2A O2A 2.087(2) 1_554 ? M2A O2A 2.087(2) 6_556 ? M2A O1A 2.142(2) 6 ? M2A O1A 2.142(2) . ? M3A O3A 2.054(3) 5_556 ? M3A O3A 2.054(3) 1_554 ? M3A O1A 2.087(2) 5 ? M3A O1A 2.087(2) . ? M3A O1A 2.087(2) 2 ? M3A O1A 2.087(2) 6 ? M4A O4A 2.349(2) 4_455 ? M4A O4A 2.349(2) 7_556 ? M4A O2A 2.426(2) 6_556 ? M4A O2A 2.426(2) . ? M4A O6A 2.509(2) 7_556 ? M4A O6A 2.509(2) 4_455 ? M4A O5A 2.726(2) 7_556 ? M4A O5A 2.726(2) 4_455 ? AM O7A 2.471(10) 3_455 ? AM O7A 2.591(10) 7 ? AM O6A 2.932(7) 8_556 ? AM O6A 2.932(7) 7_556 ? AM O5A 2.986(6) 8 ? AM O5A 2.986(6) 7 ? AM O5A 3.047(7) 3_455 ? AM O5A 3.047(7) 4_455 ? AM O7A 3.349(10) 7_556 ? M42 O2A 1.988(2) 6_556 ? M42 O2A 1.988(2) . ? M42 O4A 2.294(2) 4_455 ? M42 O4A 2.294(2) 7_556 ? M42 O6A 2.962(2) 7_556 ? M42 O6A 2.962(2) 4_455 ? M42 O5A 3.095(2) 7_556 ? M42 O5A 3.095(2) 4_455 ? O3A H 0.936(3) . ? 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 O7A T1A O1A 110.8(1) . . ? O7A T1A O6A 109.6(1) . . ? O1A T1A O6A 110.3(1) . . ? O7A T1A O5A 109.2(1) . . ? O1A T1A O5A 111.2(1) . . ? O6A T1A O5A 105.7(1) . . ? O4A T2A O2A 115.9(1) . . ? O4A T2A O5A 109.7(1) . 1_556 ? O2A T2A O5A 109.1(1) . 1_556 ? O4A T2A O6A 102.9(1) . . ? O2A T2A O6A 108.4(1) . . ? O5A T2A O6A 110.6(1) 1_556 . ? O1A M1A O1A 178.7(1) 6_556 . ? O1A M1A O3A 96.2(1) 6_556 5_556 ? O1A M1A O3A 82.8(1) . 5_556 ? O1A M1A O3A 82.8(1) 6_556 . ? O1A M1A O3A 96.2(1) . . ? O3A M1A O3A 78.8(1) 5_556 . ? O1A M1A O2A 84.6(1) 6_556 . ? O1A M1A O2A 96.3(1) . . ? O3A M1A O2A 175.0(1) 5_556 . ? O3A M1A O2A 96.5(1) . . ? O1A M1A O2A 96.3(1) 6_556 6_556 ? O1A M1A O2A 84.6(1) . 6_556 ? O3A M1A O2A 96.5(1) 5_556 6_556 ? O3A M1A O2A 175.0(1) . 6_556 ? O2A M1A O2A 88.3(1) . 6_556 ? O4A M2A O4A 97.6(1) 7_556 4_454 ? O4A M2A O2A 90.5(1) 7_556 1_554 ? O4A M2A O2A 94.1(1) 4_454 1_554 ? O4A M2A O2A 94.1(1) 7_556 6_556 ? O4A M2A O2A 90.5(1) 4_454 6_556 ? O2A M2A O2A 173.0(1) 1_554 6_556 ? O4A M2A O1A 168.8(1) 7_556 6 ? O4A M2A O1A 92.0(1) 4_454 6 ? O2A M2A O1A 82.9(1) 1_554 6 ? O2A M2A O1A 91.6(1) 6_556 6 ? O4A M2A O1A 92.0(1) 7_556 . ? O4A M2A O1A 168.8(1) 4_454 . ? O2A M2A O1A 91.6(1) 1_554 . ? O2A M2A O1A 82.9(1) 6_556 . ? O1A M2A O1A 79.1(1) 6 . ? O3A M3A O3A 180.0 5_556 1_554 ? O3A M3A O1A 97.1(1) 5_556 5 ? O3A M3A O1A 82.9(1) 1_554 5 ? O3A M3A O1A 82.9(1) 5_556 . ? O3A M3A O1A 97.1(1) 1_554 . ? O1A M3A O1A 180.0 5 . ? O3A M3A O1A 82.9(1) 5_556 2 ? O3A M3A O1A 97.1(1) 1_554 2 ? O1A M3A O1A 81.6(1) 5 2 ? O1A M3A O1A 98.4(1) . 2 ? O3A M3A O1A 97.1(1) 5_556 6 ? O3A M3A O1A 82.9(1) 1_554 6 ? O1A M3A O1A 98.4(1) 5 6 ? O1A M3A O1A 81.6(1) . 6 ? O1A M3A O1A 180.0 2 6 ? O4A M4A O4A 154.8(1) 4_455 7_556 ? O4A M4A O2A 82.9(1) 4_455 6_556 ? O4A M4A O2A 77.0(1) 7_556 6_556 ? O4A M4A O2A 77.0(1) 4_455 . ? O4A M4A O2A 82.9(1) 7_556 . ? O2A M4A O2A 73.8(1) 6_556 . ? O4A M4A O6A 139.9(1) 4_455 7_556 ? O4A M4A O6A 63.4(1) 7_556 7_556 ? O2A M4A O6A 136.4(1) 6_556 7_556 ? O2A M4A O6A 116.0(1) . 7_556 ? O4A M4A O6A 63.4(1) 4_455 4_455 ? O4A M4A O6A 139.9(1) 7_556 4_455 ? O2A M4A O6A 116.0(1) 6_556 4_455 ? O2A M4A O6A 136.4(1) . 4_455 ? O6A M4A O6A 86.8(1) 7_556 4_455 ? O4A M4A O5A 84.0(1) 4_455 7_556 ? O4A M4A O5A 110.5(1) 7_556 7_556 ? O2A M4A O5A 159.6(1) 6_556 7_556 ? O2A M4A O5A 88.0(1) . 7_556 ? O6A M4A O5A 60.2(1) 7_556 7_556 ? O6A M4A O5A 71.2(1) 4_455 7_556 ? O4A M4A O5A 110.5(1) 4_455 4_455 ? O4A M4A O5A 84.0(1) 7_556 4_455 ? O2A M4A O5A 88.0(1) 6_556 4_455 ? O2A M4A O5A 159.6(1) . 4_455 ? O6A M4A O5A 71.2(1) 7_556 4_455 ? O6A M4A O5A 60.2(1) 4_455 4_455 ? O5A M4A O5A 111.3(1) 7_556 4_455 ? O7A AM O7A 164.8(5) 3_455 7 ? O7A AM O6A 86.6(2) 3_455 8_556 ? O7A AM O6A 103.4(3) 7 8_556 ? O7A AM O6A 86.6(2) 3_455 7_556 ? O7A AM O6A 103.4(3) 7 7_556 ? O6A AM O6A 95.7(3) 8_556 7_556 ? O7A AM O5A 124.6(2) 3_455 8 ? O7A AM O5A 56.8(2) 7 8 ? O6A AM O5A 54.7(1) 8_556 8 ? O6A AM O5A 130.0(4) 7_556 8 ? O7A AM O5A 124.6(2) 3_455 7 ? O7A AM O5A 56.8(2) 7 7 ? O6A AM O5A 130.0(4) 8_556 7 ? O6A AM O5A 54.7(1) 7_556 7 ? O5A AM O5A 110.9(3) 8 7 ? O7A AM O5A 56.9(2) 3_455 3_455 ? O7A AM O5A 117.9(3) 7 3_455 ? O6A AM O5A 61.3(2) 8_556 3_455 ? O6A AM O5A 135.8(4) 7_556 3_455 ? O5A AM O5A 69.3(2) 8 3_455 ? O5A AM O5A 167.1(4) 7 3_455 ? O7A AM O5A 56.9(2) 3_455 4_455 ? O7A AM O5A 117.9(3) 7 4_455 ? O6A AM O5A 135.8(4) 8_556 4_455 ? O6A AM O5A 61.3(2) 7_556 4_455 ? O5A AM O5A 167.1(4) 8 4_455 ? O5A AM O5A 69.3(2) 7 4_455 ? O5A AM O5A 107.6(3) 3_455 4_455 ? O7A AM O7A 68.5(2) 3_455 7_556 ? O7A AM O7A 126.7(3) 7 7_556 ? O6A AM O7A 49.9(2) 8_556 7_556 ? O6A AM O7A 49.9(2) 7_556 7_556 ? O5A AM O7A 101.9(2) 8 7_556 ? O5A AM O7A 101.9(2) 7 7_556 ? O5A AM O7A 90.5(2) 3_455 7_556 ? O5A AM O7A 90.5(2) 4_455 7_556 ? O2A M42 O2A 94.1(24) 6_556 . ? O2A M42 O4A 94.9(10) 6_556 4_455 ? O2A M42 O4A 87.6(9) . 4_455 ? O2A M42 O4A 87.6(9) 6_556 7_556 ? O2A M42 O4A 94.9(10) . 7_556 ? O4A M42 O4A 176.4(29) 4_455 7_556 ? O2A M42 O6A 134.5(6) 6_556 7_556 ? O2A M42 O6A 114.0(5) . 7_556 ? O4A M42 O6A 120.0(19) 4_455 7_556 ? O4A M42 O6A 56.5(8) 7_556 7_556 ? O2A M42 O6A 114.0(5) 6_556 4_455 ? O2A M42 O6A 134.5(6) . 4_455 ? O4A M42 O6A 56.5(8) 4_455 4_455 ? O4A M42 O6A 120.0(19) 7_556 4_455 ? O6A M42 O6A 71.2(13) 7_556 4_455 ? O2A M42 O5A 171.7(4) 6_556 7_556 ? O2A M42 O5A 86.9(5) . 7_556 ? O4A M42 O5A 76.9(9) 4_455 7_556 ? O4A M42 O5A 100.5(12) 7_556 7_556 ? O6A M42 O5A 51.5(8) 7_556 7_556 ? O6A M42 O5A 60.4(10) 4_455 7_556 ? O2A M42 O5A 86.9(5) 6_556 4_455 ? O2A M42 O5A 171.7(4) . 4_455 ? O4A M42 O5A 100.5(12) 4_455 4_455 ? O4A M42 O5A 76.9(9) 7_556 4_455 ? O6A M42 O5A 60.4(10) 7_556 4_455 ? O6A M42 O5A 51.5(8) 4_455 4_455 ? O5A M42 O5A 93.3(15) 7_556 4_455 ? T2A O5A T1A 136.4(1) 1_554 . ? T1A O6A T2A 139.8(1) . . ? T1A O7A T1A 140.0(2) 2 . ? O5A O6A O5A 167.6(1) . 1_556 ? O6A O7A O6A 108.5(1) . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.32 _refine_diff_density_min -0.52 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 2 0 358.4 2.9 0 4 0 940.9 6.5 0 6 0 124.3 4.3 0 8 0 4.9 2.7 0 10 0 1155.6 11.0 0 12 0 5724.0 27.4 0 14 0 50.2 4.4 0 16 0 -5.8 4.0 0 18 0 27.6 4.8 0 20 0 501.3 11.5 0 22 0 983.5 16.5 0 24 0 941.7 18.0 1 1 0 787.4 2.9 1 3 0 5.0 1.3 1 5 0 16.3 1.6 1 7 0 10.4 1.9 1 9 0 614.4 14.6 1 11 0 3257.7 23.0 1 13 0 5.2 2.6 1 15 0 44.9 3.2 1 17 0 20.2 3.0 1 19 0 38.4 3.8 1 21 0 174.0 7.3 1 23 0 58.6 4.9 1 25 0 5.4 4.3 2 0 0 153.2 3.2 2 2 0 122.8 5.2 2 4 0 1221.7 5.9 2 6 0 30.5 15.5 2 8 0 2.4 2.2 2 10 0 380.6 11.0 2 12 0 37.4 2.7 2 14 0 30.7 3.2 2 16 0 5.9 4.3 2 18 0 113.8 4.8 2 20 0 16.2 4.6 2 22 0 168.3 6.1 2 24 0 158.5 6.4 3 1 0 3673.0 19.1 3 3 0 1101.4 24.9 3 5 0 306.9 3.8 3 7 0 582.7 30.1 3 9 0 162.8 3.6 3 11 0 1765.5 30.1 3 13 0 1.1 2.6 3 15 0 4.3 2.8 3 17 0 106.4 4.6 3 19 0 247.9 6.3 3 21 0 28.7 4.4 3 23 0 302.7 8.0 4 0 0 311.0 5.8 4 2 0 39.3 2.2 4 4 0 7.3 1.9 4 6 0 1.2 2.1 4 8 0 1662.1 57.5 4 10 0 606.1 27.8 4 12 0 453.6 17.2 4 14 0 1.1 3.0 4 16 0 308.4 10.2 4 18 0 43.4 4.4 4 20 0 289.3 7.1 4 22 0 400.3 8.6 4 24 0 -1.9 4.4 5 1 0 665.7 6.1 5 3 0 293.7 4.4 5 5 0 3.3 2.1 5 7 0 109.7 3.5 5 9 0 3.0 2.6 5 11 0 11.1 2.8 5 13 0 469.9 7.7 5 15 0 163.2 9.3 5 17 0 10.5 3.6 5 19 0 1.6 3.6 5 21 0 220.0 7.0 5 23 0 193.6 6.8 6 0 0 3144.5 19.2 6 2 0 258.5 7.5 6 4 0 3.8 2.4 6 6 0 119.7 3.8 6 8 0 102.7 3.8 6 10 0 84.9 3.9 6 12 0 7.2 4.0 6 14 0 8.8 3.1 6 16 0 68.1 4.5 6 18 0 90.4 5.0 6 20 0 47.6 4.7 6 22 0 163.1 6.5 7 1 0 1049.2 11.6 7 3 0 398.0 12.5 7 5 0 -0.2 2.9 7 7 0 151.5 5.7 7 9 0 1177.6 10.5 7 11 0 3461.2 74.7 7 13 0 156.5 5.3 7 15 0 447.0 7.8 7 17 0 9.4 3.9 7 19 0 198.0 6.4 7 21 0 4.6 4.3 8 0 0 2205.2 19.3 8 2 0 116.9 7.7 8 4 0 36.9 3.5 8 6 0 28.7 3.6 8 8 0 3.7 3.0 8 10 0 144.4 12.8 8 12 0 256.5 6.4 8 14 0 -0.7 3.6 8 16 0 0.6 3.7 8 18 0 2.0 4.0 8 20 0 22.0 7.3 9 1 0 203.3 5.5 9 3 0 7.1 3.0 9 5 0 7.1 3.2 9 7 0 344.4 6.8 9 9 0 9.1 3.4 9 11 0 192.4 8.1 9 13 0 63.5 4.5 9 15 0 72.1 4.9 9 17 0 96.0 5.5 10 0 0 1711.1 20.0 10 2 0 29.5 3.9 10 4 0 3.9 4.0 10 6 0 49.6 4.6 10 8 0 588.0 11.3 10 10 0 242.1 6.7 10 12 0 837.7 14.5 10 14 0 22.2 4.2 10 16 0 132.7 9.4 11 1 0 564.6 9.0 11 3 0 47.7 4.4 11 5 0 59.2 6.6 11 7 0 2.9 3.8 11 9 0 35.2 4.3 11 11 0 709.5 10.9 11 13 0 20.0 4.6 12 0 0 11.2 5.7 12 2 0 -3.2 4.1 12 4 0 59.3 4.7 12 6 0 1.1 4.1 12 8 0 80.0 5.6 12 10 0 91.5 5.6 13 1 0 11.9 4.4 13 3 0 4.4 4.1 13 5 0 38.6 4.8 0 0 1 4.3 1.9 0 2 1 165.3 2.4 0 4 1 7.8 1.9 0 6 1 3711.1 17.0 0 8 1 115.3 3.0 0 10 1 260.3 4.4 0 12 1 245.9 4.6 0 14 1 358.2 6.1 0 16 1 751.9 19.0 0 18 1 23.1 3.2 0 20 1 5.4 3.6 0 22 1 4.8 4.0 0 24 1 4.8 4.3 1 1 1 63.0 3.9 -1 1 1 444.6 10.8 1 3 1 2648.1 72.8 -1 3 1 173.5 5.8 1 5 1 7721.5 687.1 -1 5 1 17.3 1.8 1 7 1 576.5 5.2 -1 7 1 1151.2 22.4 1 9 1 314.1 7.0 -1 9 1 941.9 21.8 1 11 1 1.9 3.5 -1 11 1 6.8 2.5 1 13 1 345.6 10.3 -1 13 1 146.3 4.2 1 15 1 265.4 7.4 -1 15 1 173.4 4.9 1 17 1 2780.7 59.7 -1 17 1 89.3 4.3 1 19 1 115.6 5.1 -1 19 1 132.0 5.3 1 21 1 451.0 8.4 -1 21 1 86.6 6.2 1 23 1 38.3 4.3 -1 23 1 83.8 5.2 1 25 1 218.6 8.5 -1 25 1 5.0 4.0 2 0 1 23.1 3.2 -2 0 1 -1.4 2.6 2 2 1 1416.9 19.5 -2 2 1 68.2 2.3 2 4 1 3.7 2.0 -2 4 1 5.7 1.9 2 6 1 4478.7 106.7 -2 6 1 18.9 5.5 2 8 1 28.7 2.3 -2 8 1 13.9 2.2 2 10 1 316.3 7.9 -2 10 1 15.8 2.4 2 12 1 104.4 7.1 -2 12 1 131.0 9.1 2 14 1 36.7 6.4 -2 14 1 878.0 8.8 2 16 1 649.9 14.2 -2 16 1 657.8 8.4 2 18 1 2.1 3.5 -2 18 1 11.9 4.6 2 20 1 11.5 3.7 -2 20 1 2.4 3.7 2 22 1 132.2 16.0 -2 22 1 30.7 4.1 2 24 1 0.7 5.0 -2 24 1 7.2 4.4 3 1 1 93.8 5.8 -3 1 1 89.6 2.5 3 3 1 288.1 4.0 -3 3 1 1977.7 73.5 3 5 1 2815.9 90.9 -3 5 1 3513.8 54.5 3 7 1 30.8 2.4 -3 7 1 173.3 5.3 3 9 1 3.9 2.4 -3 9 1 494.2 6.8 3 11 1 3.8 2.7 -3 11 1 118.5 3.9 3 13 1 97.4 13.3 -3 13 1 34.3 3.1 3 15 1 26.1 3.5 -3 15 1 105.6 4.5 3 17 1 215.0 13.7 -3 17 1 840.2 12.1 3 19 1 17.2 3.5 -3 19 1 7.4 3.8 3 21 1 2.1 4.7 -3 21 1 87.1 5.1 3 23 1 116.4 5.7 -3 23 1 71.9 6.6 4 0 1 5.5 3.0 -4 0 1 5.9 3.6 4 2 1 360.6 4.6 -4 2 1 869.9 29.8 4 4 1 29.4 6.1 -4 4 1 1.6 2.1 4 6 1 6328.2 130.2 -4 6 1 747.2 6.4 4 8 1 124.6 3.8 -4 8 1 22.5 2.5 4 10 1 107.5 5.6 -4 10 1 250.7 4.7 4 12 1 56.9 3.6 -4 12 1 72.5 3.7 4 14 1 1457.2 22.4 -4 14 1 5.4 3.3 4 16 1 1166.5 11.2 -4 16 1 463.1 7.3 4 18 1 1119.2 60.4 -4 18 1 15.2 3.7 4 20 1 75.2 5.0 -4 20 1 13.8 4.0 4 22 1 59.4 4.6 -4 22 1 44.0 5.0 -4 24 1 2.3 4.4 5 1 1 17.6 3.8 -5 1 1 72.2 2.9 5 3 1 43.4 2.8 -5 3 1 205.6 5.4 5 5 1 1791.5 43.3 -5 5 1 585.4 6.0 5 7 1 120.4 12.0 -5 7 1 150.7 6.4 5 9 1 38.9 3.2 -5 9 1 83.0 3.4 5 11 1 22.9 3.3 -5 11 1 13.8 2.8 5 13 1 4.6 3.2 -5 13 1 4.8 2.9 5 15 1 45.4 3.6 -5 15 1 3.5 3.1 5 17 1 328.4 9.9 -5 17 1 131.8 6.1 5 19 1 3.7 4.0 -5 19 1 30.3 4.3 5 21 1 1.6 4.1 -5 21 1 19.9 4.1 5 23 1 40.2 4.9 -5 23 1 71.5 5.6 6 0 1 3.8 3.6 -6 0 1 3.9 3.5 6 2 1 193.7 4.3 -6 2 1 192.7 4.4 6 4 1 9.6 2.9 -6 4 1 4.7 2.5 6 6 1 368.9 7.6 -6 6 1 8896.7 155.7 6 8 1 3.3 3.1 -6 8 1 258.6 5.1 6 10 1 24.4 3.1 -6 10 1 225.1 10.4 6 12 1 143.9 4.8 -6 12 1 114.4 11.0 6 14 1 2.7 3.4 -6 14 1 422.4 11.3 6 16 1 171.2 5.6 -6 16 1 703.8 9.3 6 18 1 736.4 19.9 -6 18 1 724.7 10.3 6 20 1 78.4 5.5 -6 20 1 44.5 4.3 6 22 1 25.6 4.9 -6 22 1 12.4 4.4 7 1 1 13.3 3.1 -7 1 1 3.8 2.8 7 3 1 376.8 6.1 -7 3 1 177.9 4.4 7 5 1 490.8 11.2 -7 5 1 3064.5 24.4 7 7 1 16.8 3.2 -7 7 1 331.5 10.8 7 9 1 6.3 5.9 -7 9 1 4.9 3.0 7 11 1 25.6 7.5 -7 11 1 2.4 3.1 7 13 1 27.1 3.9 -7 13 1 23.4 3.7 7 15 1 73.9 4.5 -7 15 1 8.1 4.6 7 17 1 310.5 11.9 -7 17 1 1168.2 20.2 7 19 1 5.3 4.1 -7 19 1 62.1 4.7 -7 21 1 52.9 5.2 8 0 1 8.7 4.7 -8 0 1 1.1 4.5 8 2 1 66.2 4.0 -8 2 1 149.6 8.2 8 4 1 2.9 7.4 -8 4 1 9.5 3.2 8 6 1 1892.2 18.9 -8 6 1 3.6 3.1 8 8 1 38.1 3.7 -8 8 1 11.3 3.1 8 10 1 77.5 4.6 -8 10 1 42.9 3.6 8 12 1 19.1 3.8 -8 12 1 63.4 4.3 8 14 1 220.8 6.4 -8 14 1 11.6 3.8 8 16 1 348.3 8.1 -8 16 1 341.5 7.4 8 18 1 113.5 7.6 -8 18 1 175.3 6.4 -8 20 1 21.0 4.6 9 1 1 0.1 3.4 -9 1 1 26.6 3.4 9 3 1 2.2 3.4 -9 3 1 197.6 5.4 9 5 1 67.0 9.0 -9 5 1 829.8 11.7 9 7 1 110.0 4.9 -9 7 1 12.8 3.6 9 9 1 50.5 6.5 -9 9 1 23.9 3.7 9 11 1 -2.2 4.0 -9 11 1 -1.0 3.6 9 13 1 5.1 4.0 -9 13 1 30.8 4.1 9 15 1 12.9 4.5 -9 15 1 1.2 3.9 9 17 1 0.8 4.3 -9 17 1 127.8 6.1 -9 19 1 1.8 4.4 10 0 1 19.3 5.2 -10 0 1 5.0 4.6 10 2 1 33.1 3.8 -10 2 1 69.3 4.3 10 4 1 64.7 4.5 -10 4 1 40.8 4.0 10 6 1 226.6 6.7 -10 6 1 1148.4 11.7 10 8 1 97.9 5.1 -10 8 1 3.9 4.3 10 10 1 41.8 4.5 -10 10 1 26.7 3.7 10 12 1 48.5 4.4 -10 12 1 38.1 4.5 10 14 1 63.7 5.1 -10 14 1 419.6 8.4 -10 16 1 495.0 19.7 11 1 1 4.9 3.8 -11 1 1 0.5 3.6 11 3 1 351.3 8.0 -11 3 1 3.2 3.6 11 5 1 1516.9 25.0 -11 5 1 5.2 3.8 11 7 1 318.5 13.3 -11 7 1 121.3 8.4 11 9 1 129.8 5.8 -11 9 1 90.5 5.2 11 11 1 -0.5 4.2 -11 11 1 15.4 4.2 -11 13 1 1.4 4.3 -11 15 1 16.7 4.6 12 0 1 48.5 6.6 -12 0 1 4.8 5.5 12 2 1 3.8 4.3 -12 2 1 73.5 5.0 12 4 1 44.8 5.1 -12 4 1 57.1 4.8 12 6 1 346.9 8.5 -12 6 1 12.5 4.3 12 8 1 -3.0 4.4 -12 8 1 71.2 4.9 -12 10 1 17.4 4.4 -12 12 1 56.7 5.0 -13 1 1 5.6 4.2 -13 3 1 254.6 7.2 -13 5 1 624.8 10.5 -13 7 1 51.3 5.2 0 0 2 294.1 5.5 0 2 2 136.3 5.7 0 4 2 9.5 2.2 0 6 2 27.4 2.2 0 8 2 29.7 2.3 0 10 2 137.5 3.9 0 12 2 1236.4 19.7 0 14 2 68.3 3.8 0 16 2 7.1 3.3 0 18 2 79.0 10.0 0 20 2 9.3 3.8 0 22 2 98.2 5.3 0 24 2 324.0 8.3 1 1 2 161.6 3.1 -1 1 2 115.7 2.9 1 3 2 6.3 2.1 -1 3 2 26.5 6.1 1 5 2 115.2 4.7 -1 5 2 181.7 4.4 1 7 2 96.7 3.0 -1 7 2 429.5 5.0 1 9 2 1223.9 38.8 -1 9 2 5.9 2.4 1 11 2 3422.9 91.3 -1 11 2 169.6 8.8 1 13 2 86.8 4.2 -1 13 2 280.7 9.4 1 15 2 242.4 8.8 -1 15 2 109.4 7.3 1 17 2 23.4 6.2 -1 17 2 36.2 3.7 1 19 2 100.5 4.8 -1 19 2 56.6 4.4 1 21 2 30.9 4.1 -1 21 2 162.3 6.0 1 23 2 180.0 12.4 -1 23 2 6.7 4.4 2 0 2 4897.8 21.0 -2 0 2 10679.1 28.5 2 2 2 133.7 3.1 -2 2 2 166.5 3.2 2 4 2 544.3 16.8 -2 4 2 635.2 16.8 2 6 2 21.8 2.6 -2 6 2 8.2 2.2 2 8 2 122.8 14.4 -2 8 2 1507.4 15.7 2 10 2 369.0 17.1 -2 10 2 949.3 14.8 2 12 2 175.2 8.8 -2 12 2 5115.2 101.3 2 14 2 6.8 3.2 -2 14 2 66.6 3.7 2 16 2 23.2 5.6 -2 16 2 163.6 5.2 2 18 2 20.6 3.9 -2 18 2 62.9 7.8 2 20 2 297.3 8.9 -2 20 2 229.5 7.0 2 22 2 395.8 8.7 -2 22 2 619.3 10.3 -2 24 2 396.3 11.7 3 1 2 10.1 2.3 -3 1 2 2212.0 9.8 3 3 2 28.8 2.5 -3 3 2 753.6 21.1 3 5 2 4.1 2.4 -3 5 2 254.1 4.0 3 7 2 185.0 6.5 -3 7 2 141.0 4.8 3 9 2 7.4 3.0 -3 9 2 265.5 5.3 3 11 2 95.9 3.9 -3 11 2 1868.4 11.3 3 13 2 347.2 15.9 -3 13 2 9.5 3.2 3 15 2 99.4 4.5 -3 15 2 14.8 3.3 3 17 2 59.1 4.3 -3 17 2 43.2 3.9 3 19 2 4.0 3.9 -3 19 2 179.2 7.0 3 21 2 171.2 9.5 -3 21 2 66.3 5.2 3 23 2 57.1 5.4 -3 23 2 163.9 6.6 4 0 2 3781.3 21.5 -4 0 2 3770.1 19.0 4 2 2 221.4 4.4 -4 2 2 142.9 3.4 4 4 2 614.0 15.2 -4 4 2 432.6 5.5 4 6 2 74.5 3.4 -4 6 2 29.6 2.6 4 8 2 233.0 9.7 -4 8 2 370.5 17.2 4 10 2 282.3 7.8 -4 10 2 286.4 5.0 4 12 2 1602.9 27.0 -4 12 2 21.2 3.4 4 14 2 55.6 4.0 -4 14 2 18.2 3.4 4 16 2 5.6 3.6 -4 16 2 103.8 4.5 4 18 2 102.0 5.1 -4 18 2 62.5 4.4 4 20 2 10.5 7.0 -4 20 2 25.4 3.9 4 22 2 262.8 7.9 -4 22 2 196.0 6.6 5 1 2 3885.9 21.8 -5 1 2 1266.3 8.7 5 3 2 1175.2 19.5 -5 3 2 6.8 2.4 5 5 2 182.3 7.7 -5 5 2 123.5 4.8 5 7 2 34.1 3.3 -5 7 2 15.8 3.4 5 9 2 421.6 13.4 -5 9 2 728.2 7.7 5 11 2 3295.7 36.3 -5 11 2 4253.8 65.2 5 13 2 173.5 12.7 -5 13 2 182.2 7.9 5 15 2 139.0 6.3 -5 15 2 197.0 5.5 5 17 2 29.8 3.9 -5 17 2 36.6 4.1 5 19 2 319.8 7.7 -5 19 2 47.4 4.3 5 21 2 13.6 4.8 -5 21 2 68.6 4.9 -5 23 2 318.8 16.3 6 0 2 884.9 12.2 -6 0 2 6065.5 28.1 6 2 2 6.5 3.0 -6 2 2 25.0 2.8 6 4 2 80.0 4.0 -6 4 2 754.2 26.5 6 6 2 36.2 3.7 -6 6 2 31.4 3.1 6 8 2 7.8 3.8 -6 8 2 388.1 13.7 6 10 2 297.8 6.3 -6 10 2 569.5 12.3 6 12 2 64.7 5.8 -6 12 2 620.3 34.6 6 14 2 6.2 3.6 -6 14 2 3.1 3.4 6 16 2 3.5 3.8 -6 16 2 95.1 4.9 6 18 2 0.5 4.3 -6 18 2 20.5 4.0 6 20 2 6.7 4.4 -6 20 2 476.6 9.2 -6 22 2 561.1 24.9 7 1 2 -0.5 3.0 -7 1 2 29.5 3.1 7 3 2 234.2 9.2 -7 3 2 153.6 4.5 7 5 2 138.5 4.8 -7 5 2 8.3 3.1 7 7 2 105.6 4.5 -7 7 2 131.6 6.7 7 9 2 -0.1 3.4 -7 9 2 11.2 3.1 7 11 2 297.3 6.8 -7 11 2 29.4 3.4 7 13 2 23.3 3.9 -7 13 2 226.3 5.6 7 15 2 31.8 4.2 -7 15 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