data_FLUORO-RICHTERITE_JAX _publ_contact_author ; Roberta Oberti ; _publ_contact_author_email ; oberti@crystal.unipv.it ; _audit_creation_method 'manually entered' _chemical_name_systematic ; ? ; _chemical_name_common ; (Ti-rich) fluoro-richterite ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0.80 Ca1.40 F1.40 Fe1.76 K0.23 Mg2.52 Na1.32 O22.60 Si7.20 Ti0.72' _chemical_formula_weight 901.36 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.082 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+' 0.082 0.0704 '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' 'Fe2+' 'Fe2+' 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' '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_ _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 9.9220(3) _cell_length_b 18.1008(5) _cell_length_c 5.2994(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.858(3) _cell_angle_gamma 90.00 _cell_volume 919.93(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.25 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886.5 _exptl_absorpt_coefficient_mu 2.90 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.82 _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_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 2740 _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 _diffrn_reflns_theta_max 30 _reflns_number_total 1400 _reflns_number_gt 1075 _reflns_threshold_expression >3\s(I) _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 'secondary isotropic' _refine_ls_extinction_coef 0.000014(2) _refine_ls_extinction_expression 'Zachariasen, 1967' _refine_ls_number_reflns 1075 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0349 _refine_ls_wR_factor_gt 0.0237 _refine_ls_restrained_S_all 1.46 _refine_ls_shift/su_max 0.10 _refine_ls_shift/su_mean 0.05 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 0.11030(18) 0.08590(9) 0.21909(34) 0.0090(5) Uani 0.31(13) 1 d P . . O1B O2- 0.11030(18) 0.08590(9) 0.21909(34) 0.0090(5) Uani 0.69(13) 1 d P . . O2A O 0.11993(18) 0.17048(9) 0.72565(33) 0.0094(5) Uani 0.37(14) 1 d P . . O2B O2- 0.11993(18) 0.17048(9) 0.72565(33) 0.0094(5) Uani 0.63(14) 1 d P . . O3A O- 0.10646(24) 0.0000 0.71302(46) 0.0129(7) Uani 0.30(5) 2 d SP . . O3B F- 0.10646(24) 0.0000 0.71302(46) 0.0129(7) Uani 0.70(5) 2 d SP . . O4A O 0.36314(19) 0.24836(10) 0.79098(37) 0.0117(5) Uani 0.47(12) 1 d P . . O4B O2- 0.36314(19) 0.24836(10) 0.79098(37) 0.0117(5) Uani 0.53(12) 1 d P . . O5A O 0.34772(19) 0.13371(10) 0.09774(38) 0.0145(5) Uani 0.22(13) 1 d P . . O5B O2- 0.34772(19) 0.13371(10) 0.09774(38) 0.0145(5) Uani 0.78(13) 1 d P . . O6A O 0.34499(19) 0.11738(10) 0.59598(36) 0.0123(5) Uani 0.12(13) 1 d P . . O6B O2- 0.34499(19) 0.11738(10) 0.59598(36) 0.0123(5) Uani 0.88(13) 1 d P . . O7A O 0.34104(27) 0.0000 0.28937(54) 0.0142(8) Uani 0.40(10) 2 d SP . . O7B O2- 0.34104(27) 0.0000 0.28937(54) 0.0142(8) Uani 0.60(10) 2 d SP . . T1A Al 0.28041(7) 0.08459(3) 0.29867(13) 0.0065(2) Uani 0.05(11) 1 d P . . T1B Si 0.28041(7) 0.08459(3) 0.29867(13) 0.0065(2) Uani 0.18(11) 1 d P . . T1C Al3+ 0.28041(7) 0.08459(3) 0.29867(13) 0.0065(2) Uani 0.15(11) 1 d P . . T1D Si4+ 0.28041(7) 0.08459(3) 0.29867(13) 0.0065(2) Uani 0.62(11) 1 d P . . T2A Si 0.28874(6) 0.17117(3) 0.80514(12) 0.0062(2) Uani 0.63(10) 1 d P . . T2B Si4+ 0.28874(6) 0.17117(3) 0.80514(12) 0.0062(2) Uani 0.37(10) 1 d P . . M1A Ti4+ 0.0000 0.08766(5) 0.5000 0.0108(3) Uani 0.360(7) 2 d SP . . M1B Fe2+ 0.0000 0.08766(5) 0.5000 0.0108(3) Uani 0.120(7) 2 d SP . . M1C Mg2+ 0.0000 0.08766(5) 0.5000 0.0108(3) Uani 0.520(7) 2 d SP . . M2A Mg2+ 0.0000 0.17868(3) 0.0000 0.0074(2) Uani 0.390(5) 2 d SP . . M2B Fe2+ 0.0000 0.17868(3) 0.0000 0.0074(2) Uani 0.610(5) 2 d SP . . M3A Mg2+ 0.0000 0.0000 0.0000 0.0078(4) Uani 0.697(3) 4 d SP . . M3B Fe2+ 0.0000 0.0000 0.0000 0.0078(4) Uani 0.303(3) 4 d SP . . M4A Na+ 0.0000 0.27751(4) 0.5000 0.0117(3) Uani 0.302(10) 2 d SP . . M4B Ca2+ 0.0000 0.27751(4) 0.5000 0.0117(3) Uani 0.698(10) 2 d SP . . A K+ 0.0000 0.5000 0.0000 0.047(3) Uani 0.230(2) 4 d SP . . AM Na+ 0.0457(6) 0.5000 0.0998(11) 0.036(2) Uani 0.356(5) 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 0.0090(7) 0.0088(7) 0.0091(8) -0.0009(6) 0.0020(6) -0.0006(6) O1B 0.0090(7) 0.0088(7) 0.0091(8) -0.0009(6) 0.0020(6) -0.0006(6) O2A 0.0085(7) 0.0101(7) 0.0092(8) -0.0008(6) 0.0014(6) -0.0006(6) O2B 0.0085(7) 0.0101(7) 0.0092(8) -0.0008(6) 0.0014(6) -0.0006(6) O3A 0.0137(11) 0.0100(10) 0.0148(12) 0.0000 0.0032(9) 0.0000 O3B 0.0137(11) 0.0100(10) 0.0148(12) 0.0000 0.0032(9) 0.0000 O4A 0.0143(8) 0.0088(7) 0.0130(9) -0.0036(6) 0.0056(6) -0.0023(6) O4B 0.0143(8) 0.0088(7) 0.0130(9) -0.0036(6) 0.0056(6) -0.0023(6) O5A 0.0097(7) 0.0201(8) 0.0137(9) 0.0011(7) 0.0028(6) 0.0066(7) O5B 0.0097(7) 0.0201(8) 0.0137(9) 0.0011(7) 0.0028(6) 0.0066(7) O6A 0.0096(7) 0.0148(8) 0.0131(9) 0.0006(7) 0.0039(6) -0.0047(7) O6B 0.0096(7) 0.0148(8) 0.0131(9) 0.0006(7) 0.0039(6) -0.0047(7) O7A 0.0133(12) 0.0081(10) 0.0205(14) 0.0000 0.0029(10) 0.0000 O7B 0.0133(12) 0.0081(10) 0.0205(14) 0.0000 0.0029(10) 0.0000 T1A 0.0066(3) 0.0055(2) 0.0071(3) -0.0007(3) 0.0012(2) -0.0004(2) T1B 0.0066(3) 0.0055(2) 0.0071(3) -0.0007(3) 0.0012(2) -0.0004(2) T1C 0.0066(3) 0.0055(2) 0.0071(3) -0.0007(3) 0.0012(2) -0.0004(2) T1D 0.0066(3) 0.0055(2) 0.0071(3) -0.0007(3) 0.0012(2) -0.0004(2) T2A 0.0059(3) 0.0061(2) 0.0065(3) -0.0010(3) 0.0015(2) 0.0000(2) T2B 0.0059(3) 0.0061(2) 0.0065(3) -0.0010(3) 0.0015(2) 0.0000(2) M1A 0.0109(4) 0.0129(3) 0.0092(5) 0.0000 0.0035(3) 0.0000 M1B 0.0109(4) 0.0129(3) 0.0092(5) 0.0000 0.0035(3) 0.0000 M1C 0.0109(4) 0.0129(3) 0.0092(5) 0.0000 0.0035(3) 0.0000 M2A 0.0075(3) 0.0061(3) 0.0089(3) 0.0000 0.0029(2) 0.0000 M2B 0.0075(3) 0.0061(3) 0.0089(3) 0.0000 0.0029(2) 0.0000 M3A 0.0095(6) 0.0051(5) 0.0079(6) 0.0000 0.0009(4) 0.0000 M3B 0.0095(6) 0.0051(5) 0.0079(6) 0.0000 0.0009(4) 0.0000 M4A 0.0144(5) 0.0081(3) 0.0154(5) 0.0000 0.0089(3) 0.0000 M4B 0.0144(5) 0.0081(3) 0.0154(5) 0.0000 0.0089(3) 0.0000 A 0.0349(37) 0.0805(55) 0.0364(39) 0.0000 0.0283(33) 0.0000 AM 0.0371(34) 0.0437(33) 0.0351(33) 0.0000 0.0213(26) 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 O1A 1.632(2) . ? T1A O7A 1.650(1) . ? T1A O6A 1.652(2) . ? T1A O5A 1.654(2) . ? T2A O4A 1.591(2) . ? T2A O2A 1.619(2) . ? T2A O5A 1.656(2) 1_556 ? T2A O6A 1.675(2) . ? M1A O1A 2.062(2) . ? M1A O1A 2.062(2) 6_556 ? M1A O3A 2.073(2) 5_556 ? M1A O3A 2.073(2) . ? M1A O2A 2.089(2) . ? M1A O2A 2.089(2) 6_556 ? M2A O4A 2.011(2) 7_556 ? M2A O4A 2.011(2) 4_454 ? M2A O2A 2.107(2) 6_556 ? M2A O2A 2.107(2) 1_554 ? M2A O1A 2.171(2) 6 ? M2A O1A 2.171(2) . ? M3A O3A 2.062(2) 1_554 ? M3A O3A 2.062(2) 5_556 ? M3A O1A 2.077(2) . ? M3A O1A 2.077(2) 5 ? M3A O1A 2.077(2) 2 ? M3A O1A 2.077(2) 6 ? M4A O4A 2.348(2) 4_455 ? M4A O4A 2.348(2) 7_556 ? M4A O2A 2.423(2) 6_556 ? M4A O2A 2.423(2) . ? M4A O6A 2.578(2) 7_556 ? M4A O6A 2.578(2) 4_455 ? M4A O5A 2.785(2) 7_556 ? M4A O5A 2.785(2) 4_455 ? A O7A 2.466(3) 7 ? A O7A 2.466(3) 3_455 ? A O5A 2.968(2) 8 ? A O5A 2.968(2) 3_455 ? A O5A 2.968(2) 4_455 ? A O5A 2.968(2) 7 ? A O6A 3.127(2) 8_556 ? A O6A 3.127(2) 4_454 ? A O6A 3.127(2) 3_454 ? A O6A 3.127(2) 7_556 ? AM O7A 2.486(3) 3_455 ? AM O7A 2.590(3) 7 ? AM O6A 2.719(2) 8_556 ? AM O6A 2.719(2) 7_556 ? AM O5A 2.939(2) 8 ? AM O5A 2.939(2) 7 ? AM O5A 3.115(2) 4_455 ? AM O5A 3.115(2) 3_455 ? AM O7A 3.143(3) 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 O7A 111.5(1) . . ? O1A T1A O6A 111.3(1) . . ? O7A T1A O6A 107.9(1) . . ? O1A T1A O5A 112.8(1) . . ? O7A T1A O5A 105.6(1) . . ? O6A T1A O5A 107.4(1) . . ? O4A T2A O2A 117.1(1) . . ? O4A T2A O5A 110.3(1) . 1_556 ? O2A T2A O5A 109.5(1) . 1_556 ? O4A T2A O6A 104.0(1) . . ? O2A T2A O6A 108.7(1) . . ? O5A T2A O6A 106.5(1) 1_556 . ? O1A M1A O1A 178.2(1) . 6_556 ? O1A M1A O3A 83.4(1) . 5_556 ? O1A M1A O3A 95.2(1) 6_556 5_556 ? O1A M1A O3A 95.2(1) . . ? O1A M1A O3A 83.4(1) 6_556 . ? O3A M1A O3A 80.1(1) 5_556 . ? O1A M1A O2A 95.4(1) . . ? O1A M1A O2A 85.9(1) 6_556 . ? O3A M1A O2A 175.6(1) 5_556 . ? O3A M1A O2A 95.8(1) . . ? O1A M1A O2A 85.9(1) . 6_556 ? O1A M1A O2A 95.4(1) 6_556 6_556 ? O3A M1A O2A 95.8(1) 5_556 6_556 ? O3A M1A O2A 175.6(1) . 6_556 ? O2A M1A O2A 88.3(1) . 6_556 ? O4A M2A O4A 97.9(1) 7_556 4_454 ? O4A M2A O2A 95.0(1) 7_556 6_556 ? O4A M2A O2A 90.3(1) 4_454 6_556 ? O4A M2A O2A 90.3(1) 7_556 1_554 ? O4A M2A O2A 95.0(1) 4_454 1_554 ? O2A M2A O2A 171.9(1) 6_556 1_554 ? O4A M2A O1A 168.3(1) 7_556 6 ? O4A M2A O1A 92.1(1) 4_454 6 ? O2A M2A O1A 91.0(1) 6_556 6 ? O2A M2A O1A 82.7(1) 1_554 6 ? O4A M2A O1A 92.1(1) 7_556 . ? O4A M2A O1A 168.3(1) 4_454 . ? O2A M2A O1A 82.7(1) 6_556 . ? O2A M2A O1A 91.0(1) 1_554 . ? O1A M2A O1A 78.7(1) 6 . ? O3A M3A O3A 180.0 1_554 5_556 ? O3A M3A O1A 96.7(1) 1_554 . ? O3A M3A O1A 83.3(1) 5_556 . ? O3A M3A O1A 83.3(1) 1_554 5 ? O3A M3A O1A 96.7(1) 5_556 5 ? O1A M3A O1A 180.0 . 5 ? O3A M3A O1A 96.7(1) 1_554 2 ? O3A M3A O1A 83.3(1) 5_556 2 ? O1A M3A O1A 97.0(1) . 2 ? O1A M3A O1A 83.0(1) 5 2 ? O3A M3A O1A 83.3(1) 1_554 6 ? O3A M3A O1A 96.7(1) 5_556 6 ? O1A M3A O1A 83.0(1) . 6 ? O1A M3A O1A 97.0(1) 5 6 ? O1A M3A O1A 180.0 2 6 ? O4A M4A O4A 157.0(1) 4_455 7_556 ? O4A M4A O2A 82.6(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 82.6(1) 7_556 . ? O2A M4A O2A 73.8(1) 6_556 . ? O4A M4A O6A 138.7(1) 4_455 7_556 ? O4A M4A O6A 62.8(1) 7_556 7_556 ? O2A M4A O6A 137.3(1) 6_556 7_556 ? O2A M4A O6A 116.4(1) . 7_556 ? O4A M4A O6A 62.8(1) 4_455 4_455 ? O4A M4A O6A 138.7(1) 7_556 4_455 ? O2A M4A O6A 116.4(1) 6_556 4_455 ? O2A M4A O6A 137.3(1) . 4_455 ? O6A M4A O6A 84.9(1) 7_556 4_455 ? O4A M4A O5A 84.5(1) 4_455 7_556 ? O4A M4A O5A 109.0(1) 7_556 7_556 ? O2A M4A O5A 160.1(1) 6_556 7_556 ? O2A M4A O5A 89.0(1) . 7_556 ? O6A M4A O5A 59.4(1) 7_556 7_556 ? O6A M4A O5A 70.0(1) 4_455 7_556 ? O4A M4A O5A 109.0(1) 4_455 4_455 ? O4A M4A O5A 84.5(1) 7_556 4_455 ? O2A M4A O5A 89.0(1) 6_556 4_455 ? O2A M4A O5A 160.1(1) . 4_455 ? O6A M4A O5A 70.0(1) 7_556 4_455 ? O6A M4A O5A 59.4(1) 4_455 4_455 ? O5A M4A O5A 109.5(1) 7_556 4_455 ? O7A A O7A 180.0 7 3_455 ? O7A A O5A 57.05(4) 7 8 ? O7A A O5A 122.95(4) 3_455 8 ? O7A A O5A 122.95(4) 7 3_455 ? O7A A O5A 57.05(4) 3_455 3_455 ? O5A A O5A 70.7(1) 8 3_455 ? O7A A O5A 122.95(4) 7 4_455 ? O7A A O5A 57.05(4) 3_455 4_455 ? O5A A O5A 180.0 8 4_455 ? O5A A O5A 109.3(1) 3_455 4_455 ? O7A A O5A 57.05(4) 7 7 ? O7A A O5A 122.95(4) 3_455 7 ? O5A A O5A 109.3(1) 8 7 ? O5A A O5A 180.0 3_455 7 ? O5A A O5A 70.7(1) 4_455 7 ? O7A A O6A 98.3(1) 7 8_556 ? O7A A O6A 81.7(1) 3_455 8_556 ? O5A A O6A 51.9(1) 8 8_556 ? O5A A O6A 60.6(1) 3_455 8_556 ? O5A A O6A 128.1(1) 4_455 8_556 ? O5A A O6A 119.4(1) 7 8_556 ? O7A A O6A 81.7(1) 7 4_454 ? O7A A O6A 98.3(1) 3_455 4_454 ? O5A A O6A 128.1(1) 8 4_454 ? O5A A O6A 119.4(1) 3_455 4_454 ? O5A A O6A 51.9(1) 4_455 4_454 ? O5A A O6A 60.6(1) 7 4_454 ? O6A A O6A 180.0 8_556 4_454 ? O7A A O6A 81.7(1) 7 3_454 ? O7A A O6A 98.3(1) 3_455 3_454 ? O5A A O6A 60.6(1) 8 3_454 ? O5A A O6A 51.9(1) 3_455 3_454 ? O5A A O6A 119.4(1) 4_455 3_454 ? O5A A O6A 128.1(1) 7 3_454 ? O6A A O6A 94.4(1) 8_556 3_454 ? O6A A O6A 85.6(1) 4_454 3_454 ? O7A A O6A 98.3(1) 7 7_556 ? O7A A O6A 81.7(1) 3_455 7_556 ? O5A A O6A 119.4(1) 8 7_556 ? O5A A O6A 128.1(1) 3_455 7_556 ? O5A A O6A 60.6(1) 4_455 7_556 ? O5A A O6A 51.9(1) 7 7_556 ? O6A A O6A 85.6(1) 8_556 7_556 ? O6A A O6A 94.4(1) 4_454 7_556 ? O6A A O6A 180.0 3_454 7_556 ? O7A AM O7A 152.7(1) 3_455 7 ? O7A AM O6A 90.2(1) 3_455 8_556 ? O7A AM O6A 106.5(1) 7 8_556 ? O7A AM O6A 90.2(1) 3_455 7_556 ? O7A AM O6A 106.5(1) 7 7_556 ? O6A AM O6A 102.8(1) 8_556 7_556 ? O7A AM O5A 123.4(1) 3_455 8 ? O7A AM O5A 56.4(1) 7 8 ? O6A AM O5A 56.1(1) 8_556 8 ? O6A AM O5A 136.8(1) 7_556 8 ? O7A AM O5A 123.4(1) 3_455 7 ? O7A AM O5A 56.4(1) 7 7 ? O6A AM O5A 136.8(1) 8_556 7 ? O6A AM O5A 56.1(1) 7_556 7 ? O5A AM O5A 110.8(1) 8 7 ? O7A AM O5A 54.7(1) 3_455 4_455 ? O7A AM O5A 113.5(1) 7 4_455 ? O6A AM O5A 139.9(1) 8_556 4_455 ? O6A AM O5A 63.3(1) 7_556 4_455 ? O5A AM O5A 157.3(1) 8 4_455 ? O5A AM O5A 69.1(1) 7 4_455 ? O7A AM O5A 54.7(1) 3_455 3_455 ? O7A AM O5A 113.5(1) 7 3_455 ? O6A AM O5A 63.3(1) 8_556 3_455 ? O6A AM O5A 139.9(1) 7_556 3_455 ? O5A AM O5A 69.1(1) 8 3_455 ? O5A AM O5A 157.3(1) 7 3_455 ? O5A AM O5A 102.0(1) 4_455 3_455 ? O7A AM O7A 72.4(1) 3_455 7_556 ? O7A AM O7A 135.0(1) 7 7_556 ? O6A AM O7A 53.6(1) 8_556 7_556 ? O6A AM O7A 53.6(1) 7_556 7_556 ? O5A AM O7A 107.5(1) 8 7_556 ? O5A AM O7A 107.5(1) 7 7_556 ? O5A AM O7A 93.6(1) 4_455 7_556 ? O5A AM O7A 93.6(1) 3_455 7_556 ? T1A O5A T2A 136.0(1) . 1_554 ? T1A O6A T2A 136.6(1) . . ? T1A O7A T1A 136.2(1) 2 . ? O5A O6A O5A 167.2(1) . 1_556 ? O6A O7A O6A 105.5(1) . 2 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.69 _refine_diff_density_min -0.41 _refine_diff_density_rms 0.099 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 2 0 117.6 1.4 0 4 0 674.5 4.8 0 6 0 68.6 2.1 0 8 0 22.2 1.6 0 10 0 1092.9 9.7 0 12 0 5970.7 25.0 0 14 0 35.9 2.7 0 16 0 1.6 2.6 0 18 0 50.4 3.7 0 20 0 504.2 10.3 0 22 0 868.2 14.5 0 24 0 913.2 16.3 1 1 0 459.0 9.6 1 3 0 1.3 1.2 1 5 0 3.3 0.9 1 7 0 26.4 1.2 1 9 0 763.3 5.5 1 11 0 2569.9 30.5 1 13 0 6.2 1.5 1 15 0 11.6 2.9 1 17 0 0.3 1.8 1 19 0 34.0 3.0 1 21 0 103.3 3.7 1 23 0 66.2 3.4 1 25 0 0.0 2.6 2 0 0 61.6 1.6 2 2 0 24.8 0.8 2 4 0 1264.1 10.8 2 6 0 36.5 1.9 2 8 0 8.4 0.9 2 10 0 295.2 3.8 2 12 0 37.1 1.7 2 14 0 62.8 5.8 2 16 0 9.3 1.8 2 18 0 79.2 3.4 2 20 0 12.0 2.4 2 22 0 157.3 8.1 2 24 0 157.2 12.0 3 1 0 2823.9 14.5 3 3 0 898.4 12.3 3 5 0 367.9 8.7 3 7 0 371.1 3.9 3 9 0 78.1 2.1 3 11 0 1408.1 28.6 3 13 0 3.9 1.6 3 15 0 2.9 1.7 3 17 0 95.5 3.3 3 19 0 174.6 4.4 3 21 0 9.3 2.9 3 23 0 251.2 5.9 4 0 0 226.0 4.0 4 2 0 16.1 1.0 4 4 0 7.6 1.4 4 6 0 0.9 1.2 4 8 0 1449.9 28.5 4 10 0 473.1 5.3 4 12 0 455.3 5.6 4 14 0 3.2 1.7 4 16 0 267.4 8.0 4 18 0 20.3 2.1 4 20 0 275.2 6.3 4 22 0 403.3 23.9 4 24 0 0.2 2.6 5 1 0 577.7 5.8 5 3 0 230.2 3.3 5 5 0 4.7 1.7 5 7 0 78.2 2.2 5 9 0 -0.9 1.5 5 11 0 9.8 3.0 5 13 0 404.2 10.9 5 15 0 173.3 4.1 5 17 0 5.3 2.2 5 19 0 -1.2 2.4 5 21 0 190.4 5.2 5 23 0 175.5 8.4 6 0 0 2099.4 14.5 6 2 0 178.8 3.4 6 4 0 6.9 2.8 6 6 0 58.5 2.1 6 8 0 152.2 5.5 6 10 0 56.9 3.0 6 12 0 0.7 1.8 6 14 0 4.6 5.8 6 16 0 71.0 3.1 6 18 0 78.8 3.3 6 20 0 30.1 3.8 6 22 0 91.9 4.3 7 1 0 817.2 7.2 7 3 0 321.1 4.7 7 5 0 0.3 1.5 7 7 0 108.2 3.0 7 9 0 1056.6 12.4 7 11 0 2908.2 15.6 7 13 0 163.3 4.1 7 15 0 294.3 5.7 7 17 0 2.5 2.6 7 19 0 143.0 4.6 7 21 0 -1.9 2.8 8 0 0 1769.9 15.9 8 2 0 42.6 2.1 8 4 0 18.5 1.7 8 6 0 26.2 1.9 8 8 0 1.6 2.0 8 10 0 116.4 3.6 8 12 0 291.5 5.6 8 14 0 1.0 3.0 8 16 0 -0.1 2.4 8 18 0 -3.4 2.6 8 20 0 24.2 2.7 9 1 0 154.3 3.8 9 3 0 12.9 1.8 9 5 0 2.9 2.2 9 7 0 286.6 5.4 9 9 0 24.3 2.3 9 11 0 140.0 4.2 9 13 0 46.1 2.8 9 15 0 106.3 3.9 9 17 0 77.5 3.6 9 19 0 0.9 2.7 10 0 0 1043.0 14.3 10 2 0 15.1 2.0 10 4 0 1.8 2.1 10 6 0 49.7 2.7 10 8 0 525.2 7.8 10 10 0 164.2 4.6 10 12 0 653.4 9.1 10 14 0 6.6 2.5 10 16 0 108.6 6.3 11 1 0 529.7 7.9 11 3 0 47.0 2.9 11 5 0 50.6 2.9 11 7 0 2.0 2.2 11 9 0 32.3 2.8 11 11 0 692.0 11.6 11 13 0 29.8 2.9 12 0 0 3.1 3.3 12 2 0 6.3 2.5 12 4 0 36.8 2.7 12 6 0 0.0 2.6 12 8 0 80.3 3.8 12 10 0 78.4 5.8 13 1 0 42.9 9.6 13 3 0 10.9 2.9 13 5 0 41.4 4.7 13 7 0 0.0 2.9 0 0 1 9.2 0.8 0 2 1 61.3 3.1 0 4 1 22.2 0.9 0 6 1 3280.3 45.0 0 8 1 32.5 1.3 0 10 1 156.4 2.8 0 12 1 135.8 3.8 0 14 1 245.8 7.3 0 16 1 680.5 17.7 0 18 1 18.6 1.8 0 20 1 -0.4 2.3 0 22 1 6.5 2.5 0 24 1 -2.9 2.7 1 1 1 98.8 4.5 -1 1 1 207.1 1.8 1 3 1 2290.1 57.7 -1 3 1 170.0 1.9 1 5 1 5387.2 81.6 -1 5 1 84.6 3.4 1 7 1 463.8 4.1 -1 7 1 1111.3 26.7 1 9 1 262.0 6.5 -1 9 1 771.6 16.8 1 11 1 6.9 1.5 -1 11 1 -0.2 1.8 1 13 1 288.0 4.4 -1 13 1 131.0 3.1 1 15 1 357.4 10.8 -1 15 1 155.2 6.0 1 17 1 2343.7 68.8 -1 17 1 87.2 8.5 1 19 1 138.1 3.9 -1 19 1 127.6 3.8 1 21 1 311.6 18.9 -1 21 1 100.0 7.7 1 23 1 10.6 2.7 -1 23 1 67.4 3.5 1 25 1 178.1 8.8 -1 25 1 -0.4 3.7 2 0 1 6.3 1.0 -2 0 1 12.2 1.0 2 2 1 1166.3 35.1 -2 2 1 15.1 1.4 2 4 1 10.7 1.5 -2 4 1 4.0 0.9 2 6 1 4010.2 106.4 -2 6 1 15.2 1.1 2 8 1 5.8 1.3 -2 8 1 -1.4 1.9 2 10 1 275.6 3.9 -2 10 1 -1.3 1.3 2 12 1 60.0 3.1 -2 12 1 125.6 3.3 2 14 1 39.2 6.5 -2 14 1 666.6 30.6 2 16 1 465.4 11.0 -2 16 1 515.4 6.6 2 18 1 5.5 3.4 -2 18 1 7.9 2.0 2 20 1 17.6 2.5 -2 20 1 11.4 2.4 2 22 1 81.5 3.7 -2 22 1 43.1 3.0 2 24 1 -0.4 2.4 -2 24 1 2.4 4.6 3 1 1 64.1 1.6 -3 1 1 131.4 2.6 3 3 1 205.5 11.4 -3 3 1 1704.0 28.8 3 5 1 1810.8 33.3 -3 5 1 2877.6 29.4 3 7 1 28.1 1.4 -3 7 1 154.2 7.5 3 9 1 8.1 1.2 -3 9 1 435.9 14.6 3 11 1 1.1 1.5 -3 11 1 152.0 9.9 3 13 1 90.2 2.7 -3 13 1 41.2 2.0 3 15 1 18.5 2.0 -3 15 1 84.1 2.8 3 17 1 177.1 4.7 -3 17 1 822.1 16.7 3 19 1 15.3 2.2 -3 19 1 0.9 3.6 3 21 1 10.5 2.5 -3 21 1 63.4 3.9 3 23 1 85.0 3.9 -3 23 1 60.0 3.5 4 0 1 0.8 1.6 -4 0 1 9.2 1.5 4 2 1 311.0 3.7 -4 2 1 873.8 19.2 4 4 1 27.1 1.4 -4 4 1 1.4 1.2 4 6 1 5183.8 83.6 -4 6 1 795.3 15.8 4 8 1 74.8 3.3 -4 8 1 4.8 1.6 4 10 1 66.5 2.3 -4 10 1 272.8 11.5 4 12 1 48.5 2.3 -4 12 1 54.4 4.1 4 14 1 1219.8 10.1 -4 14 1 1.1 1.7 4 16 1 797.6 8.7 -4 16 1 335.5 13.4 4 18 1 935.3 30.0 -4 18 1 7.7 2.2 4 20 1 18.9 2.7 -4 20 1 25.2 2.4 4 22 1 79.0 3.8 -4 22 1 27.6 2.5 -4 24 1 -0.2 3.2 5 1 1 7.4 1.1 -5 1 1 39.1 1.5 5 3 1 28.6 1.5 -5 3 1 177.4 2.8 5 5 1 1490.5 9.0 -5 5 1 318.3 4.0 5 7 1 141.2 3.0 -5 7 1 161.9 7.1 5 9 1 28.1 1.7 -5 9 1 80.0 3.4 5 11 1 16.5 1.7 -5 11 1 6.9 1.5 5 13 1 0.4 1.9 -5 13 1 10.4 3.2 5 15 1 31.7 2.3 -5 15 1 5.9 1.9 5 17 1 352.8 6.3 -5 17 1 97.3 3.5 5 19 1 6.9 2.5 -5 19 1 16.8 2.3 5 21 1 0.1 2.5 -5 21 1 5.5 2.4 5 23 1 39.6 4.8 -5 23 1 23.4 2.8 6 0 1 2.3 2.0 -6 0 1 4.0 1.8 6 2 1 157.2 3.2 -6 2 1 126.1 11.3 6 4 1 5.3 1.6 -6 4 1 2.2 1.4 6 6 1 421.3 5.3 -6 6 1 7666.4 115.2 6 8 1 3.4 1.8 -6 8 1 138.5 5.1 6 10 1 21.3 2.0 -6 10 1 143.6 8.3 6 12 1 60.0 2.7 -6 12 1 74.6 3.7 6 14 1 12.1 5.2 -6 14 1 326.0 20.3 6 16 1 132.4 4.0 -6 16 1 605.6 42.3 6 18 1 723.0 9.6 -6 18 1 644.0 36.1 6 20 1 71.0 3.6 -6 20 1 28.6 2.5 6 22 1 18.2 2.9 -6 22 1 13.0 2.7 7 1 1 16.2 1.7 -7 1 1 -1.0 1.4 7 3 1 200.6 3.9 -7 3 1 168.8 3.3 7 5 1 286.3 4.8 -7 5 1 2649.8 75.8 7 7 1 22.3 2.0 -7 7 1 366.4 8.7 7 9 1 3.4 1.9 -7 9 1 -0.7 1.7 7 11 1 23.5 1.9 -7 11 1 0.7 1.9 7 13 1 13.8 4.5 -7 13 1 20.1 6.6 7 15 1 64.1 5.3 -7 15 1 15.7 2.2 7 17 1 201.1 6.1 -7 17 1 1126.3 52.1 7 19 1 -2.1 5.8 -7 19 1 86.1 3.7 7 21 1 55.0 4.7 -7 21 1 29.4 2.7 8 0 1 6.7 3.0 -8 0 1 1.3 2.1 8 2 1 65.3 2.6 -8 2 1 112.2 3.0 8 4 1 3.2 1.9 -8 4 1 20.9 1.7 8 6 1 1705.0 12.2 -8 6 1 14.8 1.6 8 8 1 40.4 2.3 -8 8 1 14.3 1.9 8 10 1 60.0 3.3 -8 10 1 40.5 3.4 8 12 1 2.4 2.2 -8 12 1 35.0 4.2 8 14 1 176.6 6.4 -8 14 1 12.6 2.4 8 16 1 294.0 6.4 -8 16 1 236.1 8.6 8 18 1 127.0 4.4 -8 18 1 174.6 6.0 -8 20 1 48.8 3.2 9 1 1 2.7 2.0 -9 1 1 24.7 1.9 9 3 1 3.2 2.1 -9 3 1 98.2 3.1 9 5 1 62.4 2.8 -9 5 1 545.2 19.6 9 7 1 52.7 2.7 -9 7 1 12.0 2.1 9 9 1 43.5 2.7 -9 9 1 6.9 2.7 9 11 1 6.9 2.4 -9 11 1 2.2 2.7 9 13 1 7.4 3.0 -9 13 1 25.6 2.3 9 15 1 6.9 2.9 -9 15 1 3.3 2.4 9 17 1 9.1 3.9 -9 17 1 89.3 8.3 -9 19 1 5.2 2.8 10 0 1 12.1 3.6 -10 0 1 3.8 2.6 10 2 1 52.2 2.7 -10 2 1 81.6 5.1 10 4 1 39.6 3.8 -10 4 1 28.6 2.4 10 6 1 118.4 4.0 -10 6 1 974.6 29.3 10 8 1 61.2 3.3 -10 8 1 10.6 2.1 10 10 1 64.6 3.3 -10 10 1 33.1 8.4 10 12 1 42.3 2.9 -10 12 1 18.7 2.4 10 14 1 28.5 2.9 -10 14 1 379.1 7.3 -10 16 1 355.8 18.9 11 1 1 6.9 2.4 -11 1 1 -1.2 2.0 11 3 1 301.1 6.3 -11 3 1 2.0 4.3 11 5 1 1335.4 13.0 -11 5 1 3.2 2.2 11 7 1 320.6 8.9 -11 7 1 94.8 4.3 11 9 1 107.0 4.6 -11 9 1 74.5 3.5 11 11 1 0.3 3.1 -11 11 1 18.4 2.5 11 13 1 3.6 2.9 -11 13 1 5.9 2.7 -11 15 1 14.9 8.7 12 0 1 32.3 3.9 -12 0 1 1.8 3.2 12 2 1 17.3 5.4 -12 2 1 94.5 8.1 12 4 1 50.8 3.2 -12 4 1 47.1 3.0 12 6 1 412.5 10.7 -12 6 1 5.3 2.5 12 8 1 -2.7 4.2 -12 8 1 56.1 3.8 -12 10 1 31.7 2.9 -12 12 1 32.5 3.2 -13 1 1 8.1 3.2 -13 3 1 220.9 8.5 -13 5 1 554.7 9.1 -13 7 1 49.8 5.6 -13 9 1 41.4 3.9 0 0 2 355.3 4.8 0 2 2 55.3 2.8 0 4 2 16.4 1.0 0 6 2 14.5 1.8 0 8 2 54.9 2.6 0 10 2 106.6 2.6 0 12 2 1108.8 15.9 0 14 2 46.6 2.2 0 16 2 8.6 1.9 0 18 2 63.8 2.9 0 20 2 7.3 2.3 0 22 2 83.1 3.7 0 24 2 324.1 19.0 1 1 2 77.3 3.4 -1 1 2 64.8 1.5 1 3 2 4.7 1.3 -1 3 2 21.8 1.1 1 5 2 114.4 2.3 -1 5 2 169.8 5.5 1 7 2 83.2 2.4 -1 7 2 270.0 6.6 1 9 2 882.0 17.1 -1 9 2 1.5 1.4 1 11 2 2403.9 23.0 -1 11 2 129.6 3.0 1 13 2 84.5 2.7 -1 13 2 250.1 14.1 1 15 2 115.0 3.3 -1 15 2 102.1 3.1 1 17 2 6.5 2.0 -1 17 2 26.0 2.0 1 19 2 83.2 10.2 -1 19 2 21.7 2.2 1 21 2 40.4 2.8 -1 21 2 103.3 4.0 1 23 2 163.1 14.6 -1 23 2 0.0 4.1 2 0 2 4103.6 17.7 -2 0 2 7263.9 80.1 2 2 2 71.3 1.8 -2 2 2 95.7 2.1 2 4 2 413.0 18.3 -2 4 2 610.6 28.7 2 6 2 1.7 1.3 -2 6 2 19.2 1.3 2 8 2 78.9 2.2 -2 8 2 1134.1 38.0 2 10 2 288.7 4.3 -2 10 2 610.1 24.4 2 12 2 164.9 3.5 -2 12 2 4448.5 165.9 2 14 2 0.6 1.9 -2 14 2 23.8 1.8 2 16 2 19.5 1.8 -2 16 2 132.5 9.5 2 18 2 13.9 2.1 -2 18 2 30.6 3.3 2 20 2 280.9 13.6 -2 20 2 228.6 9.9 2 22 2 316.8 17.3 -2 22 2 586.4 11.3 -2 24 2 346.7 16.8 3 1 2 7.4 0.9 -3 1 2 1591.2 7.3 3 3 2 33.0 1.5 -3 3 2 706.3 8.8 3 5 2 2.7 1.4 -3 5 2 332.0 10.7 3 7 2 142.7 2.9 -3 7 2 63.2 2.2 3 9 2 0.4 1.9 -3 9 2 267.0 9.0 3 11 2 54.7 2.3 -3 11 2 1418.9 47.8 3 13 2 235.1 5.8 -3 13 2 8.9 1.7 3 15 2 112.8 3.5 -3 15 2 0.7 1.8 3 17 2 17.5 2.3 -3 17 2 9.7 2.2 3 19 2 -3.2 2.2 -3 19 2 123.1 5.2 3 21 2 120.2 4.2 -3 21 2 18.9 2.2 3 23 2 48.4 3.5 -3 23 2 149.5 9.2 4 0 2 2448.9 16.1 -4 0 2 3302.6 16.0 4 2 2 154.4 3.0 -4 2 2 25.1 1.2 4 4 2 555.8 8.6 -4 4 2 476.5 4.6 4 6 2 40.1 2.1 -4 6 2 25.1 3.3 4 8 2 134.6 3.5 -4 8 2 421.1 12.1 4 10 2 137.3 3.5 -4 10 2 230.2 16.1 4 12 2 1198.6 9.9 -4 12 2 29.0 6.6 4 14 2 19.6 1.8 -4 14 2 21.5 2.7 4 16 2 0.4 2.1 -4 16 2 104.1 9.7 4 18 2 56.6 4.3 -4 18 2 67.0 4.4 4 20 2 5.9 2.8 -4 20 2 21.1 2.3 4 22 2 213.1 8.2 -4 22 2 162.3 9.4 5 1 2 3234.3 30.7 -5 1 2 793.7 10.7 5 3 2 899.9 9.8 -5 3 2 10.4 1.2 5 5 2 134.4 4.0 -5 5 2 84.2 6.4 5 7 2 18.7 1.6 -5 7 2 24.0 1.5 5 9 2 300.9 6.1 -5 9 2 730.3 18.9 5 11 2 2822.1 15.3 -5 11 2 3109.2 130.7 5 13 2 153.0 4.0 -5 13 2 185.0 12.5 5 15 2 90.6 3.3 -5 15 2 104.2 9.4 5 17 2 22.1 4.0 -5 17 2 12.9 2.3 5 19 2 206.2 7.3 -5 19 2 42.7 2.8 5 21 2 -1.0 2.8 -5 21 2 48.3 4.8 -5 23 2 302.0 12.4 6 0 2 721.9 10.3 -6 0 2 5471.2 23.8 6 2 2 1.5 1.7 -6 2 2 1.7 1.4 6 4 2 24.1 9.2 -6 4 2 611.0 20.6 6 6 2 23.7 1.8 -6 6 2 11.0 2.0 6 8 2 10.7 2.2 -6 8 2 287.7 10.5 6 10 2 204.2 4.5 -6 10 2 540.3 7.2 6 12 2 88.0 3.3 -6 12 2 572.2 7.0 6 14 2 6.0 2.4 -6 14 2 1.5 1.9 6 16 2 0.2 2.5 -6 16 2 77.1 8.8 6 18 2 1.3 2.5 -6 18 2 19.5 2.4 6 20 2 7.9 4.1 -6 20 2 490.0 25.9 -6 22 2 507.9 25.0 7 1 2 4.0 3.5 -7 1 2 36.7 2.6 7 3 2 257.5 4.8 -7 3 2 123.9 3.0 7 5 2 131.1 3.6 -7 5 2 15.9 3.4 7 7 2 77.1 2.9 -7 7 2 68.2 3.4 7 9 2 2.6 3.8 -7 9 2 14.5 1.6 7 11 2 166.5 4.6 -7 11 2 12.4 4.2 7 13 2 11.4 2.5 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