#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 09/06/2017' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section C' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; ? # name ; ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. # enable this reference if Diamond ver. 2 was used for visualization #Brandenburg, K. (1999). DIAMOND. Version. 2.1c. #Crystal Impact GbR, Bonn, Germany. # enable this reference if Diamond ver. 3 was used for visualization #Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. #Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. # enable this reference if SIR97 was used for solving of the structure #Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., #Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). #SIR97. A Package for Crystal Structure Solution by Direct Methods #and Refinement, Bari, Rome, Italy. # use this reference if SIR2002 was used for solving of the structure #Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., #Polidori, G., Spagna, R. #SIR2002: the program, J. Appl. Cryst, (2003). 36, 1103 # use this reference if SIR2011 was used for solving of the structure #Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, #G.L., Giacovazzo, C., Mallamo. M., Mazzone, A., Polidori, G., Spagna, R. #SIR2011: a new package for crystal structure determination and refinement, #J.Appl.Cryst. (2012) 45, 357-361 # enable this reference if bond valences were calculated #Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # enable this reference if Xshape wase used for crystal shape refinement #Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. # enable this reference if Flack coefficient was refined #Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'O7 Ti2 Yb2' _chemical_formula_weight 553.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F d -3 m' _symmetry_space_group_name_Hall '-F 4abvw;2abvw;3' _symmetry_Int_Tables_number 227 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+3/4,-y+1/4,z+1/2 3 -x+1/4,y+1/2,-z+3/4 4 x+1/2,-y+3/4,-z+1/4 5 z,x,y 6 z+1/2,-x+3/4,-y+1/4 7 -z+3/4,-x+1/4,y+1/2 8 -z+1/4,x+1/2,-y+3/4 9 y,z,x 10 -y+1/4,z+1/2,-x+3/4 11 y+1/2,-z+3/4,-x+1/4 12 -y+3/4,-z+1/4,x+1/2 13 y+3/4,x+1/4,-z+1/2 14 -y,-x,-z 15 y+1/4,-x+1/2,z+3/4 16 -y+1/2,x+3/4,z+1/4 17 x+3/4,z+1/4,-y+1/2 18 -x+1/2,z+3/4,y+1/4 19 -x,-z,-y 20 x+1/4,-z+1/2,y+3/4 21 z+3/4,y+1/4,-x+1/2 22 z+1/4,-y+1/2,x+3/4 23 -z+1/2,y+3/4,x+1/4 24 -z,-y,-x 25 -x,-y,-z 26 x+1/4,y+3/4,-z+1/2 27 x+3/4,-y+1/2,z+1/4 28 -x+1/2,y+1/4,z+3/4 29 -z,-x,-y 30 -z+1/2,x+1/4,y+3/4 31 z+1/4,x+3/4,-y+1/2 32 z+3/4,-x+1/2,y+1/4 33 -y,-z,-x 34 y+3/4,-z+1/2,x+1/4 35 -y+1/2,z+1/4,x+3/4 36 y+1/4,z+3/4,-x+1/2 37 -y+1/4,-x+3/4,z+1/2 38 y,x,z 39 -y+3/4,x+1/2,-z+1/4 40 y+1/2,-x+1/4,-z+3/4 41 -x+1/4,-z+3/4,y+1/2 42 x+1/2,-z+1/4,-y+3/4 43 x,z,y 44 -x+3/4,z+1/2,-y+1/4 45 -z+1/4,-y+3/4,x+1/2 46 -z+3/4,y+1/2,-x+1/4 47 z+1/2,-y+1/4,-x+3/4 48 z,y,x 49 x,y+1/2,z+1/2 50 -x+3/4,-y+3/4,z 51 -x+1/4,y,-z+1/4 52 x+1/2,-y+1/4,-z+3/4 53 z,x+1/2,y+1/2 54 z+1/2,-x+1/4,-y+3/4 55 -z+3/4,-x+3/4,y 56 -z+1/4,x,-y+1/4 57 y,z+1/2,x+1/2 58 -y+1/4,z,-x+1/4 59 y+1/2,-z+1/4,-x+3/4 60 -y+3/4,-z+3/4,x 61 y+3/4,x+3/4,-z 62 -y,-x+1/2,-z+1/2 63 y+1/4,-x,z+1/4 64 -y+1/2,x+1/4,z+3/4 65 x+3/4,z+3/4,-y 66 -x+1/2,z+1/4,y+3/4 67 -x,-z+1/2,-y+1/2 68 x+1/4,-z,y+1/4 69 z+3/4,y+3/4,-x 70 z+1/4,-y,x+1/4 71 -z+1/2,y+1/4,x+3/4 72 -z,-y+1/2,-x+1/2 73 -x,-y+1/2,-z+1/2 74 x+1/4,y+1/4,-z 75 x+3/4,-y,z+3/4 76 -x+1/2,y+3/4,z+1/4 77 -z,-x+1/2,-y+1/2 78 -z+1/2,x+3/4,y+1/4 79 z+1/4,x+1/4,-y 80 z+3/4,-x,y+3/4 81 -y,-z+1/2,-x+1/2 82 y+3/4,-z,x+3/4 83 -y+1/2,z+3/4,x+1/4 84 y+1/4,z+1/4,-x 85 -y+1/4,-x+1/4,z 86 y,x+1/2,z+1/2 87 -y+3/4,x,-z+3/4 88 y+1/2,-x+3/4,-z+1/4 89 -x+1/4,-z+1/4,y 90 x+1/2,-z+3/4,-y+1/4 91 x,z+1/2,y+1/2 92 -x+3/4,z,-y+3/4 93 -z+1/4,-y+1/4,x 94 -z+3/4,y,-x+3/4 95 z+1/2,-y+3/4,-x+1/4 96 z,y+1/2,x+1/2 97 x+1/2,y,z+1/2 98 -x+1/4,-y+1/4,z 99 -x+3/4,y+1/2,-z+1/4 100 x,-y+3/4,-z+3/4 101 z+1/2,x,y+1/2 102 z,-x+3/4,-y+3/4 103 -z+1/4,-x+1/4,y 104 -z+3/4,x+1/2,-y+1/4 105 y+1/2,z,x+1/2 106 -y+3/4,z+1/2,-x+1/4 107 y,-z+3/4,-x+3/4 108 -y+1/4,-z+1/4,x 109 y+1/4,x+1/4,-z 110 -y+1/2,-x,-z+1/2 111 y+3/4,-x+1/2,z+1/4 112 -y,x+3/4,z+3/4 113 x+1/4,z+1/4,-y 114 -x,z+3/4,y+3/4 115 -x+1/2,-z,-y+1/2 116 x+3/4,-z+1/2,y+1/4 117 z+1/4,y+1/4,-x 118 z+3/4,-y+1/2,x+1/4 119 -z,y+3/4,x+3/4 120 -z+1/2,-y,-x+1/2 121 -x+1/2,-y,-z+1/2 122 x+3/4,y+3/4,-z 123 x+1/4,-y+1/2,z+3/4 124 -x,y+1/4,z+1/4 125 -z+1/2,-x,-y+1/2 126 -z,x+1/4,y+1/4 127 z+3/4,x+3/4,-y 128 z+1/4,-x+1/2,y+3/4 129 -y+1/2,-z,-x+1/2 130 y+1/4,-z+1/2,x+3/4 131 -y,z+1/4,x+1/4 132 y+3/4,z+3/4,-x 133 -y+3/4,-x+3/4,z 134 y+1/2,x,z+1/2 135 -y+1/4,x+1/2,-z+3/4 136 y,-x+1/4,-z+1/4 137 -x+3/4,-z+3/4,y 138 x,-z+1/4,-y+1/4 139 x+1/2,z,y+1/2 140 -x+1/4,z+1/2,-y+3/4 141 -z+3/4,-y+3/4,x 142 -z+1/4,y+1/2,-x+3/4 143 z,-y+1/4,-x+1/4 144 z+1/2,y,x+1/2 145 x+1/2,y+1/2,z 146 -x+1/4,-y+3/4,z+1/2 147 -x+3/4,y,-z+3/4 148 x,-y+1/4,-z+1/4 149 z+1/2,x+1/2,y 150 z,-x+1/4,-y+1/4 151 -z+1/4,-x+3/4,y+1/2 152 -z+3/4,x,-y+3/4 153 y+1/2,z+1/2,x 154 -y+3/4,z,-x+3/4 155 y,-z+1/4,-x+1/4 156 -y+1/4,-z+3/4,x+1/2 157 y+1/4,x+3/4,-z+1/2 158 -y+1/2,-x+1/2,-z 159 y+3/4,-x,z+3/4 160 -y,x+1/4,z+1/4 161 x+1/4,z+3/4,-y+1/2 162 -x,z+1/4,y+1/4 163 -x+1/2,-z+1/2,-y 164 x+3/4,-z,y+3/4 165 z+1/4,y+3/4,-x+1/2 166 z+3/4,-y,x+3/4 167 -z,y+1/4,x+1/4 168 -z+1/2,-y+1/2,-x 169 -x+1/2,-y+1/2,-z 170 x+3/4,y+1/4,-z+1/2 171 x+1/4,-y,z+1/4 172 -x,y+3/4,z+3/4 173 -z+1/2,-x+1/2,-y 174 -z,x+3/4,y+3/4 175 z+3/4,x+1/4,-y+1/2 176 z+1/4,-x,y+1/4 177 -y+1/2,-z+1/2,-x 178 y+1/4,-z,x+1/4 179 -y,z+3/4,x+3/4 180 y+3/4,z+1/4,-x+1/2 181 -y+3/4,-x+1/4,z+1/2 182 y+1/2,x+1/2,z 183 -y+1/4,x,-z+1/4 184 y,-x+3/4,-z+3/4 185 -x+3/4,-z+1/4,y+1/2 186 x,-z+3/4,-y+3/4 187 x+1/2,z+1/2,y 188 -x+1/4,z,-y+1/4 189 -z+3/4,-y+1/4,x+1/2 190 -z+1/4,y,-x+1/4 191 z,-y+3/4,-x+3/4 192 z+1/2,y+1/2,x _cell_length_a 10.0838(14) _cell_length_b 10.0838(14) _cell_length_c 10.0838(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1025.4(2) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 ? ? ? ? ? ? ? ? ? ? ? _cell_formula_units_Z 8 _cell_measurement_reflns_used 415 _cell_measurement_theta_min 6.7 _cell_measurement_theta_max 28.09 _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 7.1754 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2101 _exptl_absorpt_coefficient_mu 47.418 _exptl_crystal_description ? _exptl_crystal_size_max 0.354 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.082 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.014 _exptl_absorpt_correction_T_max 0.095 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0178 _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 725 _diffrn_reflns_theta_min 3.5 _diffrn_reflns_theta_max 28.81 _diffrn_reflns_theta_full 28.81 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_unetI/netI 0.0078 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 84 _reflns_number_gt 79 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_gt 0.0488 _refine_ls_R_factor_all 0.0401 _refine_ls_wR_factor_ref 0.0490 _refine_ls_goodness_of_fit_ref 3.47 _refine_ls_goodness_of_fit_gt 3.58 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 84 _refine_ls_number_parameters 14 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 2.0705 _refine_ls_shift/su_mean 0.4732 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method 'B-C type 2 (Becker & Coppens, 1974)' _refine_ls_extinction_coef 3100(600) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Ti 0.2776 0.4457 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Yb -0.3850 5.5486 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? loop_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param ? ? ? ? ? ? loop_ _restr_angle_atom_site_label_1 _restr_angle_site_symmetry_1 _restr_angle_atom_site_label_2 _restr_angle_site_symmetry_2 _restr_angle_atom_site_label_3 _restr_angle_site_symmetry_3 _restr_angle_target _restr_angle_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_torsion_atom_site_label_1 _restr_torsion_site_symmetry_1 _restr_torsion_atom_site_label_2 _restr_torsion_site_symmetry_2 _restr_torsion_atom_site_label_3 _restr_torsion_site_symmetry_3 _restr_torsion_atom_site_label_4 _restr_torsion_site_symmetry_4 _restr_torsion_angle_target _restr_torsion_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_site_symmetry_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param ? ? ? ? ? ? loop_ _restr_equal_angle_atom_site_label_1 _restr_equal_angle_site_symmetry_1 _restr_equal_angle_atom_site_label_2 _restr_equal_angle_site_symmetry_2 _restr_equal_angle_atom_site_label_3 _restr_equal_angle_site_symmetry_3 _restr_equal_angle_class_class_id _restr_equal_angle_class_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_equal_torsion_atom_site_label_1 _restr_equal_torsion_site_symmetry_1 _restr_equal_torsion_atom_site_label_2 _restr_equal_torsion_site_symmetry_2 _restr_equal_torsion_atom_site_label_3 _restr_equal_torsion_site_symmetry_3 _restr_equal_torsion_atom_site_label_4 _restr_equal_torsion_site_symmetry_4 _restr_equal_torsion_class_class_id _restr_equal_torsion_class_target_weight_param ? ? ? ? ? ? ? ? ? ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.5 0.5 0.5 Uani 0.0279(8) 16 1 d . . . Ti1 Ti 0 0 0 Uani 0.052(13) 16 0.74(3) d . . . O1 O 0.375 0.375 0.375 Uani 0.016(3) 8 1 d . . . O2 O 0.3397(14) 0.125 0.125 Uani 0.035(3) 48 0.96 d . . . Yb2 Yb 0 0 0 Uani 0.027(3) 16 0.26(3) d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Yb1 Yb 0.0279(13) 0.0279(13) 0.0279(13) -0.0058(2) -0.0058(2) -0.0058(2) Ti1 Ti 0.05(2) 0.05(2) 0.05(2) -0.008(6) -0.008(6) -0.008(6) O1 O 0.016(4) 0.016(4) 0.016(4) 0 0 0 O2 O 0.050(7) 0.028(4) 0.028(4) 0 0 -0.004(5) Yb2 Yb 0.027(5) 0.027(5) 0.027(5) 0.008(3) 0.008(3) 0.008(3) loop_ _jana_atom_site_ADP_C_label _jana_atom_site_ADP_C_type_symbol _jana_atom_site_ADP_C_111 _jana_atom_site_ADP_C_112 _jana_atom_site_ADP_C_113 _jana_atom_site_ADP_C_122 _jana_atom_site_ADP_C_123 _jana_atom_site_ADP_C_133 _jana_atom_site_ADP_C_222 _jana_atom_site_ADP_C_223 _jana_atom_site_ADP_C_233 _jana_atom_site_ADP_C_333 ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_D_label _jana_atom_site_ADP_D_type_symbol _jana_atom_site_ADP_D_1111 _jana_atom_site_ADP_D_1112 _jana_atom_site_ADP_D_1113 _jana_atom_site_ADP_D_1122 _jana_atom_site_ADP_D_1123 _jana_atom_site_ADP_D_1133 _jana_atom_site_ADP_D_1222 _jana_atom_site_ADP_D_1223 _jana_atom_site_ADP_D_1233 _jana_atom_site_ADP_D_1333 _jana_atom_site_ADP_D_2222 _jana_atom_site_ADP_D_2223 _jana_atom_site_ADP_D_2233 _jana_atom_site_ADP_D_2333 _jana_atom_site_ADP_D_3333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_E_label _jana_atom_site_ADP_E_type_symbol _jana_atom_site_ADP_E_11111 _jana_atom_site_ADP_E_11112 _jana_atom_site_ADP_E_11113 _jana_atom_site_ADP_E_11122 _jana_atom_site_ADP_E_11123 _jana_atom_site_ADP_E_11133 _jana_atom_site_ADP_E_11222 _jana_atom_site_ADP_E_11223 _jana_atom_site_ADP_E_11233 _jana_atom_site_ADP_E_11333 _jana_atom_site_ADP_E_12222 _jana_atom_site_ADP_E_12223 _jana_atom_site_ADP_E_12233 _jana_atom_site_ADP_E_12333 _jana_atom_site_ADP_E_13333 _jana_atom_site_ADP_E_22222 _jana_atom_site_ADP_E_22223 _jana_atom_site_ADP_E_22233 _jana_atom_site_ADP_E_22333 _jana_atom_site_ADP_E_23333 _jana_atom_site_ADP_E_33333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_F_label _jana_atom_site_ADP_F_type_symbol _jana_atom_site_ADP_F_111111 _jana_atom_site_ADP_F_111112 _jana_atom_site_ADP_F_111113 _jana_atom_site_ADP_F_111122 _jana_atom_site_ADP_F_111123 _jana_atom_site_ADP_F_111133 _jana_atom_site_ADP_F_111222 _jana_atom_site_ADP_F_111223 _jana_atom_site_ADP_F_111233 _jana_atom_site_ADP_F_111333 _jana_atom_site_ADP_F_112222 _jana_atom_site_ADP_F_112223 _jana_atom_site_ADP_F_112233 _jana_atom_site_ADP_F_112333 _jana_atom_site_ADP_F_113333 _jana_atom_site_ADP_F_122222 _jana_atom_site_ADP_F_122223 _jana_atom_site_ADP_F_122233 _jana_atom_site_ADP_F_122333 _jana_atom_site_ADP_F_123333 _jana_atom_site_ADP_F_133333 _jana_atom_site_ADP_F_222222 _jana_atom_site_ADP_F_222223 _jana_atom_site_ADP_F_222233 _jana_atom_site_ADP_F_222333 _jana_atom_site_ADP_F_223333 _jana_atom_site_ADP_F_233333 _jana_atom_site_ADP_F_333333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag ? ? ? ? ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 1 1 1 65410. 61533. 375. o 0 2 2 1011. 1382. 41. o 2 2 2 1794090. 1776660. 4552. o 1 1 3 44772. 49706. 192. o 1 3 3 94414. 95086. 278. o 3 3 3 7714. 7880. 129. o 0 0 4 1033030. 1025900. 5598. o 2 2 4 1283. 1243. 32. o 0 4 4 1411350. 1591950. 5955. o 2 4 4 463. 416. 26. o 4 4 4 585008. 588149. 2404. o 1 1 5 55246. 56047. 284. o 1 3 5 47590. 46712. 218. o 3 3 5 30026. 30795. 212. o 1 5 5 12179. 11730. 188. o 3 5 5 31847. 33935. 313. o 5 5 5 17264. 15339. 315. o 0 2 6 1443. 1689. 87. o 2 2 6 810555. 803425. 1744. o 2 4 6 99. 89. 16. o 4 4 6 255. 200. 39. o 0 6 6 37. 288. 50. o 2 6 6 428135. 448413. 1713. o 4 6 6 2334. 1984. 119. o 1 1 7 45321. 39814. 442. o 1 3 7 12454. 13764. 165. o 3 3 7 30543. 29127. 279. o 1 5 7 25303. 26941. 211. o 3 5 7 31050. 31800. 277. o 5 5 7 20430. 18815. 378. o 1 7 7 17177. 17648. 300. o 3 7 7 750. 814. 103. o 5 7 7 8682. 7977. 235. o 7 7 7 3300. 2123. 204. o 0 0 8 657809. 561684. 4946. o 2 2 8 1912. 1640. 78. o 0 4 8 327717. 336870. 1388. o 2 4 8 606. 410. 35. o 4 4 8 337879. 315675. 1844. o 2 6 8 6. 52. 30. < 4 6 8 485. 264. 39. o 6 6 8 421. 156. 39. o 0 8 8 191679. 219173. 2573. o 2 8 8 1000. 1111. 128. o 4 8 8 124520. 126322. 1942. o 6 8 8 785. 487. 109. o 1 1 9 13171. 12328. 323. o 1 3 9 17609. 17795. 228. o 3 3 9 26560. 27025. 459. o 1 5 9 9488. 10092. 199. o 3 5 9 10500. 11222. 224. o 5 5 9 742. 620. 83. o 1 7 9 16508. 19302. 307. o 3 7 9 10237. 12052. 345. o 5 7 9 9657. 9420. 264. o 7 7 9 10974. 12325. 630. o 1 9 9 1177. 1486. 244. o 3 9 9 4069. 4867. 406. o 5 9 9 504. 742. 175. o 0 2 10 132. 240. 51. o 2 2 10 237946. 212755. 1452. o 2 4 10 634. 648. 50. o 4 4 10 169. 91. 44. < 0 6 10 3192. 4096. 214. o 2 6 10 140975. 154669. 1025. o 4 6 10 56. -47. 45. < 2 8 10 71. 74. 51. < 4 8 10 223. 131. 60. < 1 1 11 10261. 10254. 290. o 1 3 11 10384. 9655. 207. o 3 3 11 1304. 1344. 105. o 1 5 11 11795. 12689. 257. o 3 5 11 7132. 8775. 227. o 5 5 11 10242. 11872. 549. o 1 7 11 1585. 1940. 136. o 3 7 11 2064. 2689. 240. o 0 0 12 107947. 98434. 2183. o 2 2 12 293. 384. 56. o 0 4 12 116554. 115508. 1174. o 2 4 12 325. 321. 57. o 4 4 12 71685. 55039. 2654. o 2 6 12 216. 382. 104. o 1 1 13 3669. 3464. 311. o 1 3 13 6934. 5483. 490. o loop_ _twin_refln_datum_id _twin_refln_individual_id _twin_refln_index_h _twin_refln_index_k _twin_refln_index_l _twin_refln_F_squared_calc _twin_refln_F_squared_meas _twin_refln_F_squared_sigma _twin_refln_include_status ? ? ? ? ? ? ? ? ?