#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:21:39 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286867 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022903.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022903 loop_ _publ_author_name 'Comboni, Davide' 'Poreba, Tomasz' 'Pagliaro, Francesco' 'Battiston, Tommaso' 'Lotti, Paolo' 'Gatta, Giacomo Diego' 'Garbarino, Gaston' 'Hanfland, Michael' _publ_section_title ; Crystal structure of the high-P polymorph of Ca2B6O6(OH)10·2(H2O) (meyerhofferite) ; _journal_coeditor_code DK5106 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials' _journal_page_first 940 _journal_page_last 945 _journal_paper_doi 10.1107/S2052520621009768 _journal_volume 77 _journal_year 2021 _chemical_formula_structural 'Ca (B3 O3 (O H)5) (H2 O)' _chemical_formula_sum 'B3 Ca H7 O9' _chemical_formula_weight 223.6 _chemical_name_common meyerhofferite _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_date 2021-04-028 _audit_creation_method ; 'Jana2006 Version : 14/01/2019' ; _cell_angle_alpha 89.922(3) _cell_angle_beta 103.380(10) _cell_angle_gamma 86.859(10) _cell_formula_units_Z 2 _cell_length_a 6.465(3) _cell_length_b 8.059(3) _cell_length_c 6.388(3) _cell_measurement_pressure 3140000 _cell_measurement_reflns_used 718 _cell_measurement_temperature 293 _cell_measurement_theta_max 19.5850 _cell_measurement_theta_min 2.3780 _cell_volume 323.3(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_structure_refinement 'Jana2006 (Petricek et al., 2014)' _computing_structure_solution 'Olex2 (Dolomanov et al., 2009)' _diffrn_ambient_pressure 3140000 _diffrn_ambient_temperature 293(1) _diffrn_detector 'Eiger2 9M CdTe' _diffrn_measured_fraction_theta_full 0.30 _diffrn_measured_fraction_theta_max 0.16 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): RUN TYPE OF SCAN START(DEG) END(DEG) # FRAMES EXP(SEC) OMEGA(DEG) THETA(DEG) KAPPA(DEG) PHI(DEG) Run 1 Omega scan: (-32.000 - 32.000,128 frames, 0.200 sec, 0.500 deg) at th=0.000, ka=0.000,ph=0.000 (rot geo dd=199.206) 1 OMEGA -32.00000 32.00000 128 0.20000 n/a -0.01874 0.00000 0.00000 ; _diffrn_measurement_device ID15b _diffrn_measurement_device_type beamline _diffrn_measurement_method 'omega scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.065312 _diffrn_orient_matrix_UB_12 0.005584 _diffrn_orient_matrix_UB_13 -0.013494 _diffrn_orient_matrix_UB_21 0.003872 _diffrn_orient_matrix_UB_22 0.047299 _diffrn_orient_matrix_UB_23 0.023853 _diffrn_orient_matrix_UB_31 -0.000466 _diffrn_orient_matrix_UB_32 0.018331 _diffrn_orient_matrix_UB_33 -0.060132 _diffrn_radiation_collimation '0.2 mm double pinhole' _diffrn_radiation_monochromator silicon _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.41066 _diffrn_reflns_av_R_equivalents 0.0126 _diffrn_reflns_av_unetI/netI 0.0164 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 718 _diffrn_reflns_theta_full 12.09 _diffrn_reflns_theta_max 19.59 _diffrn_reflns_theta_min 2.28 _diffrn_source 'ESRF: Synchrotron radiation' _diffrn_source_power '200 mA' _diffrn_source_type 'undulator, IVU20c' _diffrn_source_voltage 30keV _diffrn_standards_decay_% 0.5(1) _diffrn_standards_interval_count 15 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.2244 _exptl_crystal_description 'prismatic habit' _exptl_crystal_F_000 214 _exptl_crystal_size_max 0.020 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.33 _refine_diff_density_min -0.27 _refine_ls_extinction_coef none _refine_ls_extinction_method none _refine_ls_goodness_of_fit_gt 3.63 _refine_ls_goodness_of_fit_ref 3.48 _refine_ls_hydrogen_treatment undef _refine_ls_number_constraints 0 _refine_ls_number_parameters 53 _refine_ls_number_reflns 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0465 _refine_ls_shift/su_max 0.0148 _refine_ls_shift/su_mean 0.0041 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.0627 _reflns_number_gt 437 _reflns_number_total 479 _reflns_threshold_expression I>3\s(I) _cod_data_source_file dk5106sup1.cif _cod_data_source_block I_3.14GPa _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_formula_sum 'H7 B3 Ca1 O9' _cod_database_code 2022903 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z 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 Ca Ca 0.0100(5) 0.37346(11) 0.24576(17) Uiso 0.0125(3) 2 1 d . . . B1 B 0.310(3) 0.8070(7) 0.4896(11) Uiso 0.0135(10) 2 1 d . . . B2 B 0.295(4) 0.6347(7) 0.1720(11) Uiso 0.0137(11) 2 1 d . . . B3 B 0.053(3) 0.2623(6) 0.7058(10) Uiso 0.0139(10) 2 1 d . . . O1 O 0.411(2) 0.7404(4) 0.3383(7) Uiso 0.0179(8) 2 1 d . . . O2 O 0.4387(18) 0.8965(4) 0.6594(6) Uiso 0.0154(7) 2 1 d . . . O3 O 0.111(2) 0.7868(4) 0.4910(7) Uiso 0.0141(7) 2 1 d . . . O4 O 0.346(2) 0.4576(4) 0.2144(7) Uiso 0.0179(8) 2 1 d . . . O5 O 0.061(2) 0.6539(4) 0.1465(7) Uiso 0.0131(8) 2 1 d . . . O6 O 0.1791(19) 0.3841(4) 0.6245(6) Uiso 0.0142(7) 2 1 d . . . O7 O 0.153(2) 0.0979(4) 0.2161(6) Uiso 0.0172(8) 2 1 d . . . O8 O 0.170(2) 0.1184(4) 0.8114(7) Uiso 0.0175(8) 2 1 d . . . O9 O 0.3386(19) 0.6788(4) 0.9620(6) Uiso 0.0165(8) 2 1 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 ? ? ? ? ? ? ? ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B -0.0004 0.0002 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Ca 0.0949 0.1047 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? 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 B2 Ca B2 . . 2_565 102.1(4) ? B2 Ca B3 . . 2_566 52.7(5) ? B2 Ca O3 . . 2_566 146.2(2) ? B2 Ca O4 . . . 28.9(4) ? B2 Ca O5 . . . 29.6(5) ? B2 Ca O5 . . 2_565 83.7(3) ? B2 Ca O6 . . . 87.7(3) ? B2 Ca O6 . . 2_566 81.9(4) ? B2 Ca O7 . . . 113.4(4) ? B2 Ca O9 . . 2_566 128.0(3) ? B2 Ca B3 2_565 . 2_566 94.3(2) ? B2 Ca O3 2_565 . 2_566 110.1(4) ? B2 Ca O4 2_565 . . 112.2(4) ? B2 Ca O5 2_565 . . 85.5(3) ? B2 Ca O5 2_565 . 2_565 30.3(5) ? B2 Ca O6 2_565 . . 165.3(5) ? B2 Ca O6 2_565 . 2_566 94.1(3) ? B2 Ca O7 2_565 . . 93.6(2) ? B2 Ca O9 2_565 . 2_566 30.2(4) ? B3 Ca O3 2_566 . 2_566 113.2(3) ? B3 Ca O4 2_566 . . 80.2(4) ? B3 Ca O5 2_566 . . 29.5(4) ? B3 Ca O5 2_566 . 2_565 102.04(15) ? B3 Ca O6 2_566 . . 82.89(17) ? B3 Ca O6 2_566 . 2_566 29.7(4) ? B3 Ca O7 2_566 . . 165.4(5) ? B3 Ca O9 2_566 . 2_566 98.5(3) ? O3 Ca O4 2_566 . . 134.2(3) ? O3 Ca O5 2_566 . . 142.4(2) ? O3 Ca O5 2_566 . 2_565 129.9(3) ? O3 Ca O6 2_566 . . 58.7(3) ? O3 Ca O6 2_566 . 2_566 85.6(2) ? O3 Ca O7 2_566 . . 75.3(3) ? O3 Ca O9 2_566 . 2_566 81.1(3) ? O4 Ca O5 . . . 58.3(4) ? O4 Ca O5 . . 2_565 84.6(3) ? O4 Ca O6 . . . 81.6(3) ? O4 Ca O6 . . 2_566 107.6(3) ? O4 Ca O7 . . . 85.4(3) ? O4 Ca O9 . . 2_566 142.5(2) ? O5 Ca O5 . . 2_565 80.30(15) ? O5 Ca O6 . . . 98.50(18) ? O5 Ca O6 . . 2_566 58.6(3) ? O5 Ca O7 . . . 139.6(4) ? O5 Ca O9 . . 2_566 103.8(3) ? O5 Ca O6 2_565 . . 164.3(5) ? O5 Ca O6 2_565 . 2_566 115.2(2) ? O5 Ca O7 2_565 . . 79.07(17) ? O5 Ca O9 2_565 . 2_566 58.8(4) ? O6 Ca O6 . . 2_566 76.3(2) ? O6 Ca O7 . . . 92.43(18) ? O6 Ca O9 . . 2_566 135.8(4) ? O6 Ca O7 2_566 . . 160.9(3) ? O6 Ca O9 2_566 . 2_566 83.5(3) ? O7 Ca O9 . . 2_566 94.6(3) ? B2 B1 B3 . . 2_566 64.7(7) ? B2 B1 O1 . . . 31.4(7) ? B2 B1 O2 . . . 147.5(14) ? B2 B1 O3 . . . 93.0(8) ? B2 B1 O5 . . . 32.5(6) ? B2 B1 O7 . . 1_565 90.5(3) ? B3 B1 O1 2_566 . . 95.3(7) ? B3 B1 O2 2_566 . . 147.6(11) ? B3 B1 O3 2_566 . . 30.6(4) ? B3 B1 O5 2_566 . . 32.2(4) ? B3 B1 O7 2_566 . 1_565 76.0(4) ? O1 B1 O2 . . . 116.3(15) ? O1 B1 O3 . . . 124.4(9) ? O1 B1 O5 . . . 63.2(6) ? O1 B1 O7 . . 1_565 91.2(4) ? O2 B1 O3 . . . 119.3(10) ? O2 B1 O5 . . . 176.2(4) ? O2 B1 O7 . . 1_565 95.4(3) ? O3 B1 O5 . . . 61.6(5) ? O3 B1 O7 . . 1_565 86.4(6) ? O5 B1 O7 . . 1_565 80.9(3) ? Ca B2 Ca . . 2_565 77.9(4) ? Ca B2 B1 . . . 101.6(7) ? Ca B2 B3 . . 2_566 63.5(5) ? Ca B2 O1 . . . 125.0(7) ? Ca B2 O3 . . . 79.3(5) ? Ca B2 O4 . . . 51.5(8) ? Ca B2 O5 . . . 53.4(5) ? Ca B2 O9 . . 1_554 125.7(6) ? Ca B2 B1 2_565 . . 132.8(8) ? Ca B2 B3 2_565 . 2_566 81.3(6) ? Ca B2 O1 2_565 . . 145.6(4) ? Ca B2 O3 2_565 . . 112.1(7) ? Ca B2 O4 2_565 . . 100.8(5) ? Ca B2 O5 2_565 . . 56.7(4) ? Ca B2 O9 2_565 . 1_554 54.5(6) ? B1 B2 B3 . . 2_566 58.4(6) ? B1 B2 O1 . . . 29.6(7) ? B1 B2 O3 . . . 27.5(5) ? B1 B2 O4 . . . 115.7(4) ? B1 B2 O5 . . . 84.8(8) ? B1 B2 O9 . . 1_554 129.0(6) ? B3 B2 O1 2_566 . . 87.2(9) ? B3 B2 O3 2_566 . . 31.9(4) ? B3 B2 O4 2_566 . . 112.2(11) ? B3 B2 O5 2_566 . . 26.5(4) ? B3 B2 O9 2_566 . 1_554 123.8(9) ? O1 B2 O3 . . . 57.0(7) ? O1 B2 O4 . . . 113.6(9) ? O1 B2 O5 . . . 113.1(11) ? O1 B2 O9 . . 1_554 109.3(12) ? O3 B2 O4 . . . 112.3(7) ? O3 B2 O5 . . . 58.3(6) ? O3 B2 O9 . . 1_554 138.5(5) ? O4 B2 O5 . . . 104.5(12) ? O4 B2 O9 . . 1_554 109.0(9) ? O5 B2 O9 . . 1_554 107.0(9) ? Ca B3 B1 2_566 . 2_566 100.8(5) ? Ca B3 B2 2_566 . 2_566 63.8(3) ? Ca B3 O1 2_566 . 2_566 84.9(4) ? Ca B3 O3 2_566 . 2_566 107.1(5) ? Ca B3 O5 2_566 . 2_566 53.6(3) ? Ca B3 O6 2_566 . . 56.9(4) ? Ca B3 O8 2_566 . . 142.1(6) ? B1 B3 B2 2_566 . 2_566 56.9(6) ? B1 B3 O1 2_566 . 2_566 27.7(4) ? B1 B3 O3 2_566 . 2_566 26.1(7) ? B1 B3 O5 2_566 . 2_566 83.5(10) ? B1 B3 O6 2_566 . . 123.3(6) ? B1 B3 O8 2_566 . . 110.8(7) ? B2 B3 O1 2_566 . 2_566 29.5(3) ? B2 B3 O3 2_566 . 2_566 81.1(9) ? B2 B3 O5 2_566 . 2_566 26.6(6) ? B2 B3 O6 2_566 . . 119.5(6) ? B2 B3 O8 2_566 . . 117.6(9) ? O1 B3 O3 2_566 . 2_566 53.2(8) ? O1 B3 O5 2_566 . 2_566 55.9(8) ? O1 B3 O6 2_566 . . 129.8(7) ? O1 B3 O8 2_566 . . 114.2(9) ? O3 B3 O5 2_566 . 2_566 107.6(13) ? O3 B3 O6 2_566 . . 104.7(6) ? O3 B3 O8 2_566 . . 110.4(5) ? O5 B3 O6 2_566 . . 108.9(5) ? O5 B3 O8 2_566 . . 108.9(6) ? O6 B3 O8 . . . 115.8(14) ? B1 O1 B2 . . . 119.0(14) ? B1 O1 B3 . . 2_566 57.0(8) ? B1 O1 O2 . . . 32.5(7) ? B1 O1 O3 . . . 27.0(8) ? B1 O1 O4 . . . 119.7(8) ? B1 O1 O5 . . . 86.6(9) ? B1 O1 O6 . . 2_666 131.1(7) ? B1 O1 O9 . . 1_554 140.1(9) ? B2 O1 B3 . . 2_566 63.2(10) ? B2 O1 O2 . . . 151.2(12) ? B2 O1 O3 . . . 92.0(11) ? B2 O1 O4 . . . 33.2(4) ? B2 O1 O5 . . . 33.7(9) ? B2 O1 O6 . . 2_666 101.3(9) ? B2 O1 O9 . . 1_554 35.6(6) ? B3 O1 O2 2_566 . . 89.2(5) ? B3 O1 O3 2_566 . . 30.7(3) ? B3 O1 O4 2_566 . . 79.3(4) ? B3 O1 O5 2_566 . . 29.8(3) ? B3 O1 O6 2_566 . 2_666 158.1(2) ? B3 O1 O9 2_566 . 1_554 86.1(4) ? O2 O1 O3 . . . 59.4(4) ? O2 O1 O4 . . . 139.0(3) ? O2 O1 O5 . . . 119.0(6) ? O2 O1 O6 . . 2_666 102.4(4) ? O2 O1 O9 . . 1_554 159.6(2) ? O3 O1 O4 . . . 98.3(5) ? O3 O1 O5 . . . 59.9(4) ? O3 O1 O6 . . 2_666 149.6(2) ? O3 O1 O9 . . 1_554 116.5(6) ? O4 O1 O5 . . . 56.7(4) ? O4 O1 O6 . . 2_666 79.8(4) ? O4 O1 O9 . . 1_554 59.27(17) ? O5 O1 O6 . . 2_666 134.3(3) ? O5 O1 O9 . . 1_554 58.8(4) ? O6 O1 O9 2_666 . 1_554 88.8(4) ? B1 O2 O1 . . . 31.3(8) ? B1 O2 O2 . . 2_676 89.3(5) ? B1 O2 O3 . . . 28.9(8) ? B1 O2 O7 . . 2_666 130.3(9) ? B1 O2 O8 . . 1_565 107.3(9) ? B1 O2 O9 . . . 89.7(5) ? O1 O2 O2 . . 2_676 71.8(2) ? O1 O2 O3 . . . 60.2(4) ? O1 O2 O7 . . 2_666 99.8(5) ? O1 O2 O8 . . 1_565 134.7(5) ? O1 O2 O9 . . . 105.6(2) ? O2 O2 O3 2_676 . . 106.9(3) ? O2 O2 O7 2_676 . 2_666 75.4(4) ? O2 O2 O8 2_676 . 1_565 100.4(2) ? O2 O2 O9 2_676 . . 176.1(4) ? O3 O2 O7 . . 2_666 156.3(3) ? O3 O2 O8 . . 1_565 81.5(4) ? O3 O2 O9 . . . 73.7(3) ? O7 O2 O8 2_666 . 1_565 121.8(3) ? O7 O2 O9 2_666 . . 102.5(3) ? O8 O2 O9 1_565 . . 83.4(3) ? Ca O3 B1 2_566 . . 125.5(5) ? Ca O3 B2 2_566 . . 122.1(2) ? Ca O3 B3 2_566 . 2_566 97.7(7) ? Ca O3 O1 2_566 . . 130.5(3) ? Ca O3 O2 2_566 . . 108.5(2) ? Ca O3 O5 2_566 . . 112.9(3) ? Ca O3 O6 2_566 . 2_566 60.7(3) ? Ca O3 O7 2_566 . 2_566 51.9(2) ? Ca O3 O8 2_566 . 2_566 113.7(6) ? B1 O3 B2 . . . 59.6(6) ? B1 O3 B3 . . 2_566 123.3(9) ? B1 O3 O1 . . . 28.6(4) ? B1 O3 O2 . . . 31.8(4) ? B1 O3 O5 . . . 89.9(6) ? B1 O3 O6 . . 2_566 144.8(5) ? B1 O3 O7 . . 2_566 132.2(4) ? B1 O3 O8 . . 2_566 120.3(5) ? B2 O3 B3 . . 2_566 67.0(8) ? B2 O3 O1 . . . 31.0(4) ? B2 O3 O2 . . . 91.3(6) ? B2 O3 O5 . . . 31.5(5) ? B2 O3 O6 . . 2_566 87.2(4) ? B2 O3 O7 . . 2_566 168.1(6) ? B2 O3 O8 . . 2_566 84.3(4) ? B3 O3 O1 2_566 . . 96.1(8) ? B3 O3 O2 2_566 . . 152.5(8) ? B3 O3 O5 2_566 . . 35.6(7) ? B3 O3 O6 2_566 . 2_566 37.0(5) ? B3 O3 O7 2_566 . 2_566 102.5(9) ? B3 O3 O8 2_566 . 2_566 33.6(3) ? O1 O3 O2 . . . 60.4(4) ? O1 O3 O5 . . . 61.6(4) ? O1 O3 O6 . . 2_566 117.6(3) ? O1 O3 O7 . . 2_566 160.8(4) ? O1 O3 O8 . . 2_566 103.7(4) ? O2 O3 O5 . . . 121.7(6) ? O2 O3 O6 . . 2_566 165.3(3) ? O2 O3 O7 . . 2_566 100.3(3) ? O2 O3 O8 . . 2_566 132.5(3) ? O5 O3 O6 . . 2_566 60.2(4) ? O5 O3 O7 . . 2_566 137.5(6) ? O5 O3 O8 . . 2_566 58.5(3) ? O6 O3 O7 2_566 . 2_566 80.9(5) ? O6 O3 O8 2_566 . 2_566 61.8(3) ? O7 O3 O8 2_566 . 2_566 89.5(5) ? Ca O4 B2 . . . 99.6(11) ? Ca O4 O1 . . . 112.6(5) ? Ca O4 O5 . . . 61.8(4) ? Ca O4 O9 . . 1_554 115.6(5) ? Ca O4 O9 . . 2_666 134.4(2) ? B2 O4 O1 . . . 33.2(5) ? B2 O4 O5 . . . 38.1(10) ? B2 O4 O9 . . 1_554 35.8(6) ? B2 O4 O9 . . 2_666 115.7(10) ? O1 O4 O5 . . . 61.9(4) ? O1 O4 O9 . . 1_554 59.48(17) ? O1 O4 O9 . . 2_666 112.8(5) ? O5 O4 O9 . . 1_554 60.6(4) ? O5 O4 O9 . . 2_666 142.0(3) ? O9 O4 O9 1_554 . 2_666 83.8(4) ? Ca O5 Ca . . 2_565 99.70(16) ? Ca O5 B1 . . . 109.7(2) ? Ca O5 B2 . . . 97.1(4) ? Ca O5 B3 . . 2_566 96.9(6) ? Ca O5 O1 . . . 110.7(3) ? Ca O5 O3 . . . 100.7(2) ? Ca O5 O4 . . . 59.9(3) ? Ca O5 O6 . . 2_566 62.5(3) ? Ca O5 O8 . . 2_566 123.0(6) ? Ca O5 O9 . . 1_554 114.4(4) ? Ca O5 B1 2_565 . . 143.3(6) ? Ca O5 B2 2_565 . . 93.0(5) ? Ca O5 B3 2_565 . 2_566 134.1(7) ? Ca O5 O1 2_565 . . 118.5(5) ? Ca O5 O3 2_565 . . 158.80(18) ? Ca O5 O4 2_565 . . 94.5(3) ? Ca O5 O6 2_565 . 2_566 127.8(6) ? Ca O5 O8 2_565 . 2_566 102.6(3) ? Ca O5 O9 2_565 . 1_554 59.4(3) ? B1 O5 B2 . . . 62.7(5) ? B1 O5 B3 . . 2_566 64.3(7) ? B1 O5 O1 . . . 30.2(4) ? B1 O5 O3 . . . 28.5(5) ? B1 O5 O4 . . . 82.3(5) ? B1 O5 O6 . . 2_566 86.2(4) ? B1 O5 O8 . . 2_566 79.6(4) ? B1 O5 O9 . . 1_554 88.0(6) ? B2 O5 B3 . . 2_566 126.9(8) ? B2 O5 O1 . . . 33.2(4) ? B2 O5 O3 . . . 90.2(5) ? B2 O5 O4 . . . 37.4(4) ? B2 O5 O6 . . 2_566 135.3(4) ? B2 O5 O8 . . 2_566 132.8(5) ? B2 O5 O9 . . 1_554 36.5(4) ? B3 O5 O1 2_566 . . 94.4(7) ? B3 O5 O3 2_566 . . 36.8(7) ? B3 O5 O4 2_566 . . 130.5(5) ? B3 O5 O6 2_566 . 2_566 35.6(5) ? B3 O5 O8 2_566 . 2_566 34.9(3) ? B3 O5 O9 2_566 . 1_554 144.2(7) ? O1 O5 O3 . . . 58.6(4) ? O1 O5 O4 . . . 61.4(4) ? O1 O5 O6 . . 2_566 113.7(3) ? O1 O5 O8 . . 2_566 103.2(3) ? O1 O5 O9 . . 1_554 59.5(4) ? O3 O5 O4 . . . 100.7(4) ? O3 O5 O6 . . 2_566 59.0(4) ? O3 O5 O8 . . 2_566 60.9(3) ? O3 O5 O9 . . 1_554 116.0(6) ? O4 O5 O6 . . 2_566 112.3(3) ? O4 O5 O8 . . 2_566 161.4(3) ? O4 O5 O9 . . 1_554 61.1(4) ? O6 O5 O8 2_566 . 2_566 62.3(4) ? O6 O5 O9 2_566 . 1_554 171.8(5) ? O8 O5 O9 2_566 . 1_554 122.2(3) ? Ca O6 Ca . . 2_566 103.7(3) ? Ca O6 B3 . . . 98.7(5) ? Ca O6 O1 . . 2_666 105.7(3) ? Ca O6 O3 . . 2_566 60.6(2) ? Ca O6 O5 . . 2_566 113.3(5) ? Ca O6 O8 . . . 112.1(2) ? Ca O6 B3 2_566 . . 93.3(7) ? Ca O6 O1 2_566 . 2_666 138.3(3) ? Ca O6 O3 2_566 . 2_566 99.5(5) ? Ca O6 O5 2_566 . 2_566 59.0(2) ? Ca O6 O8 2_566 . . 115.5(4) ? B3 O6 O1 . . 2_666 110.5(7) ? B3 O6 O3 . . 2_566 38.2(4) ? B3 O6 O5 . . 2_566 35.5(5) ? B3 O6 O8 . . . 31.5(7) ? O1 O6 O3 2_666 . 2_566 120.6(3) ? O1 O6 O5 2_666 . 2_566 130.1(3) ? O1 O6 O8 2_666 . . 79.3(4) ? O3 O6 O5 2_566 . 2_566 60.8(4) ? O3 O6 O8 2_566 . . 60.1(3) ? O5 O6 O8 2_566 . . 58.1(3) ? Ca O7 B1 . . 1_545 139.0(3) ? Ca O7 O2 . . 2_666 107.2(3) ? Ca O7 O3 . . 2_566 52.8(2) ? Ca O7 O8 . . 1_554 97.23(17) ? Ca O7 O8 . . 2_556 108.4(5) ? B1 O7 O2 1_545 . 2_666 71.6(4) ? B1 O7 O3 1_545 . 2_566 90.9(4) ? B1 O7 O8 1_545 . 1_554 123.6(4) ? B1 O7 O8 1_545 . 2_556 70.4(4) ? O2 O7 O3 2_666 . 2_566 119.1(3) ? O2 O7 O8 2_666 . 1_554 91.4(5) ? O2 O7 O8 2_666 . 2_556 140.4(3) ? O3 O7 O8 2_566 . 1_554 140.9(4) ? O3 O7 O8 2_566 . 2_556 72.0(4) ? O8 O7 O8 1_554 . 2_556 100.6(3) ? B3 O8 O2 . . 1_545 128.5(6) ? B3 O8 O3 . . 2_566 36.0(4) ? B3 O8 O5 . . 2_566 36.1(5) ? B3 O8 O6 . . . 32.7(8) ? B3 O8 O7 . . 1_556 112.2(6) ? B3 O8 O7 . . 2_556 100.7(9) ? O2 O8 O3 1_545 . 2_566 107.7(3) ? O2 O8 O5 1_545 . 2_566 164.5(3) ? O2 O8 O6 1_545 . . 106.1(4) ? O2 O8 O7 1_545 . 1_556 118.8(3) ? O2 O8 O7 1_545 . 2_556 95.2(3) ? O3 O8 O5 2_566 . 2_566 60.6(3) ? O3 O8 O6 2_566 . . 58.1(3) ? O3 O8 O7 2_566 . 1_556 127.6(6) ? O3 O8 O7 2_566 . 2_556 73.6(4) ? O5 O8 O6 2_566 . . 59.6(3) ? O5 O8 O7 2_566 . 1_556 76.2(3) ? O5 O8 O7 2_566 . 2_556 91.0(5) ? O6 O8 O7 . . 1_556 123.1(2) ? O6 O8 O7 . . 2_556 131.0(5) ? O7 O8 O7 1_556 . 2_556 79.4(3) ? Ca O9 B2 2_566 . 1_556 95.3(10) ? Ca O9 O1 2_566 . 1_556 123.1(6) ? Ca O9 O2 2_566 . . 95.7(2) ? Ca O9 O4 2_566 . 1_556 94.2(4) ? Ca O9 O4 2_566 . 2_666 112.5(2) ? Ca O9 O5 2_566 . 1_556 61.8(4) ? B2 O9 O1 1_556 . 1_556 35.0(6) ? B2 O9 O2 1_556 . . 154.5(3) ? B2 O9 O4 1_556 . 1_556 35.2(4) ? B2 O9 O4 1_556 . 2_666 127.0(8) ? B2 O9 O5 1_556 . 1_556 36.5(9) ? O1 O9 O2 1_556 . . 121.7(3) ? O1 O9 O4 1_556 . 1_556 61.25(18) ? O1 O9 O4 1_556 . 2_666 120.1(5) ? O1 O9 O5 1_556 . 1_556 61.7(4) ? O2 O9 O4 . . 1_556 164.2(6) ? O2 O9 O4 . . 2_666 68.6(3) ? O2 O9 O5 . . 1_556 137.6(4) ? O4 O9 O4 1_556 . 2_666 96.2(4) ? O4 O9 O5 1_556 . 1_556 58.3(4) ? O4 O9 O5 2_666 . 1_556 151.4(2) ? 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 Ca B2 . . 2.977(17) ? Ca B2 . 2_565 2.930(13) ? Ca B3 . 2_566 2.968(6) ? Ca O3 . 2_566 2.414(8) ? Ca O4 . . 2.364(13) ? Ca O5 . . 2.407(5) ? Ca O5 . 2_565 2.453(5) ? Ca O6 . . 2.417(5) ? Ca O6 . 2_566 2.492(7) ? Ca O7 . . 2.383(6) ? Ca O9 . 2_566 2.395(11) ? B1 B2 . . 2.446(10) ? B1 B3 . 2_566 2.49(2) ? B1 O1 . . 1.380(16) ? B1 O2 . . 1.427(12) ? B1 O3 . . 1.31(2) ? B1 O5 . . 2.741(12) ? B1 O7 . 1_565 2.914(8) ? B2 B3 . 2_566 2.64(3) ? B2 O1 . . 1.458(12) ? B2 O3 . . 2.833(17) ? B2 O4 . . 1.458(7) ? B2 O5 . . 1.48(3) ? B2 O9 . 1_554 1.481(14) ? B3 O1 . 2_566 2.95(2) ? B3 O3 . 2_566 1.515(14) ? B3 O5 . 2_566 1.471(17) ? B3 O6 . . 1.475(16) ? B3 O8 . . 1.427(10) ? O1 O2 . . 2.384(6) ? O1 O3 . . 2.378(17) ? O1 O4 . . 2.440(6) ? O1 O5 . . 2.451(16) ? O1 O6 . 2_666 2.737(17) ? O1 O9 . 1_554 2.398(6) ? O2 O2 . 2_676 2.906(9) ? O2 O3 . . 2.361(15) ? O2 O7 . 2_666 2.578(17) ? O2 O8 . 1_565 2.756(12) ? O2 O9 . . 2.815(9) ? O3 O5 . . 2.410(6) ? O3 O6 . 2_566 2.368(14) ? O3 O7 . 2_566 2.931(14) ? O3 O8 . 2_566 2.417(11) ? O4 O5 . . 2.323(14) ? O4 O9 . 1_554 2.393(6) ? O4 O9 . 2_666 2.730(15) ? O5 O6 . 2_566 2.397(16) ? O5 O8 . 2_566 2.359(13) ? O5 O9 . 1_554 2.380(17) ? O6 O8 . . 2.459(6) ? O7 O8 . 1_554 2.619(8) ? O7 O8 . 2_556 2.769(14) ? 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 ? ? ? ? ? ? ? ? ? ? ? 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_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 0 2 0 933.54 720.96 4.23 o 1 2 0 333.55 333.36 4.37 o 0 3 0 531.05 567.45 4.54 o 1 3 0 154.95 251.00 3.16 o -1 5 0 704.72 679.48 6.63 o 0 5 0 0.71 0.03 0.37 < 1 5 0 337.39 310.91 4.41 o 2 5 0 279.46 277.68 4.30 o -1 6 0 61.40 72.80 2.46 o 0 6 0 48.96 47.66 1.91 o 1 6 0 184.19 189.80 3.76 o 2 6 0 8.92 4.73 0.69 o -1 7 0 752.18 728.47 8.36 o 0 7 0 467.86 462.35 6.38 o 1 7 0 63.33 57.84 2.38 o 2 7 0 72.43 73.09 2.60 o -1 8 0 356.22 347.35 5.98 o 0 8 0 443.89 413.36 6.46 o 1 8 0 196.54 186.64 4.52 o 2 8 0 127.64 129.43 3.68 o -1 9 0 9.47 11.94 1.77 o 0 9 0 6.02 7.97 1.54 o 1 9 0 105.77 113.53 5.20 o 2 9 0 33.02 28.25 2.68 o 3 9 0 72.82 56.96 3.75 o -1 10 0 14.56 10.68 1.34 o 0 10 0 1.17 0.47 0.55 < 1 10 0 3.32 3.46 0.81 o 2 10 0 0.91 1.49 0.68 < 3 10 0 10.89 7.19 1.54 o -2 -11 1 81.49 87.82 3.51 o -1 -11 1 112.01 111.65 3.88 o 0 -11 1 42.68 43.43 2.51 o 1 -11 1 24.53 22.80 2.83 o -3 -10 1 127.91 133.37 5.79 o -2 -10 1 99.47 84.01 3.32 o -1 -10 1 292.33 272.58 5.74 o 0 -10 1 163.21 176.61 4.61 o 1 -10 1 53.47 44.89 3.61 o -3 -9 1 116.89 114.71 5.00 o -2 -9 1 135.30 137.32 3.99 o -1 -9 1 112.88 120.23 3.63 o 0 -9 1 10.42 17.96 1.44 o 1 -9 1 6.83 7.53 1.51 o -2 -8 1 4.68 1.49 0.74 < -1 -8 1 61.12 50.21 3.11 o 0 -8 1 114.19 118.04 4.81 o 1 -8 1 30.68 27.37 2.63 o -2 -7 1 858.39 755.17 7.87 o -1 -7 1 160.70 160.69 3.66 o 0 -7 1 1.45 1.18 0.46 < 1 -7 1 42.33 57.21 3.55 o -2 -6 1 739.70 641.76 6.73 o -1 -6 1 419.35 448.73 5.65 o 0 -6 1 309.90 300.54 4.50 o 1 -6 1 281.87 320.21 7.30 o -2 -5 1 246.36 244.21 3.82 o -1 -5 1 826.68 881.64 7.01 o 0 -5 1 477.20 448.49 4.99 o -1 -4 1 220.24 254.06 3.36 o 0 -4 1 254.05 255.83 3.35 o -1 -3 1 113.01 71.03 1.54 o 0 -3 1 3755.73 3618.48 10.97 o -1 -2 1 2480.87 2455.91 10.21 o 0 -2 1 119.76 147.62 1.68 o 0 1 1 98.96 93.07 1.34 o 0 2 1 336.22 291.42 4.18 o 0 3 1 317.40 400.38 4.20 o 1 3 1 16.97 25.34 1.10 o -1 4 1 164.82 163.34 4.33 o 0 4 1 101.63 79.03 2.99 o 1 4 1 5.08 20.08 1.61 o -1 5 1 105.83 107.54 2.82 o 0 5 1 154.54 173.15 3.49 o 1 5 1 84.05 107.37 2.81 o 2 5 1 1404.12 1372.33 14.49 o -1 6 1 589.28 625.44 7.45 o 0 6 1 57.27 55.61 2.15 o 1 6 1 442.78 428.73 6.01 o 2 6 1 346.58 352.42 5.58 o -1 7 1 32.21 24.32 1.56 o 0 7 1 23.28 23.07 1.52 o 1 7 1 321.98 293.81 5.31 o 2 7 1 219.56 212.01 4.62 o -1 8 1 27.48 27.54 1.79 o 0 8 1 35.95 38.20 2.06 o 1 8 1 21.84 20.70 1.63 o 2 8 1 49.02 32.97 1.97 o -1 9 1 50.75 44.53 2.42 o 0 9 1 23.91 22.65 1.76 o 1 9 1 22.21 21.06 1.73 o 2 9 1 106.74 108.86 3.72 o -1 10 1 41.76 33.64 2.30 o 0 10 1 5.65 6.70 1.12 o 1 10 1 170.03 173.56 5.01 o 2 10 1 1.67 1.78 0.74 < -3 -11 2 24.06 32.05 3.07 o -2 -11 2 18.44 21.81 1.70 o -1 -11 2 30.77 29.63 1.96 o 0 -11 2 171.44 169.42 4.60 o -3 -10 2 103.89 94.56 4.74 o -2 -10 2 9.80 6.59 0.99 o 0 -10 2 0.93 0.82 0.55 < 1 -10 2 13.00 19.84 2.36 o -3 -9 2 241.66 247.71 6.99 o -2 -9 2 78.56 84.60 3.00 o -1 -9 2 0.76 0.39 0.45 < 0 -9 2 35.26 30.94 1.76 o 1 -9 2 107.36 95.08 4.63 o -2 -8 2 42.28 37.29 1.87 o -1 -8 2 247.49 239.51 4.49 o 0 -8 2 266.76 274.84 4.91 o 1 -8 2 62.29 53.58 3.56 o -3 -7 2 85.78 100.85 3.89 o -2 -7 2 132.29 136.26 3.20 o -1 -7 2 1.57 0.65 0.35 < 0 -7 2 13.02 11.24 0.97 o 1 -7 2 15.54 20.71 2.08 o -1 -6 2 54.20 55.27 1.83 o 0 -6 2 190.88 201.99 3.51 o 0 -5 2 420.12 414.00 6.35 o -1 -4 2 159.01 140.66 2.31 o 0 -4 2 591.16 574.08 4.71 o -1 -3 2 4.35 1.75 0.24 o 0 -3 2 692.75 688.13 6.03 o -1 -2 2 1444.84 1903.34 7.33 o 0 -2 2 1493.23 1933.32 8.13 o 0 0 2 2936.10 3590.78 10.13 o -1 1 2 426.41 528.46 3.71 o -1 2 2 89.51 96.97 1.89 o 0 2 2 17.40 23.52 0.96 o 0 3 2 2.91 1.96 0.52 o 1 3 2 1473.92 1688.73 9.58 o -1 4 2 617.64 547.36 5.93 o 0 4 2 1670.85 1650.96 10.17 o 1 4 2 1616.84 1698.33 10.65 o -1 5 2 0.82 4.12 0.65 o 0 5 2 90.77 85.82 2.72 o 1 5 2 89.47 78.88 2.55 o -1 6 2 5.90 7.53 0.89 o 0 6 2 98.66 91.06 4.10 o 1 6 2 80.02 64.88 3.47 o 2 6 2 4.47 4.24 1.08 o -1 7 2 43.59 41.96 2.10 o 0 7 2 44.47 44.35 2.18 o 1 7 2 624.61 576.31 7.82 o 2 7 2 6.43 4.48 0.81 o -1 8 2 10.34 14.37 1.37 o 0 8 2 968.56 950.41 10.64 o 1 8 2 556.61 549.88 8.35 o 2 8 2 288.07 279.89 5.85 o -1 9 2 168.49 169.47 4.78 o 0 9 2 44.92 43.15 2.47 o 1 9 2 78.70 73.00 3.32 o 2 9 2 116.07 102.44 3.80 o 0 10 2 110.73 118.39 6.09 o -2 -12 3 0.35 0.42 0.52 < -1 -12 3 0.11 0.41 0.56 < -3 -11 3 71.32 73.49 4.18 o -2 -11 3 0.02 0.23 0.58 < -1 -11 3 62.20 54.21 2.46 o 0 -11 3 77.86 90.68 4.64 o -2 -10 3 12.36 10.88 1.60 o -1 -10 3 77.28 83.37 3.99 o 0 -10 3 146.23 146.33 5.42 o -3 -9 3 27.93 26.51 2.28 o -1 -9 3 176.18 168.25 5.38 o -3 -8 3 5.94 6.60 1.13 o -2 -8 3 14.38 13.23 1.07 o -1 -8 3 0.05 0.29 0.39 < 0 -8 3 57.46 46.21 2.77 o -3 -7 3 10.26 8.93 1.20 o -2 -7 3 111.65 102.57 2.67 o -1 -7 3 197.75 201.61 3.59 o 0 -7 3 383.35 347.21 6.78 o -3 -6 3 333.29 312.23 6.15 o -2 -6 3 353.97 318.61 5.76 o -1 -6 3 1240.92 1326.13 8.32 o 0 -6 3 725.06 670.12 8.75 o -2 -5 3 4.74 5.62 0.78 o -1 -5 3 1254.98 1253.75 7.05 o 0 -5 3 1.51 2.74 0.61 o -2 -4 3 23.77 21.40 1.26 o -1 -4 3 314.16 312.72 3.04 o 0 -4 3 230.76 265.91 4.38 o -1 -3 3 364.23 387.90 2.51 o 0 -3 3 209.16 190.31 2.97 o -1 0 3 2579.27 2999.20 10.78 o -1 1 3 464.46 500.28 3.92 o 0 1 3 447.32 374.96 3.52 o -1 2 3 1102.81 1066.62 9.67 o 0 2 3 1052.25 1230.48 7.31 o -1 3 3 14.40 13.25 0.87 o 0 3 3 1582.10 1623.49 9.42 o 1 3 3 737.53 739.04 6.65 o -2 4 3 215.63 223.12 5.65 o -1 4 3 124.41 120.62 2.87 o 0 4 3 5.42 6.06 0.71 o 1 4 3 312.84 292.98 4.59 o -2 5 3 452.17 451.23 6.13 o -1 5 3 197.25 189.47 3.91 o 0 5 3 343.91 391.41 5.86 o 1 5 3 55.38 42.30 1.98 o -2 6 3 165.22 164.79 6.08 o -1 6 3 1675.23 1661.58 12.55 o 0 6 3 90.71 84.15 2.96 o 1 6 3 0.48 0.89 0.50 < 2 6 3 1.69 2.79 0.94 < -2 7 3 2.08 1.68 0.60 < -1 7 3 0.13 0.30 0.43 < 0 7 3 0.96 1.04 0.58 < 1 7 3 60.86 57.53 2.59 o 2 7 3 37.64 24.92 1.78 o -2 8 3 36.25 32.53 2.06 o -1 8 3 26.77 27.19 1.89 o 0 8 3 3.82 2.99 0.81 o 1 8 3 59.64 60.06 2.90 o 2 8 3 56.66 62.56 2.92 o -2 9 3 222.39 226.66 7.86 o -1 9 3 4.81 9.09 1.81 o 0 9 3 1.18 2.38 1.17 < 1 9 3 2.56 1.94 1.08 < 2 9 3 2.68 1.08 0.99 < -3 -12 4 142.56 145.95 5.74 o -2 -12 4 174.55 195.07 4.58 o -1 -12 4 103.46 105.09 4.85 o 0 -12 4 61.64 49.22 3.23 o -3 -11 4 22.92 22.97 2.23 o -2 -11 4 32.81 37.56 1.95 o -1 -11 4 24.37 24.40 2.32 o 0 -11 4 46.30 52.69 3.25 o -3 -10 4 9.29 10.08 1.47 o -2 -10 4 3.76 0.59 0.44 < -1 -10 4 21.71 26.81 2.28 o 0 -10 4 69.80 61.42 3.34 o -3 -9 4 375.15 406.35 8.57 o -2 -9 4 65.43 62.27 2.19 o -1 -9 4 92.67 101.52 2.75 o 0 -9 4 18.20 16.78 1.70 o -3 -8 4 76.76 65.05 3.14 o -2 -8 4 78.23 96.29 3.55 o -1 -8 4 365.42 345.28 6.65 o 0 -8 4 9.02 5.01 0.94 o -3 -7 4 6.55 1.94 0.58 o -2 -7 4 56.22 50.56 2.35 o -1 -7 4 7.32 5.49 0.60 o 0 -7 4 40.16 44.70 2.35 o -3 -6 4 79.94 78.18 2.87 o -2 -6 4 7.63 6.56 0.84 o -1 -6 4 11.58 9.72 0.68 o 0 -6 4 17.40 17.22 1.31 o -2 -5 4 493.58 487.97 6.09 o -1 -5 4 60.69 59.80 2.03 o 0 -5 4 32.30 30.63 1.58 o -2 -4 4 1152.90 1151.06 7.42 o -1 -4 4 378.07 375.81 3.82 o 0 -4 4 3.00 4.64 0.55 o -2 -3 4 207.40 194.71 2.56 o 0 -3 4 29.68 30.62 1.09 o 0 -1 4 2.58 0.57 0.17 o -1 0 4 95.92 107.49 1.54 o 0 0 4 479.96 476.23 5.07 o -1 1 4 25.07 30.18 1.45 o -1 2 4 1.46 0.09 0.21 < 0 2 4 38.53 41.15 2.03 o -2 3 4 56.39 51.59 2.61 o -1 3 4 111.82 111.51 3.76 o 0 3 4 65.20 73.15 3.12 o -2 4 4 141.66 156.16 3.51 o -1 4 4 10.98 14.59 1.60 o 0 4 4 123.13 94.61 2.68 o 1 4 4 158.66 165.62 3.62 o -2 5 4 4.08 3.60 0.65 o -1 5 4 80.65 75.56 2.57 o 0 5 4 693.67 768.80 8.44 o 1 5 4 0.15 0.37 0.40 < -2 6 4 20.63 21.11 1.49 o -1 6 4 351.34 342.55 5.84 o 1 6 4 8.37 4.79 0.82 o -2 7 4 26.29 30.51 1.93 o -1 7 4 91.17 85.96 3.19 o 0 7 4 134.31 148.03 4.23 o 1 7 4 177.40 179.98 4.68 o 2 7 4 205.58 243.87 8.15 o -2 8 4 187.73 187.66 4.92 o -1 8 4 204.79 217.49 5.37 o 0 8 4 41.08 41.92 2.44 o 1 8 4 143.31 147.93 4.63 o 2 8 4 329.35 320.59 6.74 o -1 9 4 32.08 34.46 3.32 o 0 9 4 1.10 1.19 1.04 < -4 -10 5 82.77 88.91 4.22 o -3 -10 5 44.66 62.80 3.13 o -2 -10 5 73.02 74.03 2.31 o -1 -10 5 0.59 0.92 0.63 < -4 -9 5 5.92 7.82 1.22 o -3 -9 5 83.77 84.92 3.43 o -2 -9 5 26.85 29.04 1.93 o -1 -9 5 36.49 39.26 2.40 o 0 -9 5 149.71 149.73 4.47 o -4 -8 5 2.10 3.70 0.84 o -3 -8 5 3.00 1.61 0.61 < -2 -8 5 10.75 6.46 0.88 o -1 -8 5 17.54 27.65 1.90 o 0 -8 5 2.50 1.04 0.50 < -3 -7 5 20.80 20.60 1.56 o -2 -7 5 0.09 0.48 0.36 < -1 -7 5 55.70 59.76 2.41 o 0 -7 5 31.41 32.93 1.84 o -3 -6 5 101.14 105.71 2.91 o -2 -6 5 117.05 130.69 2.95 o -1 -6 5 55.74 63.05 2.08 o 0 -6 5 161.22 144.39 3.34 o 0 -5 5 391.96 351.09 4.41 o -3 -4 5 20.53 21.04 1.08 o 0 -4 5 75.26 75.95 1.88 o -2 -1 5 0.39 0.12 0.15 < 0 -1 5 370.39 329.87 3.70 o -2 0 5 3.19 0.78 0.31 < -1 0 5 16.40 13.39 0.60 o 0 0 5 69.97 55.14 1.85 o -2 1 5 10.10 8.69 0.93 o -1 1 5 58.36 58.62 1.51 o 0 1 5 989.50 932.55 8.98 o -2 2 5 234.20 228.09 5.01 o -1 2 5 988.84 1036.96 7.24 o 0 2 5 2129.72 2170.73 10.73 o 1 2 5 2.08 3.33 0.70 o -2 3 5 52.05 51.40 2.61 o -1 3 5 498.73 579.57 6.11 o 0 3 5 71.08 52.68 1.87 o 1 3 5 295.53 281.58 6.36 o -2 4 5 26.25 21.03 1.33 o -1 4 5 571.99 586.16 6.77 o 0 4 5 505.02 484.67 6.29 o 1 4 5 9.92 7.56 1.22 o -2 5 5 49.66 48.87 2.96 o -1 5 5 343.52 337.48 7.65 o 0 5 5 66.66 76.93 4.01 o 1 5 5 100.60 106.33 4.57 o -2 6 5 54.33 61.35 2.58 o -1 6 5 391.87 361.40 6.26 o 0 6 5 141.06 141.92 4.13 o 1 6 5 69.72 73.38 2.86 o -2 7 5 8.54 6.78 1.49 o -1 7 5 41.82 46.98 3.59 o 0 7 5 49.00 56.31 3.83 o 1 7 5 123.11 102.87 3.59 o -2 8 5 16.59 12.96 1.44 o -1 8 5 24.45 25.76 2.00 o 0 8 5 44.76 35.75 2.31 o 1 8 5 102.95 107.51 4.08 o -4 -8 6 3.66 2.19 0.64 o -3 -8 6 127.90 142.19 3.57 o -4 -7 6 88.43 85.20 2.93 o -3 -7 6 21.88 27.95 1.43 o -3 -6 6 0.50 1.36 0.34 o 0 -6 6 14.80 12.64 0.95 o -3 -5 6 50.22 59.53 1.46 o 0 -5 6 23.00 19.52 0.91 o 0 -4 6 142.41 125.93 1.71 o 0 -2 6 133.37 124.59 1.91 o -3 -1 6 643.83 611.89 5.75 o -2 -1 6 384.48 397.92 3.47 o 0 -1 6 451.79 444.45 4.70 o -3 0 6 129.11 122.42 3.04 o -2 0 6 196.08 193.00 3.42 o -3 1 6 182.98 200.46 4.45 o -2 1 6 192.21 181.55 3.93 o -1 1 6 34.10 30.75 1.16 o 0 1 6 5.60 2.91 0.62 o -3 2 6 73.23 75.15 3.17 o -2 2 6 22.43 20.23 1.55 o -1 2 6 73.15 68.23 1.95 o 0 2 6 47.60 53.09 2.48 o 1 2 6 35.14 26.17 1.85 o -3 3 6 83.30 80.37 3.64 o -2 3 6 55.28 58.25 2.03 o -1 3 6 76.81 80.83 2.34 o 0 3 6 78.42 83.42 2.48 o 1 3 6 5.52 5.80 0.98 o -3 4 6 158.32 150.48 5.35 o -2 4 6 206.37 237.96 4.43 o -1 4 6 266.05 260.14 4.61 o 0 4 6 31.52 27.10 1.58 o 1 4 6 7.98 10.07 1.39 o -3 5 6 8.16 10.08 1.52 o -2 5 6 124.19 122.07 3.46 o -1 5 6 37.72 40.43 1.99 o 0 5 6 77.40 73.99 2.77 o 1 5 6 3.23 3.45 0.96 o -3 6 6 3.86 3.77 1.04 o -2 6 6 175.51 197.10 4.65 o -1 6 6 77.40 69.34 2.83 o 0 6 6 2.43 0.43 0.53 < 1 6 6 67.40 78.15 2.98 o -2 7 6 123.42 105.90 3.68 o -1 7 6 94.22 96.65 3.52 o 0 7 6 4.70 3.31 0.82 o 1 7 6 46.36 35.34 2.20 o -4 -5 7 14.03 13.19 0.69 o 0 -2 7 41.09 41.25 1.13 o -3 -1 7 25.22 22.37 1.02 o 0 -1 7 182.94 194.07 3.21 o -3 0 7 0.13 0.10 0.27 < -2 0 7 8.65 8.46 0.79 o -1 0 7 11.77 8.07 0.74 o 0 0 7 191.08 166.74 3.78 o -3 1 7 303.60 305.89 5.45 o -2 1 7 2.55 3.03 0.60 o -1 1 7 36.45 43.60 1.99 o 0 1 7 77.27 66.54 2.81 o -1 2 7 50.92 58.59 2.63 o 0 2 7 79.33 80.00 3.31 o -3 3 7 14.29 8.70 1.22 o -2 3 7 0.01 0.16 0.48 < -1 3 7 2.05 4.46 0.65 o 0 3 7 128.67 120.72 4.50 o 1 3 7 290.22 233.18 5.91 o -3 4 7 1.06 1.04 0.65 < -2 4 7 20.25 22.87 2.08 o -1 4 7 28.85 27.06 2.21 o -3 5 7 30.73 20.81 2.09 o -2 5 7 0.17 0.96 0.51 < -1 5 7 20.00 24.99 1.63 o 0 5 7 42.95 42.35 2.13 o 1 5 7 397.02 394.21 8.93 o -3 6 7 73.26 81.84 4.40 o -2 6 7 151.08 188.54 4.68 o -1 6 7 69.89 66.08 2.78 o 0 6 7 208.66 224.22 5.05 o 1 6 7 23.42 23.40 2.34 o -3 7 7 127.09 129.34 5.93 o -2 7 7 0.73 0.82 0.58 < -1 7 7 18.37 19.72 1.69 o 0 7 7 25.82 25.42 1.89 o -4 -2 8 22.43 30.47 1.03 o -4 -1 8 73.61 80.79 2.27 o 0 -1 8 121.58 127.32 2.58 o -3 0 8 30.85 30.74 1.53 o -3 1 8 2.74 3.47 0.66 o -2 1 8 141.51 159.20 4.06 o -1 1 8 20.10 18.99 1.37 o 0 1 8 28.80 29.35 1.94 o -3 2 8 3.82 1.61 0.55 < -2 2 8 34.75 46.15 2.37 o -1 2 8 140.90 155.73 4.24 o 0 2 8 12.50 10.42 1.28 o -3 3 8 24.63 26.05 2.01 o -2 3 8 172.21 222.16 5.81 o -1 3 8 106.66 110.04 2.82 o 0 3 8 240.96 287.22 6.98 o -3 4 8 288.71 339.58 7.70 o -2 4 8 55.77 57.17 2.17 o -1 4 8 42.58 44.13 1.97 o 0 4 8 37.91 40.48 2.73 o -3 5 8 1.71 1.64 0.77 < -2 5 8 0.00 0.05 0.54 < -1 5 8 29.44 37.90 2.00 o 0 5 8 104.73 75.36 4.00 o 1 5 8 30.18 29.69 2.49 o -3 6 8 30.26 32.21 2.77 o -2 6 8 93.18 97.08 3.37 o -1 6 8 45.68 44.49 2.31 o 0 6 8 1.83 3.90 0.82 o 1 6 8 0.01 0.21 0.73 < -3 2 9 82.00 103.07 3.61 o -2 3 9 8.23 7.56 1.15 o -1 3 9 9.21 6.96 1.11 o -3 4 9 16.14 19.59 1.91 o -2 4 9 6.57 9.46 1.40 o -1 4 9 5.24 6.53 1.16 o 0 4 9 12.00 11.98 1.58 o -3 5 9 82.40 78.28 4.03 o -2 5 9 16.07 19.61 1.44 o -1 5 9 12.66 13.19 1.22 o -3 6 9 40.43 36.67 2.97 o -2 6 9 25.98 31.00 1.93 o -1 6 9 0.94 0.16 0.52 < 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_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_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_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_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 ? ? ? ? ? ? ? ? ? ? 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_ _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 ? ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? _cod_database_fobs_code 2022903