#------------------------------------------------------------------------------ #$Date: 2024-08-17 01:46:53 +0300 (Sat, 17 Aug 2024) $ #$Revision: 294155 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/68/7716850.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7716850 loop_ _publ_author_name 'Dadmehr, Parvaneh' 'Bikas, Rahman' 'Lis, Tadeusz' _publ_section_title ; Chemical CO2 fixation by cyanido bridged heterometallic Zn(II)-Mn(II) 2D coordination polymer ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D4DT01630K _journal_year 2024 _chemical_formula_moiety 'C10 H10 O4' _chemical_formula_sum 'C10 H10 O4' _chemical_formula_weight 194.18 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method SHELXL-2013 _audit_update_record ; 2024-03-15 deposited with the CCDC. 2024-08-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.446(4) _cell_length_b 5.5867(18) _cell_length_c 21.823(6) _cell_measurement_reflns_used 4767 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 22 _cell_measurement_theta_min 1.8 _cell_volume 1761.2(9) _computing_cell_refinement 'CrysAlisPro 1.171.42.42a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.42a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.42a (Rigaku OD, 2022)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 150' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix-Arc 150' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_unetI/netI 0.0533 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 13456 _diffrn_reflns_point_group_measured_fraction_full 0.949 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_theta_full 25.500 _diffrn_reflns_theta_max 29.999 _diffrn_reflns_theta_min 1.866 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.42a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.465 _exptl_crystal_description irregular _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.321 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.057 _refine_ls_abs_structure_details ; Flack x determined using 1741 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.3(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 343 _refine_ls_number_reflns 4831 _refine_ls_number_restraints 205 _refine_ls_restrained_S_all 1.116 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0557 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+1.0874P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1396 _refine_ls_wR_factor_ref 0.1438 _reflns_Friedel_coverage 0.840 _reflns_Friedel_fraction_full 0.895 _reflns_Friedel_fraction_max 0.880 _reflns_number_gt 4316 _reflns_number_total 4831 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt01630k2.cif _cod_data_source_block ftco22 _cod_depositor_comments ; The following automatic conversions were performed: data item '_atom_sites_solution_primary' value 'direct methods' was changed to 'direct'. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 7716850 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.970 _shelx_estimated_absorpt_t_max 0.995 _oxdiff_exptl_absorpt_empirical_full_min 0.855 _oxdiff_exptl_absorpt_empirical_full_max 1.178 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL ftco22 in Pna2(1) CELL 0.71073 14.446 5.5867 21.823 90.000 90.000 90.000 ZERR 8.000 0.004 0.0018 0.006 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, Z SYMM 1/2-X, 1/2+Y, 1/2+Z SFAC C H O UNIT 80 80 32 acta 51 TEMP -173 size 0.04 0.21 0.27 L.S. 20 BOND $H omit -4 60 FMAP 2 PLAN 20 WGHT 0.059800 1.087400 FVAR 2.17954 0.79643 0.83195 part 1 C1A 1 0.506361 0.307324 0.227540 21.00000 0.00465 0.00579 = 0.00686 0.00171 0.00184 0.00045 C2A 1 0.527010 0.116568 0.188643 21.00000 0.01147 0.00739 = 0.01131 -0.00063 -0.00079 0.00520 AFIX 43 H2A 2 0.568036 -0.006263 0.201633 21.00000 -1.20000 AFIX 0 C3A 1 0.486930 0.107490 0.130468 21.00000 0.01329 0.01327 = 0.01651 -0.00093 0.00099 -0.00144 AFIX 43 H3A 2 0.500352 -0.022771 0.103933 21.00000 -1.20000 AFIX 0 C4A 1 0.427476 0.288106 0.111172 21.00000 0.01100 0.01812 = 0.01853 0.00483 -0.00216 -0.00765 AFIX 43 H4A 2 0.401698 0.284176 0.071137 21.00000 -1.20000 AFIX 0 C5A 1 0.406070 0.474286 0.150878 21.00000 0.00705 0.01449 = 0.01999 0.00449 -0.00150 0.00287 AFIX 43 H5A 2 0.363907 0.595019 0.138198 21.00000 -1.20000 AFIX 0 C6A 1 0.445588 0.486576 0.209113 21.00000 0.00778 0.00539 = 0.01583 -0.00001 0.00098 0.00231 AFIX 43 H6A 2 0.431198 0.615586 0.235826 21.00000 -1.20000 AFIX 0 O1A 3 0.549522 0.303362 0.283619 21.00000 0.01548 0.00882 = 0.01168 -0.00111 -0.00350 0.00310 C7A 1 0.530892 0.497258 0.324303 21.00000 0.01084 0.00501 = 0.01191 -0.00193 0.00138 0.00127 AFIX 23 H7A1 2 0.463791 0.506054 0.333244 21.00000 -1.20000 H7A2 2 0.550371 0.650474 0.305509 21.00000 -1.20000 AFIX 0 C8A 1 0.584572 0.452793 0.382558 21.00000 0.01097 0.00719 = 0.01739 0.00052 -0.00092 -0.00153 AFIX 13 H8A 2 0.652064 0.434025 0.373580 21.00000 -1.20000 AFIX 0 O2A 3 0.548543 0.241065 0.412297 21.00000 0.02052 0.00715 = 0.01169 0.00115 0.00150 -0.00351 C9A 1 0.501638 0.300506 0.463148 21.00000 0.01682 0.02309 = 0.00998 0.00149 -0.00225 -0.00283 O3A 3 0.459617 0.162822 0.494579 21.00000 0.03446 0.03254 = 0.02756 0.01035 0.00424 -0.01643 O4A 3 0.505118 0.538728 0.473253 21.00000 0.01982 0.01845 = 0.02043 -0.00418 0.00325 -0.00333 C10A 1 0.568855 0.649364 0.430472 21.00000 0.01551 0.01302 = 0.01676 -0.00244 0.00064 -0.00078 AFIX 23 H10A 2 0.627552 0.693818 0.450935 21.00000 -1.20000 H10B 2 0.541325 0.793964 0.411616 21.00000 -1.20000 AFIX 66 same 0.005 c1a > c10a same 0.005 c1c > c10c same 0.005 c1b > c10b same 0.005 c1d > c10d part 2 C1C 1 0.502042 0.192620 0.226245 -21.00000 0.03099 C2C 1 0.443612 0.007636 0.208404 -21.00000 0.05456 AFIX 43 H2C 2 0.433603 -0.124641 0.234945 -21.00000 -1.20000 AFIX 65 C3C 1 0.399827 0.016192 0.151729 -21.00000 0.06241 AFIX 43 H3C 2 0.359893 -0.110238 0.139535 -21.00000 -1.20000 AFIX 65 C4C 1 0.414472 0.209732 0.112895 -21.00000 0.04163 AFIX 43 H4C 2 0.384547 0.215579 0.074160 -21.00000 -1.20000 AFIX 65 C5C 1 0.472902 0.394719 0.130735 -21.00000 0.07978 AFIX 43 H5C 2 0.482910 0.526995 0.104194 -21.00000 -1.20000 AFIX 65 C6C 1 0.516687 0.386165 0.187410 -21.00000 0.04695 AFIX 43 H6C 2 0.556621 0.512595 0.199603 -21.00000 -1.20000 AFIX 0 O1C 3 0.537399 0.200001 0.284552 -21.00000 0.05864 C7C 1 0.522500 0.001946 0.324168 -21.00000 0.06041 AFIX 23 H7C1 2 0.544627 -0.147488 0.304674 -21.00000 -1.20000 H7C2 2 0.455701 -0.015507 0.333262 -21.00000 -1.20000 AFIX 0 C8C 1 0.575905 0.049956 0.382435 -21.00000 0.07585 AFIX 13 H8C 2 0.643538 0.064979 0.373457 -21.00000 -1.20000 AFIX 0 O2C 3 0.541707 0.265713 0.411035 -21.00000 0.07246 C9C 1 0.497819 0.215479 0.463650 -21.00000 0.07925 O3C 3 0.452005 0.355701 0.491827 -21.00000 0.10779 O4C 3 0.496738 -0.022551 0.473832 -21.00000 0.06141 C10C 1 0.559294 -0.140893 0.431595 -21.00000 0.04831 AFIX 23 H10C 2 0.530536 -0.285954 0.413803 -21.00000 -1.20000 H10D 2 0.617844 -0.186112 0.452133 -21.00000 -1.20000 AFIX 0 part 3 C1B 1 0.752627 0.194032 0.772539 31.00000 0.00980 0.01038 = 0.01782 0.00067 -0.00022 0.00287 C2B 1 0.692997 0.012149 0.790677 31.00000 0.01122 0.01380 = 0.01810 -0.00046 -0.00144 -0.00084 AFIX 43 H2B 2 0.678396 -0.115690 0.763648 31.00000 -1.20000 AFIX 0 C3B 1 0.654802 0.021282 0.849756 31.00000 0.01522 0.01118 = 0.01996 0.00351 0.00525 -0.00229 AFIX 43 H3B 2 0.613613 -0.101416 0.862601 31.00000 -1.20000 AFIX 0 C4B 1 0.676055 0.205705 0.889608 31.00000 0.01689 0.01421 = 0.01332 0.00005 0.00455 -0.00161 AFIX 43 H4B 2 0.650491 0.208308 0.929710 31.00000 -1.20000 AFIX 0 C5B 1 0.735189 0.387339 0.870455 31.00000 0.01445 0.01021 = 0.01420 -0.00200 0.00009 0.00157 AFIX 43 H5B 2 0.749748 0.514885 0.897585 31.00000 -1.20000 AFIX 0 C6B 1 0.773179 0.383759 0.811908 31.00000 0.01110 0.00991 = 0.01717 0.00155 -0.00045 -0.00107 AFIX 43 H6B 2 0.812809 0.509429 0.798799 31.00000 -1.20000 AFIX 0 O1B 3 0.796246 0.201166 0.716501 31.00000 0.01587 0.01089 = 0.01177 -0.00367 0.00119 -0.01030 C7B 1 0.778480 0.010835 0.674992 31.00000 0.01195 0.00896 = 0.01257 -0.00115 -0.00095 -0.00249 AFIX 23 H7B1 2 0.711471 0.001388 0.665797 31.00000 -1.20000 H7B2 2 0.798338 -0.143444 0.693027 31.00000 -1.20000 AFIX 0 C8B 1 0.832525 0.061623 0.617146 31.00000 0.01052 0.00657 = 0.01169 0.00042 -0.00180 0.00096 AFIX 13 H8B 2 0.899660 0.083552 0.626802 31.00000 -1.20000 AFIX 0 O2B 3 0.795729 0.274119 0.588155 31.00000 0.02238 0.01008 = 0.01296 0.00185 0.00313 0.00408 C9B 1 0.752646 0.217789 0.535759 31.00000 0.01449 0.02123 = 0.01733 0.00195 -0.00096 0.00745 O3B 3 0.710371 0.355162 0.504780 31.00000 0.03043 0.02649 = 0.02050 0.00703 -0.00453 0.01223 O4B 3 0.760470 -0.017155 0.523066 31.00000 0.02390 0.01880 = 0.01678 -0.00441 -0.00999 0.00629 C10B 1 0.820032 -0.131535 0.567987 31.00000 0.02102 0.01147 = 0.01339 -0.00069 -0.00164 0.00634 AFIX 23 H10E 2 0.880215 -0.176776 0.549638 31.00000 -1.20000 H10F 2 0.790323 -0.276259 0.585266 31.00000 -1.20000 AFIX 66 part 4 C1D 1 0.761102 0.281422 0.769804 -31.00000 0.08034 C2D 1 0.783538 0.098317 0.810290 -31.00000 0.05269 AFIX 43 H2D 2 0.824123 -0.026217 0.797765 -31.00000 -1.20000 AFIX 65 C3D 1 0.746590 0.097423 0.869100 -31.00000 0.02446 AFIX 43 H3D 2 0.761924 -0.027723 0.896770 -31.00000 -1.20000 AFIX 65 C4D 1 0.687207 0.279634 0.887426 -31.00000 0.02479 AFIX 43 H4D 2 0.661955 0.279022 0.927620 -31.00000 -1.20000 AFIX 65 C5D 1 0.664771 0.462741 0.846941 -31.00000 0.04792 AFIX 43 H5D 2 0.624185 0.587275 0.859465 -31.00000 -1.20000 AFIX 65 C6D 1 0.701718 0.463638 0.788130 -31.00000 0.06280 AFIX 43 H6D 2 0.686384 0.588784 0.760460 -31.00000 -1.20000 AFIX 0 O1D 3 0.809979 0.298497 0.716056 -31.00000 0.03353 C7D 1 0.789657 0.490528 0.675458 -31.00000 0.04039 AFIX 23 H7D1 2 0.809217 0.644697 0.693697 -31.00000 -1.20000 H7D2 2 0.722328 0.497744 0.667202 -31.00000 -1.20000 AFIX 0 C8D 1 0.842241 0.443935 0.616830 -31.00000 0.02157 AFIX 13 H8D 2 0.909410 0.418364 0.625771 -31.00000 -1.20000 AFIX 0 O2D 3 0.803805 0.236382 0.586542 -31.00000 0.06037 C9D 1 0.755636 0.302078 0.536754 -31.00000 0.09617 O3D 3 0.713830 0.166568 0.504607 -31.00000 0.03508 O4D 3 0.769582 0.535283 0.523933 -31.00000 0.03356 C10D 1 0.830100 0.642465 0.569218 -31.00000 0.03307 AFIX 23 H10G 2 0.801314 0.786176 0.587695 -31.00000 -1.20000 H10H 2 0.890272 0.687774 0.550865 -31.00000 -1.20000 AFIX 0 HKLF 4 REM ftco22 in Pna2(1) REM R1 = 0.0557 for 4316 Fo > 4sig(Fo) and 0.0632 for all 4831 data REM 343 parameters refined using 205 restraints END WGHT 0.0639 1.0677 REM Highest difference peak 0.321, deepest hole -0.272, 1-sigma level 0.057 Q1 1 0.5058 0.1211 0.1608 11.00000 0.05 0.32 Q2 1 0.8164 0.0604 0.6485 11.00000 0.05 0.32 Q3 1 0.6752 0.0142 0.8207 11.00000 0.05 0.31 Q4 1 0.8007 0.0260 0.6428 11.00000 0.05 0.30 Q5 1 0.5587 0.4677 0.3527 11.00000 0.05 0.29 Q6 1 0.4787 0.3965 0.2208 11.00000 0.05 0.27 Q7 1 0.4212 -0.0852 0.1716 11.00000 0.05 0.23 Q8 1 0.5234 0.2624 0.1974 11.00000 0.05 0.23 Q9 1 0.4214 0.5124 0.0291 11.00000 0.05 0.23 Q10 1 0.7478 0.3817 0.8410 11.00000 0.05 0.22 Q11 1 0.7755 0.2592 0.7975 11.00000 0.05 0.21 Q12 1 0.4326 0.4806 0.1789 11.00000 0.05 0.21 Q13 1 0.5186 0.3036 0.2566 11.00000 0.05 0.21 Q14 1 0.6675 0.0973 0.8683 11.00000 0.05 0.20 Q15 1 0.5604 -0.0390 0.4509 11.00000 0.05 0.20 Q16 1 0.4187 0.0590 0.2091 11.00000 0.05 0.20 Q17 1 0.4667 0.1996 0.1277 11.00000 0.05 0.20 Q18 1 0.6809 0.5138 0.6526 11.00000 0.05 0.20 Q19 1 0.4825 -0.1334 0.0778 11.00000 0.05 0.19 Q20 1 0.7202 0.1393 0.4605 11.00000 0.05 0.19 ; _shelx_res_checksum 86473 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.5064(2) 0.3073(6) 0.22754(14) 0.0058(6) Uani 0.796(4) 1 d D . P A 1 C2A C 0.5270(3) 0.1166(6) 0.18864(16) 0.0101(7) Uani 0.796(4) 1 d D . P A 1 H2A H 0.5680 -0.0063 0.2016 0.012 Uiso 0.796(4) 1 calc R U P A 1 C3A C 0.4869(3) 0.1075(7) 0.13047(17) 0.0144(8) Uani 0.796(4) 1 d D . P A 1 H3A H 0.5004 -0.0228 0.1039 0.017 Uiso 0.796(4) 1 calc R U P A 1 C4A C 0.4275(3) 0.2881(8) 0.11117(19) 0.0159(9) Uani 0.796(4) 1 d D . P A 1 H4A H 0.4017 0.2842 0.0711 0.019 Uiso 0.796(4) 1 calc R U P A 1 C5A C 0.4061(3) 0.4743(7) 0.15088(16) 0.0138(8) Uani 0.796(4) 1 d D . P A 1 H5A H 0.3639 0.5950 0.1382 0.017 Uiso 0.796(4) 1 calc R U P A 1 C6A C 0.4456(2) 0.4866(6) 0.20911(16) 0.0097(7) Uani 0.796(4) 1 d D . P A 1 H6A H 0.4312 0.6156 0.2358 0.012 Uiso 0.796(4) 1 calc R U P A 1 O1A O 0.5495(2) 0.3034(5) 0.28362(13) 0.0120(6) Uani 0.796(4) 1 d D . P A 1 C7A C 0.5309(3) 0.4973(6) 0.32430(14) 0.0093(7) Uani 0.796(4) 1 d D . P A 1 H7A1 H 0.4638 0.5061 0.3332 0.011 Uiso 0.796(4) 1 calc R U P A 1 H7A2 H 0.5504 0.6505 0.3055 0.011 Uiso 0.796(4) 1 calc R U P A 1 C8A C 0.5846(2) 0.4528(6) 0.38256(14) 0.0118(7) Uani 0.796(4) 1 d D . P A 1 H8A H 0.6521 0.4340 0.3736 0.014 Uiso 0.796(4) 1 calc R U P A 1 O2A O 0.5485(4) 0.2411(6) 0.41230(17) 0.0131(10) Uani 0.796(4) 1 d D . P A 1 C9A C 0.5016(3) 0.3005(8) 0.46315(18) 0.0166(8) Uani 0.796(4) 1 d D . P A 1 O3A O 0.4596(3) 0.1628(7) 0.49458(18) 0.0315(9) Uani 0.796(4) 1 d D . P A 1 O4A O 0.5051(2) 0.5387(5) 0.47325(15) 0.0196(7) Uani 0.796(4) 1 d D . P A 1 C10A C 0.5689(3) 0.6494(6) 0.43047(16) 0.0151(8) Uani 0.796(4) 1 d D . P A 1 H10A H 0.6276 0.6938 0.4509 0.018 Uiso 0.796(4) 1 calc R U P A 1 H10B H 0.5413 0.7940 0.4116 0.018 Uiso 0.796(4) 1 calc R U P A 1 C1C C 0.5020(11) 0.193(3) 0.2262(6) 0.031(5) Uiso 0.204(4) 1 d DG . P A 2 C2C C 0.4436(14) 0.008(3) 0.2084(7) 0.055(7) Uiso 0.204(4) 1 d DG . P A 2 H2C H 0.4336 -0.1246 0.2349 0.065 Uiso 0.204(4) 1 calc R U P A 2 C3C C 0.3998(14) 0.016(3) 0.1517(8) 0.062(8) Uiso 0.204(4) 1 d DG . P A 2 H3C H 0.3599 -0.1102 0.1395 0.075 Uiso 0.204(4) 1 calc R U P A 2 C4C C 0.4145(15) 0.210(4) 0.1129(7) 0.042(8) Uiso 0.204(4) 1 d DG . P A 2 H4C H 0.3845 0.2156 0.0742 0.050 Uiso 0.204(4) 1 calc R U P A 2 C5C C 0.4729(16) 0.395(3) 0.1307(7) 0.080(11) Uiso 0.204(4) 1 d DG . P A 2 H5C H 0.4829 0.5270 0.1042 0.096 Uiso 0.204(4) 1 calc R U P A 2 C6C C 0.5167(13) 0.386(3) 0.1874(7) 0.047(6) Uiso 0.204(4) 1 d DG . P A 2 H6C H 0.5566 0.5126 0.1996 0.056 Uiso 0.204(4) 1 calc R U P A 2 O1C O 0.5374(16) 0.200(3) 0.2846(7) 0.059(7) Uiso 0.204(4) 1 d D . P A 2 C7C C 0.523(2) 0.002(4) 0.3242(8) 0.060(8) Uiso 0.204(4) 1 d D . P A 2 H7C1 H 0.5446 -0.1475 0.3047 0.072 Uiso 0.204(4) 1 calc R U P A 2 H7C2 H 0.4557 -0.0155 0.3333 0.072 Uiso 0.204(4) 1 calc R U P A 2 C8C C 0.5759(13) 0.050(3) 0.3824(7) 0.076(11) Uiso 0.204(4) 1 d D . P A 2 H8C H 0.6435 0.0650 0.3735 0.091 Uiso 0.204(4) 1 calc R U P A 2 O2C O 0.542(2) 0.266(3) 0.4110(10) 0.072(14) Uiso 0.204(4) 1 d D . P A 2 C9C C 0.498(3) 0.215(3) 0.4637(14) 0.079(17) Uiso 0.204(4) 1 d D . P A 2 O3C O 0.452(2) 0.356(4) 0.4918(14) 0.108(11) Uiso 0.204(4) 1 d D . P A 2 O4C O 0.4967(14) -0.023(3) 0.4738(9) 0.061(6) Uiso 0.204(4) 1 d D . P A 2 C10C C 0.5593(16) -0.141(3) 0.4316(7) 0.048(6) Uiso 0.204(4) 1 d D . P A 2 H10C H 0.5305 -0.2860 0.4138 0.058 Uiso 0.204(4) 1 calc R U P A 2 H10D H 0.6178 -0.1861 0.4521 0.058 Uiso 0.204(4) 1 calc R U P A 2 C1B C 0.7526(3) 0.1940(7) 0.77254(16) 0.0127(7) Uani 0.832(4) 1 d D . P B 3 C2B C 0.6930(2) 0.0121(6) 0.79068(17) 0.0144(7) Uani 0.832(4) 1 d D . P B 3 H2B H 0.6784 -0.1157 0.7636 0.017 Uiso 0.832(4) 1 calc R U P B 3 C3B C 0.6548(3) 0.0213(6) 0.84976(17) 0.0155(7) Uani 0.832(4) 1 d D . P B 3 H3B H 0.6136 -0.1014 0.8626 0.019 Uiso 0.832(4) 1 calc R U P B 3 C4B C 0.6761(3) 0.2057(8) 0.88961(18) 0.0148(8) Uani 0.832(4) 1 d D . P B 3 H4B H 0.6505 0.2083 0.9297 0.018 Uiso 0.832(4) 1 calc R U P B 3 C5B C 0.7352(2) 0.3873(6) 0.87046(16) 0.0130(7) Uani 0.832(4) 1 d D . P B 3 H5B H 0.7497 0.5149 0.8976 0.016 Uiso 0.832(4) 1 calc R U P B 3 C6B C 0.7732(3) 0.3838(6) 0.81191(16) 0.0127(7) Uani 0.832(4) 1 d D . P B 3 H6B H 0.8128 0.5094 0.7988 0.015 Uiso 0.832(4) 1 calc R U P B 3 O1B O 0.7962(2) 0.2012(6) 0.71650(13) 0.0128(6) Uani 0.832(4) 1 d D . P B 3 C7B C 0.7785(3) 0.0108(6) 0.67499(14) 0.0112(7) Uani 0.832(4) 1 d D . P B 3 H7B1 H 0.7115 0.0014 0.6658 0.013 Uiso 0.832(4) 1 calc R U P B 3 H7B2 H 0.7983 -0.1434 0.6930 0.013 Uiso 0.832(4) 1 calc R U P B 3 C8B C 0.8325(2) 0.0616(5) 0.61715(14) 0.0096(6) Uani 0.832(4) 1 d D . P B 3 H8B H 0.8997 0.0836 0.6268 0.012 Uiso 0.832(4) 1 calc R U P B 3 O2B O 0.7957(3) 0.2741(7) 0.58816(15) 0.0151(9) Uani 0.832(4) 1 d D . P B 3 C9B C 0.7526(3) 0.2178(7) 0.53576(19) 0.0177(9) Uani 0.832(4) 1 d D . P B 3 O3B O 0.7104(3) 0.3552(6) 0.50478(16) 0.0258(7) Uani 0.832(4) 1 d D . P B 3 O4B O 0.7605(2) -0.0172(5) 0.52307(14) 0.0198(6) Uani 0.832(4) 1 d D . P B 3 C10B C 0.8200(3) -0.1315(6) 0.56799(15) 0.0153(8) Uani 0.832(4) 1 d D . P B 3 H10E H 0.8802 -0.1768 0.5496 0.018 Uiso 0.832(4) 1 calc R U P B 3 H10F H 0.7903 -0.2763 0.5853 0.018 Uiso 0.832(4) 1 calc R U P B 3 C1D C 0.7611(17) 0.281(4) 0.7698(7) 0.080(18) Uiso 0.168(4) 1 d DG . P B 4 C2D C 0.7835(15) 0.098(3) 0.8103(7) 0.053(8) Uiso 0.168(4) 1 d DG . P B 4 H2D H 0.8241 -0.0262 0.7978 0.063 Uiso 0.168(4) 1 calc R U P B 4 C3D C 0.7466(13) 0.097(3) 0.8691(6) 0.024(4) Uiso 0.168(4) 1 d DG . P B 4 H3D H 0.7619 -0.0277 0.8968 0.029 Uiso 0.168(4) 1 calc R U P B 4 C4D C 0.6872(14) 0.280(3) 0.8874(6) 0.025(7) Uiso 0.168(4) 1 d DG . P B 4 H4D H 0.6620 0.2790 0.9276 0.030 Uiso 0.168(4) 1 calc R U P B 4 C5D C 0.6648(15) 0.463(3) 0.8469(8) 0.048(8) Uiso 0.168(4) 1 d DG . P B 4 H5D H 0.6242 0.5873 0.8595 0.058 Uiso 0.168(4) 1 calc R U P B 4 C6D C 0.7017(16) 0.464(3) 0.7881(8) 0.063(10) Uiso 0.168(4) 1 d DG . P B 4 H6D H 0.6864 0.5888 0.7605 0.075 Uiso 0.168(4) 1 calc R U P B 4 O1D O 0.8100(14) 0.298(3) 0.7161(7) 0.034(5) Uiso 0.168(4) 1 d D . P B 4 C7D C 0.7897(18) 0.491(3) 0.6755(7) 0.040(7) Uiso 0.168(4) 1 d D . P B 4 H7D1 H 0.8092 0.6447 0.6937 0.048 Uiso 0.168(4) 1 calc R U P B 4 H7D2 H 0.7223 0.4977 0.6672 0.048 Uiso 0.168(4) 1 calc R U P B 4 C8D C 0.8422(10) 0.444(2) 0.6168(5) 0.022(4) Uiso 0.168(4) 1 d D . P B 4 H8D H 0.9094 0.4184 0.6258 0.026 Uiso 0.168(4) 1 calc R U P B 4 O2D O 0.804(2) 0.236(2) 0.5865(9) 0.060(16) Uiso 0.168(4) 1 d D . P B 4 C9D C 0.756(4) 0.302(3) 0.5368(17) 0.10(2) Uiso 0.168(4) 1 d D . P B 4 O3D O 0.7138(13) 0.167(3) 0.5046(9) 0.035(4) Uiso 0.168(4) 1 d D . P B 4 O4D O 0.7696(12) 0.535(2) 0.5239(7) 0.034(4) Uiso 0.168(4) 1 d D . P B 4 C10D C 0.8301(15) 0.642(3) 0.5692(6) 0.033(6) Uiso 0.168(4) 1 d D . P B 4 H10G H 0.8013 0.7862 0.5877 0.040 Uiso 0.168(4) 1 calc R U P B 4 H10H H 0.8903 0.6878 0.5509 0.040 Uiso 0.168(4) 1 calc R U P B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0047(14) 0.0058(15) 0.0069(14) 0.0017(12) 0.0018(11) 0.0004(13) C2A 0.0115(16) 0.0074(14) 0.0113(14) -0.0006(12) -0.0008(12) 0.0052(12) C3A 0.0133(17) 0.0133(17) 0.0165(16) -0.0009(13) 0.0010(13) -0.0014(14) C4A 0.011(2) 0.018(2) 0.019(2) 0.0048(16) -0.0022(15) -0.0076(18) C5A 0.0070(15) 0.0145(17) 0.0200(17) 0.0045(13) -0.0015(12) 0.0029(13) C6A 0.0078(14) 0.0054(14) 0.0158(16) 0.0000(11) 0.0010(12) 0.0023(11) O1A 0.0155(15) 0.0088(13) 0.0117(12) -0.0011(11) -0.0035(10) 0.0031(13) C7A 0.0108(15) 0.0050(14) 0.0119(14) -0.0019(11) 0.0014(12) 0.0013(12) C8A 0.0110(16) 0.0072(15) 0.0174(16) 0.0005(12) -0.0009(12) -0.0015(12) O2A 0.021(2) 0.0072(14) 0.0117(17) 0.0011(8) 0.0015(13) -0.0035(10) C9A 0.017(2) 0.023(2) 0.0100(17) 0.0015(16) -0.0022(15) -0.003(2) O3A 0.034(2) 0.0325(19) 0.0276(17) 0.0103(14) 0.0042(15) -0.0164(16) O4A 0.0198(14) 0.0185(13) 0.0204(13) -0.0042(10) 0.0033(11) -0.0033(12) C10A 0.0155(17) 0.0130(17) 0.0168(16) -0.0024(13) 0.0006(14) -0.0008(14) C1B 0.0098(16) 0.0104(17) 0.0178(17) 0.0007(14) -0.0002(13) 0.0029(15) C2B 0.0112(15) 0.0138(16) 0.0181(16) -0.0005(12) -0.0014(13) -0.0008(13) C3B 0.0152(16) 0.0112(16) 0.0200(16) 0.0035(12) 0.0053(13) -0.0023(13) C4B 0.017(2) 0.0142(19) 0.0133(17) 0.0001(14) 0.0045(14) -0.0016(17) C5B 0.0145(16) 0.0102(15) 0.0142(15) -0.0020(12) 0.0001(12) 0.0016(13) C6B 0.0111(15) 0.0099(15) 0.0172(16) 0.0015(12) -0.0005(12) -0.0011(12) O1B 0.0159(14) 0.0109(12) 0.0118(12) -0.0037(11) 0.0012(9) -0.0103(12) C7B 0.0119(15) 0.0090(15) 0.0126(14) -0.0012(11) -0.0009(11) -0.0025(12) C8B 0.0105(15) 0.0066(13) 0.0117(13) 0.0004(10) -0.0018(11) 0.0010(11) O2B 0.022(2) 0.0101(13) 0.0130(18) 0.0018(9) 0.0031(13) 0.0041(12) C9B 0.014(2) 0.021(2) 0.017(2) 0.0020(15) -0.0010(15) 0.0074(17) O3B 0.0304(17) 0.0265(16) 0.0205(13) 0.0070(11) -0.0045(12) 0.0122(14) O4B 0.0239(14) 0.0188(13) 0.0168(12) -0.0044(10) -0.0100(11) 0.0063(11) C10B 0.0210(18) 0.0115(15) 0.0134(15) -0.0007(11) -0.0016(12) 0.0063(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1A C6A 123.7(3) . . ? O1A C1A C2A 115.6(3) . . ? C6A C1A C2A 120.6(3) . . ? C1A C2A C3A 119.5(3) . . ? C1A C2A H2A 120.2 . . ? C3A C2A H2A 120.2 . . ? C4A C3A C2A 120.3(3) . . ? C4A C3A H3A 119.8 . . ? C2A C3A H3A 119.8 . . ? C5A C4A C3A 119.5(3) . . ? C5A C4A H4A 120.3 . . ? C3A C4A H4A 120.3 . . ? C4A C5A C6A 120.9(3) . . ? C4A C5A H5A 119.5 . . ? C6A C5A H5A 119.5 . . ? C1A C6A C5A 119.1(3) . . ? C1A C6A H6A 120.5 . . ? C5A C6A H6A 120.5 . . ? C1A O1A C7A 117.2(3) . . ? O1A C7A C8A 107.6(3) . . ? O1A C7A H7A1 110.2 . . ? C8A C7A H7A1 110.2 . . ? O1A C7A H7A2 110.2 . . ? C8A C7A H7A2 110.2 . . ? H7A1 C7A H7A2 108.5 . . ? O2A C8A C7A 109.1(3) . . ? O2A C8A C10A 103.1(2) . . ? C7A C8A C10A 112.4(3) . . ? O2A C8A H8A 110.7 . . ? C7A C8A H8A 110.7 . . ? C10A C8A H8A 110.7 . . ? C9A O2A C8A 110.5(3) . . ? O3A C9A O2A 124.8(4) . . ? O3A C9A O4A 124.0(4) . . ? O2A C9A O4A 111.1(3) . . ? C9A O4A C10A 109.8(3) . . ? O4A C10A C8A 103.2(2) . . ? O4A C10A H10A 111.1 . . ? C8A C10A H10A 111.1 . . ? O4A C10A H10B 111.1 . . ? C8A C10A H10B 111.1 . . ? H10A C10A H10B 109.1 . . ? O1C C1C C2C 120.6(6) . . ? O1C C1C C6C 119.0(6) . . ? C2C C1C C6C 120.0 . . ? C1C C2C C3C 120.0 . . ? C1C C2C H2C 120.0 . . ? C3C C2C H2C 120.0 . . ? C4C C3C C2C 120.0 . . ? C4C C3C H3C 120.0 . . ? C2C C3C H3C 120.0 . . ? C5C C4C C3C 120.0 . . ? C5C C4C H4C 120.0 . . ? C3C C4C H4C 120.0 . . ? C4C C5C C6C 120.0 . . ? C4C C5C H5C 120.0 . . ? C6C C5C H5C 120.0 . . ? C5C C6C C1C 120.0 . . ? C5C C6C H6C 120.0 . . ? C1C C6C H6C 120.0 . . ? C1C O1C C7C 119.0(8) . . ? O1C C7C C8C 107.2(8) . . ? O1C C7C H7C1 110.3 . . ? C8C C7C H7C1 110.3 . . ? O1C C7C H7C2 110.3 . . ? C8C C7C H7C2 110.3 . . ? H7C1 C7C H7C2 108.5 . . ? O2C C8C C7C 109.7(9) . . ? O2C C8C C10C 103.0(6) . . ? C7C C8C C10C 112.7(9) . . ? O2C C8C H8C 110.4 . . ? C7C C8C H8C 110.4 . . ? C10C C8C H8C 110.4 . . ? C9C O2C C8C 110.9(7) . . ? O3C C9C O2C 124.4(11) . . ? O3C C9C O4C 123.7(11) . . ? O2C C9C O4C 110.7(7) . . ? C9C O4C C10C 109.7(6) . . ? O4C C10C C8C 103.0(6) . . ? O4C C10C H10C 111.2 . . ? C8C C10C H10C 111.2 . . ? O4C C10C H10D 111.2 . . ? C8C C10C H10D 111.2 . . ? H10C C10C H10D 109.1 . . ? O1B C1B C2B 123.9(3) . . ? O1B C1B C6B 115.3(3) . . ? C2B C1B C6B 120.8(3) . . ? C1B C2B C3B 118.6(3) . . ? C1B C2B H2B 120.7 . . ? C3B C2B H2B 120.7 . . ? C4B C3B C2B 121.2(3) . . ? C4B C3B H3B 119.4 . . ? C2B C3B H3B 119.4 . . ? C3B C4B C5B 119.4(3) . . ? C3B C4B H4B 120.3 . . ? C5B C4B H4B 120.3 . . ? C6B C5B C4B 120.5(3) . . ? C6B C5B H5B 119.7 . . ? C4B C5B H5B 119.7 . . ? C5B C6B C1B 119.5(3) . . ? C5B C6B H6B 120.3 . . ? C1B C6B H6B 120.3 . . ? C1B O1B C7B 117.5(3) . . ? O1B C7B C8B 107.4(2) . . ? O1B C7B H7B1 110.2 . . ? C8B C7B H7B1 110.2 . . ? O1B C7B H7B2 110.2 . . ? C8B C7B H7B2 110.2 . . ? H7B1 C7B H7B2 108.5 . . ? O2B C8B C7B 109.2(3) . . ? O2B C8B C10B 103.2(2) . . ? C7B C8B C10B 113.1(3) . . ? O2B C8B H8B 110.4 . . ? C7B C8B H8B 110.4 . . ? C10B C8B H8B 110.4 . . ? C9B O2B C8B 110.6(3) . . ? O3B C9B O2B 124.8(4) . . ? O3B C9B O4B 123.7(4) . . ? O2B C9B O4B 111.5(3) . . ? C9B O4B C10B 109.9(2) . . ? O4B C10B C8B 103.4(2) . . ? O4B C10B H10E 111.1 . . ? C8B C10B H10E 111.1 . . ? O4B C10B H10F 111.1 . . ? C8B C10B H10F 111.1 . . ? H10E C10B H10F 109.0 . . ? O1D C1D C2D 118.3(7) . . ? O1D C1D C6D 120.8(7) . . ? C2D C1D C6D 120.0 . . ? C3D C2D C1D 120.0 . . ? C3D C2D H2D 120.0 . . ? C1D C2D H2D 120.0 . . ? C2D C3D C4D 120.0 . . ? C2D C3D H3D 120.0 . . ? C4D C3D H3D 120.0 . . ? C5D C4D C3D 120.0 . . ? C5D C4D H4D 120.0 . . ? C3D C4D H4D 120.0 . . ? C4D C5D C6D 120.0 . . ? C4D C5D H5D 120.0 . . ? C6D C5D H5D 120.0 . . ? C5D C6D C1D 120.0 . . ? C5D C6D H6D 120.0 . . ? C1D C6D H6D 120.0 . . ? C1D O1D C7D 118.6(8) . . ? O1D C7D C8D 107.1(8) . . ? O1D C7D H7D1 110.3 . . ? C8D C7D H7D1 110.3 . . ? O1D C7D H7D2 110.3 . . ? C8D C7D H7D2 110.3 . . ? H7D1 C7D H7D2 108.6 . . ? O2D C8D C7D 109.4(9) . . ? O2D C8D C10D 103.1(6) . . ? C7D C8D C10D 113.1(8) . . ? O2D C8D H8D 110.3 . . ? C7D C8D H8D 110.3 . . ? C10D C8D H8D 110.3 . . ? C9D O2D C8D 110.5(7) . . ? O3D C9D O2D 124.3(10) . . ? O3D C9D O4D 124.5(10) . . ? O2D C9D O4D 110.8(7) . . ? C9D O4D C10D 110.4(6) . . ? O4D C10D C8D 103.5(5) . . ? O4D C10D H10G 111.1 . . ? C8D C10D H10G 111.1 . . ? O4D C10D H10H 111.1 . . ? C8D C10D H10H 111.1 . . ? H10G C10D H10H 109.0 . . ? 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 C1A O1A 1.374(3) . ? C1A C6A 1.391(4) . ? C1A C2A 1.395(3) . ? C2A C3A 1.396(4) . ? C2A H2A 0.9500 . ? C3A C4A 1.390(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.389(4) . ? C4A H4A 0.9500 . ? C5A C6A 1.395(4) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? O1A C7A 1.426(3) . ? C7A C8A 1.510(4) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A O2A 1.446(4) . ? C8A C10A 1.533(4) . ? C8A H8A 1.0000 . ? O2A C9A 1.342(4) . ? C9A O3A 1.196(4) . ? C9A O4A 1.350(4) . ? O4A C10A 1.450(4) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C1C O1C 1.372(5) . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C2C C3C 1.3900 . ? C2C H2C 0.9500 . ? C3C C4C 1.3900 . ? C3C H3C 0.9500 . ? C4C C5C 1.3900 . ? C4C H4C 0.9500 . ? C5C C6C 1.3900 . ? C5C H5C 0.9500 . ? C6C H6C 0.9500 . ? O1C C7C 1.421(6) . ? C7C C8C 1.511(7) . ? C7C H7C1 0.9900 . ? C7C H7C2 0.9900 . ? C8C O2C 1.444(7) . ? C8C C10C 1.531(6) . ? C8C H8C 1.0000 . ? O2C C9C 1.341(6) . ? C9C O3C 1.196(6) . ? C9C O4C 1.348(7) . ? O4C C10C 1.450(6) . ? C10C H10C 0.9900 . ? C10C H10D 0.9900 . ? C1B O1B 1.376(3) . ? C1B C2B 1.390(4) . ? C1B C6B 1.396(4) . ? C2B C3B 1.403(4) . ? C2B H2B 0.9500 . ? C3B C4B 1.383(4) . ? C3B H3B 0.9500 . ? C4B C5B 1.391(4) . ? C4B H4B 0.9500 . ? C5B C6B 1.391(4) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? O1B C7B 1.420(3) . ? C7B C8B 1.511(4) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C8B O2B 1.446(4) . ? C8B C10B 1.532(4) . ? C8B H8B 1.0000 . ? O2B C9B 1.339(4) . ? C9B O3B 1.191(4) . ? C9B O4B 1.346(4) . ? O4B C10B 1.452(3) . ? C10B H10E 0.9900 . ? C10B H10F 0.9900 . ? C1D O1D 1.372(5) . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C2D C3D 1.3900 . ? C2D H2D 0.9500 . ? C3D C4D 1.3900 . ? C3D H3D 0.9500 . ? C4D C5D 1.3900 . ? C4D H4D 0.9500 . ? C5D C6D 1.3900 . ? C5D H5D 0.9500 . ? C6D H6D 0.9500 . ? O1D C7D 1.422(6) . ? C7D C8D 1.511(6) . ? C7D H7D1 0.9900 . ? C7D H7D2 0.9900 . ? C8D O2D 1.446(6) . ? C8D C10D 1.530(6) . ? C8D H8D 1.0000 . ? O2D C9D 1.341(6) . ? C9D O3D 1.196(6) . ? C9D O4D 1.348(7) . ? O4D C10D 1.449(6) . ? C10D H10G 0.9900 . ? C10D H10H 0.9900 . ?