#------------------------------------------------------------------------------ #$Date: 2024-02-04 13:41:47 +0200 (Sun, 04 Feb 2024) $ #$Revision: 289457 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247823.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_7247823 loop_ _publ_author_name 'Zhang, Menglei' 'Li, Zhongkui' 'Zhu, Yanhong' 'Yan, Li' 'Zhong, Xue' 'Zhang, Yijie' 'Li, Ziyao' 'Bai, Yixiang' 'Li, Hui' _publ_section_title ; Mimic uracil--uracil base pairing: self-assembly and single crystal structure ; _journal_issue 3 _journal_name_full CrystEngComm _journal_page_first 261 _journal_page_last 267 _journal_paper_doi 10.1039/D3CE01056B _journal_volume 26 _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety 'C30 H36 Co N8 O18 P2, 4(H2 O), Co H12 O6, 3(O), C3 H7 N O' _chemical_formula_sum 'C33 H63 Co2 N9 O32 P2' _chemical_formula_weight 1277.72 _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-06-27 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-08-16 deposited with the CCDC. 2023-12-01 downloaded from the CCDC. ; _cell_angle_alpha 68.453(3) _cell_angle_beta 89.860(3) _cell_angle_gamma 80.963(3) _cell_formula_units_Z 1 _cell_length_a 6.7824(6) _cell_length_b 13.8721(12) _cell_length_c 15.7504(14) _cell_measurement_reflns_used 4891 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 30.203 _cell_measurement_theta_min 2.482 _cell_volume 1358.8(2) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_unetI/netI 0.1018 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 18386 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.898 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.359 _diffrn_reflns_theta_min 1.601 _diffrn_source_current 30.0 _diffrn_source_power 1.35 _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.5626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0743 before and 0.0524 after correction. The Ratio of minimum to maximum transmission is 0.7542. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour pink _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.561 _exptl_crystal_description block _exptl_crystal_F_000 664 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.457 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.113 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 732 _refine_ls_number_reflns 14757 _refine_ls_number_restraints 35 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0644 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+1.1318P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1550 _refine_ls_wR_factor_ref 0.1780 _reflns_Friedel_coverage 0.872 _reflns_Friedel_fraction_full 0.969 _reflns_Friedel_fraction_max 0.837 _reflns_number_gt 10276 _reflns_number_total 14757 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01056b2.cif _cod_data_source_block 1_a_CCDC1 _cod_depositor_comments 'Adding full bibliography for 7247822--7247826.cif.' _cod_database_code 7247823 _shelx_shelxl_version_number 2018/3 _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_max 0.913 _shelx_estimated_absorpt_t_min 0.837 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.97(2) 0.03(2) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 3. Restrained distances H3B-O13 2 with sigma of 0.02 H1B-O1 0.86 with sigma of 0.02 H3A_$1-O5 1.8 with sigma of 0.02 H3A-H28A 2.12 with sigma of 0.02 O3_$1-H3A_$1 0.86 with sigma of 0.02 O1-H1A 0.86 with sigma of 0.02 O3_$1-H3B_$1 0.86 with sigma of 0.02 H3A_$1-H1B 2.12 with sigma of 0.02 O5-H1B 1.8 with sigma of 0.02 O5-H28A_$1 2.077 with sigma of 0.02 O32-H19B 1.95 with sigma of 0.02 H1A-O13_$1 1.6 with sigma of 0.02 Co2-H21A \\sim Co2-H21B with sigma of 0.02 Co2-H24A \\sim Co2-H24B with sigma of 0.02 4. Uiso/Uaniso restraints and constraints Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 5.a Free rotating group: O28(H28A,H28B), O21(H21A,H21B), O24(H24A,H24B), O25(H25C,H25D), O26(H26A, H26B), O27(H27A,H27B) 5.b Rotating group: O1(H1A,H1B), O3(H3A,H3B), O19(H19A,H19B), O20(H20A,H20B), O22(H22C,H22D), O23(H23A,H23B) 5.c Ternary CH refined with riding coordinates: C14(H14), C15(H15A), C17(H17), C23(H23), C24(H24), C26(H26) 5.d Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C16(H16A,H16B), C22(H22A,H22B), C25(H25A,H25B) 5.e Aromatic/amide H refined with riding coordinates: N6(H6), N8(H8A), C1(H1), C2(H2), C4(H4), C5(H5), C6(H6A), C7(H7), C8(H8B), C10(H10), C11(H11), C12(H12), C20(H20), C21(H21), C27(H27), C28(H28), C33(H33) 5.f Idealised Me refined as rotating group: C31(H31A,H31B,H31C), C32(H32A,H32B,H32C) 5.g Idealised tetrahedral OH refined as rotating group: O8(H8), O15(H15) ; _shelx_res_file ; TITL 1_a.res in P1 1_a.res created by SHELXL-2018/3 at 21:45:48 on 07-Apr-2022 REM Old TITL 1 in P1 REM SHELXT solution in P1 REM R1 0.110, Rweak 0.037, Alpha 0.000, Orientation as input REM Flack x = 0.167 ( 0.009 ) from Parsons' quotients REM Formula found by SHELXT: C38 N11 O23 P2 Co2 CELL 0.71073 6.7824 13.8721 15.7504 68.453 89.86 80.963 ZERR 1 0.0006 0.0012 0.0014 0.003 0.003 0.003 LATT -1 SFAC C H Co N O P UNIT 33 63 2 9 32 2 EQIV $1 -1+X,+Y,+Z EQIV $2 1+X,+Y,+Z EQIV $3 -1+X,1+Y,-1+Z EQIV $4 1+X,-1+Y,1+Z EQIV $5 -1+X,+Y,-1+Z EQIV $6 1+X,+Y,1+Z EQIV $7 +X,1+Y,+Z EQIV $8 -1+X,1+Y,+Z DFIX 2 H3b O13 DFIX 0.86 H1b O1 DFIX 1.8 H3a_$1 O5 DFIX 2.12 H3a H28a DFIX 0.86 O3_$1 H3a_$1 DFIX 0.86 O1 H1a DFIX 0.86 O3_$1 H3b_$1 DFIX 2.12 H3a_$1 H1b SADI Co2 H21a Co2 H21b DFIX 1.8 O5 H1b DFIX 2.077 O5 H28a_$1 SADI Co2 H24a Co2 H24b ISOR 0.01 0.02 C31 C32 ISOR 0.01 0.02 O31 DFIX 1.95 O32 H19b DFIX 1.6 H1a O13_$1 L.S. 20 PLAN 30 SIZE 0.12 0.12 0.24 TEMP 23 CONF HTAB O1 O5 HTAB O1 O13_$1 HTAB O3 O5_$2 HTAB O3 O13 HTAB O8 O26_$3 HTAB O15 O8_$4 HTAB N6 O17_$5 HTAB N8 O10_$6 HTAB O19 O12_$7 HTAB O19 O32 HTAB O20 O25 HTAB O21 O13_$8 HTAB O22 O12_$7 HTAB O22 O27 HTAB O23 O25_$2 HTAB O23 O28 HTAB O24 O6 HTAB O24 O31 HTAB O25 O6 HTAB O25 O18_$1 HTAB O26 O15_$1 HTAB O26 O30 HTAB O27 O6_$2 HTAB O27 O28 HTAB O28 O2 HTAB O28 O5_$2 BOND $H LIST 4 MORE -1 HTAB fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 3 0 2 OMIT 3 0 1 OMIT 3 -1 4 OMIT 3 -2 0 OMIT 3 -1 3 OMIT -3 -7 -2 OMIT 3 0 3 OMIT 3 -2 1 OMIT 3 5 -6 OMIT 3 -1 1 REM REM REM WGHT 0.080700 1.131800 BASF 0.03307 FVAR 0.62154 CO1 3 0.686761 0.465420 0.310290 11.00000 0.01759 0.01873 = 0.01201 -0.00744 0.00128 -0.00222 P1 6 1.030557 0.244895 0.377449 11.00000 0.01989 0.01708 = 0.01303 -0.00674 0.00077 -0.00241 P2 6 0.346368 0.689001 0.238906 11.00000 0.01879 0.01543 = 0.01449 -0.00619 -0.00011 -0.00254 O1 5 0.408858 0.422283 0.355360 11.00000 0.01697 0.02834 = 0.04190 -0.02167 0.00754 -0.00695 AFIX 7 H1A 2 0.375993 0.378719 0.332213 11.00000 -1.50000 H1B 2 0.313357 0.476152 0.334096 11.00000 -1.50000 AFIX 0 O2 5 0.555786 0.625732 0.249532 11.00000 0.01623 0.01583 = 0.02483 -0.00468 0.00014 0.00297 O3 5 0.962545 0.507989 0.257114 11.00000 0.01906 0.02679 = 0.02952 -0.01248 -0.00105 -0.00216 AFIX 7 H3A 2 1.006677 0.546797 0.282975 11.00000 -1.50000 H3B 2 1.055174 0.452718 0.272393 11.00000 -1.50000 AFIX 0 O4 5 0.831547 0.313868 0.373376 11.00000 0.02759 0.02120 = 0.01746 -0.00954 0.00172 -0.00298 O5 5 0.198452 0.624621 0.294402 11.00000 0.01992 0.01858 = 0.02396 -0.00554 0.00382 -0.00389 O6 5 0.345416 0.790400 0.254009 11.00000 0.03190 0.02260 = 0.02991 -0.01579 0.00354 -0.00562 O7 5 0.260710 0.720627 0.134148 11.00000 0.02387 0.02532 = 0.01513 -0.00246 -0.00530 -0.00838 O8 5 -0.018921 0.922345 -0.131590 11.00000 0.04276 0.03698 = 0.02922 0.00982 -0.01061 0.00298 AFIX 147 H8 2 -0.140070 0.942679 -0.139846 11.00000 -1.50000 AFIX 0 O9 5 0.289386 0.719430 -0.047360 11.00000 0.03266 0.02976 = 0.02912 -0.01572 0.00291 -0.00435 O10 5 0.108783 0.581442 -0.178033 11.00000 0.07375 0.03281 = 0.01257 -0.00914 0.00337 -0.00985 O11 5 0.229312 0.264168 0.054849 11.00000 0.08481 0.02655 = 0.03114 -0.01052 -0.00287 -0.00225 O12 5 1.013297 0.141402 0.367582 11.00000 0.02283 0.02063 = 0.03445 -0.01227 0.00697 -0.00440 O13 5 1.180680 0.302129 0.312402 11.00000 0.02447 0.02236 = 0.01415 -0.00650 0.00348 -0.00502 O14 5 1.123555 0.216695 0.480475 11.00000 0.03203 0.02959 = 0.01644 -0.01044 0.00111 0.00818 O15 5 1.270836 -0.000760 0.752609 11.00000 0.04689 0.03286 = 0.02683 0.00543 -0.00389 0.00160 AFIX 147 H15 2 1.180773 -0.023038 0.785122 11.00000 -1.50000 AFIX 0 O16 5 1.404661 0.202144 0.633066 11.00000 0.03252 0.03152 = 0.03288 -0.01899 0.00221 -0.00004 O17 5 1.192839 0.340700 0.800691 11.00000 0.07838 0.03267 = 0.01754 -0.01193 0.00516 -0.00688 O18 5 1.145777 0.658736 0.570832 11.00000 0.07993 0.03028 = 0.03316 -0.00827 0.00254 -0.01083 AFIX 6 O28 5 0.824691 0.760388 0.244342 11.00000 0.02285 0.03160 = 0.07515 -0.01694 0.00313 0.00118 H28A 2 0.905849 0.703686 0.271970 11.00000 -1.50000 H28B 2 0.728613 0.740801 0.223799 11.00000 -1.50000 AFIX 0 N1 4 0.699963 0.489134 0.441492 11.00000 0.01739 0.02659 = 0.01674 -0.01137 -0.00235 -0.00012 N2 4 0.659505 0.442138 1.181046 11.00000 0.02608 0.02108 = 0.01557 -0.00795 0.00363 -0.01003 N3 4 0.659608 0.472627 0.851593 11.00000 0.04763 0.03768 = 0.01828 -0.01719 0.00465 -0.00436 N4 4 0.667866 0.440134 0.775962 11.00000 0.04846 0.04905 = 0.01439 -0.01807 0.00515 -0.00927 N5 4 0.123977 0.580324 -0.032879 11.00000 0.03684 0.02704 = 0.00933 -0.00531 0.00037 -0.00366 N6 4 0.164976 0.423460 -0.059323 11.00000 0.04334 0.02870 = 0.01910 -0.01241 0.00416 -0.00626 AFIX 43 H6 2 0.168259 0.392366 -0.097669 11.00000 -1.20000 AFIX 0 N7 4 1.212386 0.345190 0.654791 11.00000 0.04332 0.02939 = 0.02052 -0.01316 0.00040 0.00381 N8 4 1.166056 0.498710 0.682754 11.00000 0.04208 0.02952 = 0.01842 -0.00997 0.00241 -0.00164 AFIX 43 H8A 2 1.150682 0.529242 0.721552 11.00000 -1.20000 AFIX 0 C1 1 0.703110 0.402530 0.518303 11.00000 0.02374 0.02482 = 0.01869 -0.01168 0.00116 -0.00326 AFIX 43 H1 2 0.713423 0.337308 0.513090 11.00000 -1.20000 AFIX 0 C2 1 0.691551 0.407620 0.604090 11.00000 0.02812 0.02421 = 0.01584 -0.00409 -0.00033 -0.00329 AFIX 43 H2 2 0.691410 0.346818 0.655452 11.00000 -1.20000 AFIX 0 C3 1 0.680130 0.504178 0.613183 11.00000 0.02957 0.03179 = 0.01541 -0.01125 -0.00274 0.00264 C4 1 0.676046 0.592090 0.534029 11.00000 0.04832 0.02872 = 0.01960 -0.01285 0.00023 -0.01035 AFIX 43 H4 2 0.666363 0.658230 0.537328 11.00000 -1.20000 AFIX 0 C5 1 0.686377 0.581673 0.449789 11.00000 0.04307 0.02750 = 0.02042 -0.00920 -0.00140 -0.00101 AFIX 43 H5 2 0.683688 0.641605 0.397334 11.00000 -1.20000 AFIX 0 C6 1 0.670195 0.516644 0.702135 11.00000 0.04502 0.03726 = 0.02384 -0.01907 -0.00197 -0.00175 AFIX 43 H6A 2 0.665494 0.583348 0.703662 11.00000 -1.20000 AFIX 0 C7 1 0.687733 0.345200 1.177629 11.00000 0.03598 0.02016 = 0.01563 -0.00488 -0.00406 -0.00467 AFIX 43 H7 2 0.703076 0.287429 1.232467 11.00000 -1.20000 AFIX 0 C8 1 0.695023 0.327312 1.097014 11.00000 0.04594 0.02060 = 0.02284 -0.01157 -0.00148 -0.00321 AFIX 43 H8B 2 0.713804 0.259197 1.097602 11.00000 -1.20000 AFIX 0 C9 1 0.673448 0.414264 1.014078 11.00000 0.03570 0.02939 = 0.01509 -0.01106 0.00218 -0.00656 C10 1 0.644366 0.514122 1.017959 11.00000 0.03126 0.02351 = 0.01502 -0.00548 0.00331 -0.00340 AFIX 43 H10 2 0.628611 0.573673 0.964483 11.00000 -1.20000 AFIX 0 C11 1 0.639252 0.523554 1.101512 11.00000 0.03203 0.02328 = 0.02153 -0.00860 -0.00411 -0.00317 AFIX 43 H11 2 0.620515 0.590838 1.102847 11.00000 -1.20000 AFIX 0 C12 1 0.678859 0.397510 0.927295 11.00000 0.03932 0.04005 = 0.01825 -0.01463 0.00344 -0.00543 AFIX 43 H12 2 0.697111 0.329137 0.928530 11.00000 -1.20000 AFIX 0 C13 1 0.353148 0.796093 0.063854 11.00000 0.03046 0.01967 = 0.02103 -0.00451 -0.00191 -0.00536 AFIX 23 H13A 2 0.495016 0.770104 0.065459 11.00000 -1.20000 H13B 2 0.337412 0.861734 0.073907 11.00000 -1.20000 AFIX 0 C14 1 0.256042 0.814049 -0.027488 11.00000 0.03117 0.02423 = 0.01412 -0.00261 0.00079 0.00031 AFIX 13 H14 2 0.316882 0.867594 -0.074454 11.00000 -1.20000 AFIX 0 C15 1 0.028016 0.850250 -0.038264 11.00000 0.03433 0.02398 = 0.02524 -0.00775 -0.00037 0.00299 AFIX 13 H15A 2 -0.018184 0.882878 0.005451 11.00000 -1.20000 AFIX 0 C16 1 -0.054397 0.750279 -0.021184 11.00000 0.02749 0.03410 = 0.02511 -0.00811 0.00112 -0.00299 AFIX 23 H16A 2 -0.186856 0.764329 -0.050636 11.00000 -1.20000 H16B 2 -0.058545 0.710133 0.043655 11.00000 -1.20000 AFIX 0 C17 1 0.102965 0.693866 -0.066329 11.00000 0.02844 0.02478 = 0.02105 -0.00822 -0.00243 -0.00752 AFIX 13 H17 2 0.072722 0.722528 -0.132605 11.00000 -1.20000 AFIX 0 C18 1 0.130773 0.532624 -0.096032 11.00000 0.03587 0.02854 = 0.02354 -0.01419 0.00245 -0.00201 C19 1 0.194302 0.359379 0.032086 11.00000 0.03283 0.02848 = 0.02016 -0.00793 -0.00072 -0.00222 C20 1 0.180414 0.416536 0.093402 11.00000 0.03668 0.03120 = 0.01248 -0.00650 0.00411 -0.00503 AFIX 43 H20 2 0.193047 0.379788 0.156321 11.00000 -1.20000 AFIX 0 C21 1 0.149812 0.520868 0.060251 11.00000 0.03539 0.02924 = 0.01357 -0.00838 -0.00382 0.00160 AFIX 43 H21 2 0.145495 0.555524 0.100957 11.00000 -1.20000 AFIX 0 C22 1 1.314980 0.151718 0.506353 11.00000 0.03557 0.03842 = 0.02239 -0.01573 -0.00391 0.00963 AFIX 23 H22A 2 1.417216 0.190463 0.474271 11.00000 -1.20000 H22B 2 1.318116 0.090639 0.489911 11.00000 -1.20000 AFIX 0 C23 1 1.356464 0.116820 0.609218 11.00000 0.03855 0.02373 = 0.01668 -0.00572 -0.00252 0.00176 AFIX 13 H23 2 1.471612 0.059666 0.628092 11.00000 -1.20000 AFIX 0 C24 1 1.184816 0.079102 0.666034 11.00000 0.03702 0.02250 = 0.02120 -0.00372 -0.00440 0.00201 AFIX 13 H24 2 1.096251 0.051730 0.634646 11.00000 -1.20000 AFIX 0 C25 1 1.080326 0.176414 0.678750 11.00000 0.03858 0.03189 = 0.02901 -0.01014 0.00756 0.00364 AFIX 23 H25A 2 1.006032 0.159074 0.733579 11.00000 -1.20000 H25B 2 0.990489 0.220599 0.626391 11.00000 -1.20000 AFIX 0 C26 1 1.257274 0.229126 0.687432 11.00000 0.04034 0.03084 = 0.01030 -0.00795 -0.00271 0.00635 AFIX 13 H26 2 1.309469 0.200886 0.751335 11.00000 -1.20000 AFIX 0 C27 1 1.202571 0.404039 0.563172 11.00000 0.03804 0.03432 = 0.01600 -0.01204 0.00163 0.00026 AFIX 43 H27 2 1.215533 0.369136 0.522570 11.00000 -1.20000 AFIX 0 C28 1 1.175308 0.509157 0.528914 11.00000 0.03291 0.03316 = 0.02613 -0.01128 -0.00037 0.00086 AFIX 43 H28 2 1.165749 0.546267 0.466054 11.00000 -1.20000 AFIX 0 C29 1 1.161109 0.563500 0.591318 11.00000 0.03636 0.02645 = 0.02410 -0.00769 0.00227 -0.00623 C30 1 1.192616 0.392257 0.717270 11.00000 0.04088 0.02877 = 0.01978 -0.01279 -0.00103 0.00067 CO2 3 0.569802 1.020560 0.309231 11.00000 0.02418 0.02058 = 0.02652 -0.00996 0.00259 -0.00365 O19 5 0.682728 1.055474 0.414481 11.00000 0.03775 0.04487 = 0.03057 -0.00913 0.00648 -0.02327 AFIX 7 H19A 2 0.775506 1.091725 0.395551 11.00000 -1.50000 H19B 2 0.740550 0.999074 0.456261 11.00000 -1.50000 AFIX 0 O20 5 0.319542 0.982146 0.383422 11.00000 0.02751 0.02982 = 0.04849 -0.01791 0.00962 -0.01063 AFIX 7 H20A 2 0.322737 0.911986 0.409008 11.00000 -1.50000 H20B 2 0.205140 1.002701 0.347482 11.00000 -1.50000 AFIX 6 O21 5 0.404283 1.170963 0.241942 11.00000 0.04443 0.01934 = 0.02852 -0.00722 0.00649 0.00425 H21A 2 0.405145 1.225864 0.253851 11.00000 -1.50000 H21B 2 0.340242 1.193073 0.190222 11.00000 -1.50000 AFIX 0 O22 5 0.823168 1.075505 0.239438 11.00000 0.02530 0.03421 = 0.04135 -0.02096 0.00547 -0.00828 AFIX 7 H22C 2 0.911535 1.023166 0.240596 11.00000 -1.50000 H22D 2 0.882182 1.105682 0.268480 11.00000 -1.50000 AFIX 0 O23 5 0.719129 0.860631 0.371240 11.00000 0.04375 0.03722 = 0.04247 -0.01510 -0.00133 -0.00830 AFIX 7 H23A 2 0.852438 0.855261 0.384882 11.00000 -1.50000 H23B 2 0.723983 0.825042 0.332279 11.00000 -1.50000 AFIX 6 O24 5 0.490288 0.974761 0.202971 11.00000 0.07022 0.03975 = 0.03576 -0.01752 -0.00137 -0.02318 H24A 2 0.470119 1.016927 0.147560 11.00000 -1.50000 H24B 2 0.408785 0.932247 0.209212 11.00000 -1.50000 AFIX 6 O25 5 0.145478 0.813062 0.402166 11.00000 0.04891 0.02954 = 0.03056 -0.01038 0.01337 -0.00614 H25C 2 0.132067 0.759152 0.448486 11.00000 -1.50000 H25D 2 0.148846 0.792202 0.357576 11.00000 -1.50000 AFIX 6 O26 5 0.595121 0.013812 0.856093 11.00000 0.06099 0.08698 = 0.11682 -0.00973 -0.04528 0.00002 H26A 2 0.614092 0.077152 0.833392 11.00000 -1.50000 H26B 2 0.510366 0.009439 0.818488 11.00000 -1.50000 AFIX 6 O27 5 1.001377 0.941394 0.160424 11.00000 0.03646 0.03261 = 0.04767 -0.01305 0.00604 0.00020 H27A 2 0.906849 0.905712 0.170310 11.00000 -1.50000 H27B 2 1.098682 0.899940 0.195888 11.00000 -1.50000 AFIX 0 O29 5 0.983939 0.123718 0.994088 11.00000 0.22695 0.10456 = 0.09130 -0.00757 -0.05507 -0.02621 O30 5 0.723502 0.198759 0.842772 11.00000 0.17688 0.07950 = 0.09507 -0.04710 -0.00923 -0.01183 O31 5 0.459519 1.088864 0.015458 11.00000 0.26639 0.13731 = 0.07124 -0.02774 0.03668 -0.02581 O32 5 0.741830 0.896973 0.580912 11.00000 0.12452 0.09338 = 0.07347 0.00318 0.01899 -0.03497 N9 4 0.532735 0.806731 0.678315 11.00000 0.12145 0.04718 = 0.03349 -0.01161 0.01150 -0.02761 C31 1 0.329039 0.777492 0.697768 11.00000 0.10757 0.11119 = 0.13892 -0.06688 0.04439 -0.05572 AFIX 137 H31A 2 0.253354 0.795036 0.641148 11.00000 -1.50000 H31B 2 0.261279 0.815399 0.732520 11.00000 -1.50000 H31C 2 0.342112 0.703328 0.732087 11.00000 -1.50000 AFIX 0 C32 1 0.644834 0.786520 0.757660 11.00000 0.14811 0.10506 = 0.07480 -0.04370 -0.03644 0.00896 AFIX 137 H32A 2 0.784129 0.770892 0.748040 11.00000 -1.50000 H32B 2 0.606729 0.727496 0.805798 11.00000 -1.50000 H32C 2 0.621742 0.847091 0.774419 11.00000 -1.50000 AFIX 0 C33 1 0.568627 0.859218 0.598118 11.00000 0.10978 0.05765 = 0.05708 -0.02088 0.00933 -0.01530 AFIX 43 H33 2 0.475630 0.872214 0.550279 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1_a.res in P1 REM wR2 = 0.1780, GooF = S = 1.018, Restrained GooF = 1.031 for all data REM R1 = 0.0644 for 10276 Fo > 4sig(Fo) and 0.1054 for all 14757 data REM 732 parameters refined using 35 restraints END WGHT 0.0807 1.1318 REM Instructions for potential hydrogen bonds HTAB O1 O13_$1 HTAB O1 O3_$1 HTAB O1 O5 HTAB O3 O5_$2 HTAB O3 O1_$2 HTAB O3 O13 HTAB O8 O26_$3 HTAB O15 O8_$4 HTAB N6 O17_$5 HTAB N8 O10_$6 HTAB C1 O4 HTAB C5 O2 HTAB C5 O28 EQIV $9 x, y, z+1 HTAB C7 O4_$9 HTAB C11 O2_$9 HTAB C12 O30 HTAB C14 O15_$3 HTAB C16 O7 HTAB C20 O13_$1 HTAB C21 O3_$1 EQIV $11 x+1, y-1, z HTAB C22 O20_$11 HTAB C25 O14 HTAB C27 O14 HTAB C28 O5_$2 HTAB O19 O12_$7 HTAB O19 O32 HTAB O20 O25 HTAB O20 O12_$8 HTAB O22 O27 HTAB O22 O12_$7 HTAB O23 O25_$2 HTAB O23 O28 HTAB C31 O10_$9 HTAB C33 O20 REM Highest difference peak 1.457, deepest hole -0.578, 1-sigma level 0.113 Q1 1 1.0182 0.4613 0.3146 11.00000 0.05 1.46 Q2 1 0.9143 1.0190 0.3080 11.00000 0.05 1.40 Q3 1 0.2363 1.0216 0.3086 11.00000 0.05 1.35 Q4 1 0.3253 0.4722 0.3080 11.00000 0.05 1.23 Q5 1 1.0351 0.6953 0.2350 11.00000 0.05 0.82 Q6 1 0.7316 0.2454 0.3718 11.00000 0.05 0.77 Q7 1 1.3929 0.2502 0.3765 11.00000 0.05 0.70 Q8 1 0.6938 0.6842 0.2389 11.00000 0.05 0.68 Q9 1 0.4200 0.7960 0.3825 11.00000 0.05 0.66 Q10 1 0.7531 0.5944 0.8195 11.00000 0.05 0.59 Q11 1 0.2846 0.9028 0.3150 11.00000 0.05 0.57 Q12 1 0.8570 0.4658 0.3134 11.00000 0.05 0.55 Q13 1 0.3789 0.5174 0.2525 11.00000 0.05 0.53 Q14 1 0.8129 0.3037 0.3164 11.00000 0.05 0.53 Q15 1 0.5231 0.6847 0.2380 11.00000 0.05 0.52 Q16 1 0.5138 0.4692 0.3079 11.00000 0.05 0.52 Q17 1 0.1839 0.4812 0.2975 11.00000 0.05 0.51 Q18 1 0.6592 0.5597 0.2918 11.00000 0.05 0.50 Q19 1 0.9204 0.8806 0.3325 11.00000 0.05 0.50 Q20 1 0.1742 0.4620 0.3159 11.00000 0.05 0.49 Q21 1 0.5606 0.6192 0.2996 11.00000 0.05 0.48 Q22 1 0.7402 0.7893 0.3811 11.00000 0.05 0.48 Q23 1 1.0065 0.4078 0.3681 11.00000 0.05 0.48 Q24 1 0.5195 1.0612 0.2483 11.00000 0.05 0.47 Q25 1 0.1798 0.7776 0.2488 11.00000 0.05 0.47 Q26 1 0.8561 0.6182 0.2868 11.00000 0.05 0.47 Q27 1 0.7522 0.2433 1.2423 11.00000 0.05 0.46 Q28 1 0.5748 0.8662 0.3289 11.00000 0.05 0.46 Q29 1 0.7374 0.4282 0.3674 11.00000 0.05 0.46 Q30 1 0.1176 1.2253 0.2435 11.00000 0.05 0.46 ; _shelx_res_checksum 52059 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz '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_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 Co1 Co 0.68676(15) 0.46542(9) 0.31029(7) 0.0157(2) Uani 1 1 d . . . . . P1 P 1.0306(3) 0.24490(15) 0.37745(13) 0.0164(4) Uani 1 1 d . . . . . P2 P 0.3464(3) 0.68900(15) 0.23891(13) 0.0161(4) Uani 1 1 d . . . . . O1 O 0.4089(9) 0.4223(5) 0.3554(5) 0.0262(14) Uani 1 1 d D . . . . H1A H 0.375993 0.378719 0.332213 0.039 Uiso 1 1 d DR U . . . H1B H 0.313357 0.476152 0.334096 0.039 Uiso 1 1 d DR U . . . O2 O 0.5558(9) 0.6257(4) 0.2495(4) 0.0204(13) Uani 1 1 d . . . . . O3 O 0.9625(9) 0.5080(5) 0.2571(4) 0.0247(14) Uani 1 1 d . . . . . H3A H 1.006677 0.546797 0.282975 0.037 Uiso 1 1 d DR U . . . H3B H 1.055174 0.452718 0.272393 0.037 Uiso 1 1 d DR U . . . O4 O 0.8315(10) 0.3139(5) 0.3734(4) 0.0215(13) Uani 1 1 d . . . . . O5 O 0.1985(8) 0.6246(4) 0.2944(4) 0.0214(12) Uani 1 1 d D . . . . O6 O 0.3454(9) 0.7904(5) 0.2540(4) 0.0263(13) Uani 1 1 d . . . . . O7 O 0.2607(9) 0.7206(5) 0.1341(4) 0.0224(12) Uani 1 1 d . . . . . O8 O -0.0189(11) 0.9223(6) -0.1316(4) 0.0438(17) Uani 1 1 d . . . . . H8 H -0.140070 0.942679 -0.139846 0.066 Uiso 1 1 calc R U . . . O9 O 0.2894(10) 0.7194(5) -0.0474(4) 0.0292(14) Uani 1 1 d . . . . . O10 O 0.1088(12) 0.5814(5) -0.1780(4) 0.0394(18) Uani 1 1 d . . . . . O11 O 0.2293(14) 0.2642(5) 0.0548(5) 0.048(2) Uani 1 1 d . . . . . O12 O 1.0133(9) 0.1414(5) 0.3676(4) 0.0253(13) Uani 1 1 d . . . . . O13 O 1.1807(9) 0.3021(4) 0.3124(4) 0.0203(11) Uani 1 1 d D . . . . O14 O 1.1236(9) 0.2167(5) 0.4805(4) 0.0270(14) Uani 1 1 d . . . . . O15 O 1.2708(11) -0.0008(5) 0.7526(4) 0.0412(17) Uani 1 1 d . . . . . H15 H 1.180773 -0.023038 0.785122 0.062 Uiso 1 1 calc R U . . . O16 O 1.4047(10) 0.2021(5) 0.6331(4) 0.0309(14) Uani 1 1 d . . . . . O17 O 1.1928(13) 0.3407(5) 0.8007(4) 0.0424(19) Uani 1 1 d . . . . . O18 O 1.1458(14) 0.6587(6) 0.5708(5) 0.049(2) Uani 1 1 d . . . . . O28 O 0.8247(10) 0.7604(5) 0.2443(6) 0.0447(18) Uani 1 1 d G . . . . H28A H 0.905849 0.703686 0.271970 0.067 Uiso 1 1 d DG U . . . H28B H 0.728613 0.740801 0.223799 0.067 Uiso 1 1 d G U . . . N1 N 0.7000(10) 0.4891(6) 0.4415(5) 0.0197(14) Uani 1 1 d . . . . . N2 N 0.6595(11) 0.4421(5) 1.1810(4) 0.0199(14) Uani 1 1 d . . . . . N3 N 0.6596(13) 0.4726(6) 0.8516(5) 0.0329(18) Uani 1 1 d . . . . . N4 N 0.6679(14) 0.4401(7) 0.7760(5) 0.0354(19) Uani 1 1 d . . . . . N5 N 0.1240(12) 0.5803(6) -0.0329(4) 0.0250(15) Uani 1 1 d . . . . . N6 N 0.1650(13) 0.4235(6) -0.0593(5) 0.0293(17) Uani 1 1 d . . . . . H6 H 0.168259 0.392366 -0.097669 0.035 Uiso 1 1 calc R U . . . N7 N 1.2124(13) 0.3452(6) 0.6548(5) 0.0311(18) Uani 1 1 d . . . . . N8 N 1.1661(13) 0.4987(6) 0.6828(5) 0.0302(17) Uani 1 1 d . . . . . H8A H 1.150682 0.529242 0.721552 0.036 Uiso 1 1 calc R U . . . C1 C 0.7031(12) 0.4025(7) 0.5183(5) 0.0215(16) Uani 1 1 d . . . . . H1 H 0.713423 0.337308 0.513090 0.026 Uiso 1 1 calc R U . . . C2 C 0.6916(13) 0.4076(7) 0.6041(6) 0.0238(18) Uani 1 1 d . . . . . H2 H 0.691410 0.346818 0.655452 0.029 Uiso 1 1 calc R U . . . C3 C 0.6801(14) 0.5042(7) 0.6132(6) 0.0258(18) Uani 1 1 d . . . . . C4 C 0.6760(16) 0.5921(7) 0.5340(6) 0.031(2) Uani 1 1 d . . . . . H4 H 0.666363 0.658230 0.537328 0.037 Uiso 1 1 calc R U . . . C5 C 0.6864(15) 0.5817(7) 0.4498(6) 0.031(2) Uani 1 1 d . . . . . H5 H 0.683688 0.641605 0.397334 0.037 Uiso 1 1 calc R U . . . C6 C 0.6702(16) 0.5166(8) 0.7021(6) 0.034(2) Uani 1 1 d . . . . . H6A H 0.665494 0.583348 0.703662 0.040 Uiso 1 1 calc R U . . . C7 C 0.6877(14) 0.3452(7) 1.1776(6) 0.0244(18) Uani 1 1 d . . . . . H7 H 0.703076 0.287429 1.232467 0.029 Uiso 1 1 calc R U . . . C8 C 0.6950(15) 0.3273(7) 1.0970(6) 0.029(2) Uani 1 1 d . . . . . H8B H 0.713804 0.259197 1.097602 0.035 Uiso 1 1 calc R U . . . C9 C 0.6734(14) 0.4143(7) 1.0141(6) 0.0258(18) Uani 1 1 d . . . . . C10 C 0.6444(13) 0.5141(7) 1.0180(6) 0.0239(18) Uani 1 1 d . . . . . H10 H 0.628611 0.573673 0.964483 0.029 Uiso 1 1 calc R U . . . C11 C 0.6393(14) 0.5236(7) 1.1015(6) 0.0257(18) Uani 1 1 d . . . . . H11 H 0.620515 0.590838 1.102847 0.031 Uiso 1 1 calc R U . . . C12 C 0.6789(15) 0.3975(8) 0.9273(6) 0.032(2) Uani 1 1 d . . . . . H12 H 0.697111 0.329137 0.928530 0.038 Uiso 1 1 calc R U . . . C13 C 0.3531(13) 0.7961(6) 0.0639(5) 0.0245(16) Uani 1 1 d . . . . . H13A H 0.495016 0.770104 0.065459 0.029 Uiso 1 1 calc R U . . . H13B H 0.337412 0.861734 0.073907 0.029 Uiso 1 1 calc R U . . . C14 C 0.2560(13) 0.8140(6) -0.0275(5) 0.0250(17) Uani 1 1 d . . . . . H14 H 0.316882 0.867594 -0.074454 0.030 Uiso 1 1 calc R U . . . C15 C 0.0280(14) 0.8503(7) -0.0383(6) 0.0292(18) Uani 1 1 d . . . . . H15A H -0.018184 0.882878 0.005451 0.035 Uiso 1 1 calc R U . . . C16 C -0.0544(14) 0.7503(7) -0.0212(6) 0.030(2) Uani 1 1 d . . . . . H16A H -0.186856 0.764329 -0.050636 0.036 Uiso 1 1 calc R U . . . H16B H -0.058545 0.710133 0.043655 0.036 Uiso 1 1 calc R U . . . C17 C 0.1030(13) 0.6939(7) -0.0663(6) 0.0245(18) Uani 1 1 d . . . . . H17 H 0.072722 0.722528 -0.132605 0.029 Uiso 1 1 calc R U . . . C18 C 0.1308(14) 0.5326(7) -0.0960(6) 0.0284(19) Uani 1 1 d . . . . . C19 C 0.1943(14) 0.3594(7) 0.0321(6) 0.0278(19) Uani 1 1 d . . . . . C20 C 0.1804(14) 0.4165(7) 0.0934(6) 0.0273(19) Uani 1 1 d . . . . . H20 H 0.193047 0.379788 0.156321 0.033 Uiso 1 1 calc R U . . . C21 C 0.1498(14) 0.5209(7) 0.0603(6) 0.0268(19) Uani 1 1 d . . . . . H21 H 0.145495 0.555524 0.100957 0.032 Uiso 1 1 calc R U . . . C22 C 1.3150(14) 0.1517(8) 0.5064(6) 0.033(2) Uani 1 1 d . . . . . H22A H 1.417216 0.190463 0.474271 0.039 Uiso 1 1 calc R U . . . H22B H 1.318116 0.090639 0.489911 0.039 Uiso 1 1 calc R U . . . C23 C 1.3565(14) 0.1168(7) 0.6092(5) 0.0276(18) Uani 1 1 d . . . . . H23 H 1.471612 0.059666 0.628092 0.033 Uiso 1 1 calc R U . . . C24 C 1.1848(14) 0.0791(7) 0.6660(6) 0.0290(19) Uani 1 1 d . . . . . H24 H 1.096251 0.051730 0.634646 0.035 Uiso 1 1 calc R U . . . C25 C 1.0803(16) 0.1764(8) 0.6788(7) 0.035(2) Uani 1 1 d . . . . . H25A H 1.006032 0.159074 0.733579 0.042 Uiso 1 1 calc R U . . . H25B H 0.990489 0.220599 0.626391 0.042 Uiso 1 1 calc R U . . . C26 C 1.2573(15) 0.2291(7) 0.6874(5) 0.028(2) Uani 1 1 d . . . . . H26 H 1.309469 0.200886 0.751335 0.034 Uiso 1 1 calc R U . . . C27 C 1.2026(15) 0.4040(8) 0.5632(6) 0.029(2) Uani 1 1 d . . . . . H27 H 1.215533 0.369136 0.522570 0.035 Uiso 1 1 calc R U . . . C28 C 1.1753(14) 0.5092(8) 0.5289(7) 0.031(2) Uani 1 1 d . . . . . H28 H 1.165749 0.546267 0.466054 0.038 Uiso 1 1 calc R U . . . C29 C 1.1611(15) 0.5635(7) 0.5913(6) 0.029(2) Uani 1 1 d . . . . . C30 C 1.1926(15) 0.3923(7) 0.7173(6) 0.0295(19) Uani 1 1 d . . . . . Co2 Co 0.56980(15) 1.02056(8) 0.30923(8) 0.0234(2) Uani 1 1 d D . . . . O19 O 0.6827(10) 1.0555(6) 0.4145(4) 0.0373(16) Uani 1 1 d . . . . . H19A H 0.775506 1.091725 0.395551 0.056 Uiso 1 1 d R U . . . H19B H 0.740550 0.999074 0.456261 0.056 Uiso 1 1 d DR U . . . O20 O 0.3195(10) 0.9821(5) 0.3834(5) 0.0336(15) Uani 1 1 d . . . . . H20A H 0.322737 0.911986 0.409008 0.050 Uiso 1 1 d R U . . . H20B H 0.205140 1.002701 0.347482 0.050 Uiso 1 1 d R U . . . O21 O 0.4043(11) 1.1710(5) 0.2419(4) 0.0324(15) Uani 1 1 d G . . . . H21A H 0.405145 1.225864 0.253851 0.049 Uiso 1 1 d DG U . . . H21B H 0.340242 1.193073 0.190222 0.049 Uiso 1 1 d DG U . . . O22 O 0.8232(10) 1.0755(5) 0.2394(4) 0.0313(14) Uani 1 1 d . . . . . H22C H 0.911535 1.023166 0.240596 0.047 Uiso 1 1 d R U . . . H22D H 0.882182 1.105682 0.268480 0.047 Uiso 1 1 d R U . . . O23 O 0.7191(12) 0.8606(6) 0.3712(5) 0.0409(17) Uani 1 1 d . . . . . H23A H 0.852438 0.855261 0.384882 0.061 Uiso 1 1 d R U . . . H23B H 0.723983 0.825042 0.332279 0.061 Uiso 1 1 d R U . . . O24 O 0.4903(13) 0.9748(6) 0.2030(5) 0.0459(19) Uani 1 1 d G . . . . H24A H 0.470119 1.016927 0.147560 0.069 Uiso 1 1 d DG U . . . H24B H 0.408785 0.932247 0.209212 0.069 Uiso 1 1 d DG U . . . O25 O 0.1455(11) 0.8131(5) 0.4022(5) 0.0366(15) Uani 1 1 d G . . . . H25C H 0.132067 0.759152 0.448486 0.055 Uiso 1 1 d G U . . . H25D H 0.148846 0.792202 0.357576 0.055 Uiso 1 1 d G U . . . O26 O 0.5951(18) 0.0138(9) 0.8561(9) 0.098(4) Uani 1 1 d G . . . . H26A H 0.614092 0.077152 0.833392 0.147 Uiso 1 1 d G U . . . H26B H 0.510366 0.009439 0.818488 0.147 Uiso 1 1 d G U . . . O27 O 1.0014(11) 0.9414(5) 0.1604(5) 0.0401(16) Uani 1 1 d G . . . . H27A H 0.906849 0.905712 0.170310 0.060 Uiso 1 1 d G U . . . H27B H 1.098682 0.899940 0.195888 0.060 Uiso 1 1 d G U . . . O29 O 0.984(3) 0.1237(12) 0.9941(10) 0.149(7) Uani 1 1 d . . . . . O30 O 0.724(3) 0.1988(9) 0.8428(9) 0.114(5) Uani 1 1 d . . . . . O31 O 0.460(3) 1.0889(13) 0.0155(9) 0.162(7) Uani 1 1 d . U . . . O32 O 0.742(2) 0.8970(10) 0.5809(8) 0.105(4) Uani 1 1 d D . . . . N9 N 0.533(2) 0.8067(8) 0.6783(7) 0.067(3) Uani 1 1 d . . . . . C31 C 0.329(3) 0.7775(16) 0.6978(15) 0.109(6) Uani 1 1 d . U . . . H31A H 0.253354 0.795036 0.641148 0.164 Uiso 1 1 calc R U . . . H31B H 0.261279 0.815399 0.732520 0.164 Uiso 1 1 calc R U . . . H31C H 0.342112 0.703328 0.732087 0.164 Uiso 1 1 calc R U . . . C32 C 0.645(3) 0.7865(16) 0.7577(12) 0.110(7) Uani 1 1 d . U . . . H32A H 0.784129 0.770892 0.748040 0.165 Uiso 1 1 calc R U . . . H32B H 0.606729 0.727496 0.805798 0.165 Uiso 1 1 calc R U . . . H32C H 0.621742 0.847091 0.774419 0.165 Uiso 1 1 calc R U . . . C33 C 0.569(3) 0.8592(11) 0.5981(10) 0.075(4) Uani 1 1 d . . . . . H33 H 0.475630 0.872214 0.550279 0.090 Uiso 1 1 calc R U . . . 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 Co1 0.0176(5) 0.0187(4) 0.0120(4) -0.0074(3) 0.0013(3) -0.0022(3) P1 0.0199(10) 0.0171(10) 0.0130(9) -0.0067(8) 0.0008(8) -0.0024(8) P2 0.0188(10) 0.0154(9) 0.0145(9) -0.0062(8) -0.0001(7) -0.0025(8) O1 0.017(3) 0.028(3) 0.042(4) -0.022(3) 0.008(3) -0.007(3) O2 0.016(3) 0.016(3) 0.025(3) -0.005(2) 0.000(2) 0.003(2) O3 0.019(3) 0.027(3) 0.030(3) -0.012(3) -0.001(3) -0.002(3) O4 0.028(3) 0.021(3) 0.017(3) -0.010(2) 0.002(2) -0.003(3) O5 0.020(3) 0.019(3) 0.024(3) -0.006(2) 0.004(2) -0.004(2) O6 0.032(3) 0.023(3) 0.030(3) -0.016(3) 0.004(3) -0.006(3) O7 0.024(3) 0.025(3) 0.015(3) -0.002(2) -0.005(2) -0.008(2) O8 0.043(4) 0.037(4) 0.029(3) 0.010(3) -0.011(3) 0.003(3) O9 0.033(3) 0.030(3) 0.029(3) -0.016(3) 0.003(3) -0.004(3) O10 0.074(5) 0.033(4) 0.013(3) -0.009(3) 0.003(3) -0.010(3) O11 0.085(6) 0.027(4) 0.031(4) -0.011(3) -0.003(4) -0.002(4) O12 0.023(3) 0.021(3) 0.034(3) -0.012(3) 0.007(3) -0.004(2) O13 0.024(3) 0.022(3) 0.014(3) -0.007(2) 0.003(2) -0.005(2) O14 0.032(3) 0.030(3) 0.016(3) -0.010(2) 0.001(2) 0.008(3) O15 0.047(4) 0.033(4) 0.027(3) 0.005(3) -0.004(3) 0.002(3) O16 0.033(3) 0.032(3) 0.033(3) -0.019(3) 0.002(3) 0.000(3) O17 0.078(6) 0.033(4) 0.018(3) -0.012(3) 0.005(3) -0.007(4) O18 0.080(6) 0.030(4) 0.033(4) -0.008(3) 0.003(4) -0.011(4) O28 0.023(3) 0.032(4) 0.075(5) -0.017(4) 0.003(3) 0.001(3) N1 0.017(3) 0.027(4) 0.017(3) -0.011(3) -0.002(3) 0.000(3) N2 0.026(4) 0.021(3) 0.016(3) -0.008(3) 0.004(3) -0.010(3) N3 0.048(5) 0.038(4) 0.018(4) -0.017(3) 0.005(3) -0.004(4) N4 0.048(5) 0.049(5) 0.014(3) -0.018(3) 0.005(3) -0.009(4) N5 0.037(4) 0.027(4) 0.009(3) -0.005(3) 0.000(3) -0.004(3) N6 0.043(5) 0.029(4) 0.019(4) -0.012(3) 0.004(3) -0.006(3) N7 0.043(5) 0.029(4) 0.021(4) -0.013(3) 0.000(3) 0.004(3) N8 0.042(4) 0.030(4) 0.018(4) -0.010(3) 0.002(3) -0.002(3) C1 0.024(4) 0.025(4) 0.019(4) -0.012(3) 0.001(3) -0.003(3) C2 0.028(4) 0.024(4) 0.016(4) -0.004(3) 0.000(3) -0.003(3) C3 0.030(4) 0.032(5) 0.015(4) -0.011(3) -0.003(3) 0.003(4) C4 0.048(6) 0.029(5) 0.020(4) -0.013(4) 0.000(4) -0.010(4) C5 0.043(6) 0.028(5) 0.020(4) -0.009(4) -0.001(4) -0.001(4) C6 0.045(6) 0.037(5) 0.024(5) -0.019(4) -0.002(4) -0.002(4) C7 0.036(5) 0.020(4) 0.016(4) -0.005(3) -0.004(3) -0.005(4) C8 0.046(6) 0.021(4) 0.023(4) -0.012(3) -0.001(4) -0.003(4) C9 0.036(5) 0.029(4) 0.015(4) -0.011(3) 0.002(3) -0.007(4) C10 0.031(5) 0.024(4) 0.015(4) -0.005(3) 0.003(3) -0.003(3) C11 0.032(5) 0.023(4) 0.022(4) -0.009(3) -0.004(3) -0.003(4) C12 0.039(5) 0.040(5) 0.018(4) -0.015(4) 0.003(4) -0.005(4) C13 0.030(4) 0.020(4) 0.021(4) -0.005(3) -0.002(3) -0.005(3) C14 0.031(4) 0.024(4) 0.014(3) -0.003(3) 0.001(3) 0.000(3) C15 0.034(5) 0.024(4) 0.025(4) -0.008(3) 0.000(4) 0.003(4) C16 0.027(5) 0.034(5) 0.025(4) -0.008(4) 0.001(4) -0.003(4) C17 0.028(5) 0.025(4) 0.021(4) -0.008(3) -0.002(3) -0.008(4) C18 0.036(5) 0.029(4) 0.024(4) -0.014(4) 0.002(4) -0.002(4) C19 0.033(5) 0.028(5) 0.020(4) -0.008(4) -0.001(4) -0.002(4) C20 0.037(5) 0.031(5) 0.012(4) -0.006(3) 0.004(3) -0.005(4) C21 0.035(5) 0.029(5) 0.014(4) -0.008(3) -0.004(3) 0.002(4) C22 0.036(5) 0.038(5) 0.022(4) -0.016(4) -0.004(4) 0.010(4) C23 0.039(5) 0.024(4) 0.017(4) -0.006(3) -0.003(3) 0.002(4) C24 0.037(5) 0.022(4) 0.021(4) -0.004(3) -0.004(4) 0.002(4) C25 0.039(5) 0.032(5) 0.029(5) -0.010(4) 0.008(4) 0.004(4) C26 0.040(5) 0.031(5) 0.010(4) -0.008(3) -0.003(4) 0.006(4) C27 0.038(5) 0.034(5) 0.016(4) -0.012(4) 0.002(4) 0.000(4) C28 0.033(5) 0.033(5) 0.026(5) -0.011(4) 0.000(4) 0.001(4) C29 0.036(5) 0.026(5) 0.024(5) -0.008(4) 0.002(4) -0.006(4) C30 0.041(5) 0.029(4) 0.020(4) -0.013(4) -0.001(4) 0.001(4) Co2 0.0242(6) 0.0206(5) 0.0265(6) -0.0100(4) 0.0026(4) -0.0036(4) O19 0.038(4) 0.045(4) 0.031(3) -0.009(3) 0.006(3) -0.023(3) O20 0.028(3) 0.030(3) 0.048(4) -0.018(3) 0.010(3) -0.011(3) O21 0.044(4) 0.019(3) 0.029(3) -0.007(3) 0.006(3) 0.004(3) O22 0.025(3) 0.034(3) 0.041(4) -0.021(3) 0.005(3) -0.008(3) O23 0.044(4) 0.037(4) 0.042(4) -0.015(3) -0.001(3) -0.008(3) O24 0.070(6) 0.040(4) 0.036(4) -0.018(3) -0.001(4) -0.023(4) O25 0.049(4) 0.030(3) 0.031(3) -0.010(3) 0.013(3) -0.006(3) O26 0.061(7) 0.087(8) 0.117(10) -0.010(7) -0.045(7) 0.000(6) O27 0.036(4) 0.033(4) 0.048(4) -0.013(3) 0.006(3) 0.000(3) O29 0.23(2) 0.105(10) 0.091(10) -0.008(8) -0.055(11) -0.026(11) O30 0.177(14) 0.080(8) 0.095(9) -0.047(7) -0.009(9) -0.012(8) O31 0.27(2) 0.137(13) 0.071(8) -0.028(8) 0.037(11) -0.026(12) O32 0.125(11) 0.093(9) 0.073(8) 0.003(6) 0.019(7) -0.035(8) N9 0.121(10) 0.047(6) 0.033(5) -0.012(4) 0.011(6) -0.028(6) C31 0.108(13) 0.111(13) 0.139(15) -0.067(12) 0.044(12) -0.056(11) C32 0.148(16) 0.105(13) 0.075(10) -0.044(10) -0.036(11) 0.009(12) C33 0.110(13) 0.058(8) 0.057(8) -0.021(7) 0.009(9) -0.015(9) 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' P P 0.1023 0.0942 '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 O1 Co1 O2 91.5(2) . . ? O1 Co1 O3 176.5(3) . . ? O1 Co1 N1 82.4(2) . . ? O1 Co1 N2 95.2(3) . 1_554 ? O2 Co1 O3 88.3(2) . . ? O2 Co1 N1 87.2(3) . . ? O2 Co1 N2 92.1(3) . 1_554 ? O3 Co1 N1 101.1(3) . . ? O3 Co1 N2 81.3(2) . 1_554 ? O4 Co1 O1 91.7(3) . . ? O4 Co1 O2 175.4(3) . . ? O4 Co1 O3 88.7(2) . . ? O4 Co1 N1 90.0(2) . . ? O4 Co1 N2 90.8(2) . 1_554 ? N2 Co1 N1 177.5(3) 1_554 . ? O4 P1 O12 114.1(3) . . ? O4 P1 O13 113.8(3) . . ? O4 P1 O14 103.6(3) . . ? O12 P1 O13 111.3(3) . . ? O12 P1 O14 107.2(3) . . ? O13 P1 O14 106.0(3) . . ? O2 P2 O7 107.8(3) . . ? O5 P2 O2 112.8(3) . . ? O5 P2 O6 113.0(3) . . ? O5 P2 O7 103.1(3) . . ? O6 P2 O2 112.5(4) . . ? O6 P2 O7 106.9(3) . . ? Co1 O1 H1A 110.7 . . ? Co1 O1 H1B 110.6 . . ? H1A O1 H1B 103.4 . . ? P2 O2 Co1 136.0(4) . . ? Co1 O3 H3A 110.4 . . ? Co1 O3 H3B 110.3 . . ? H3A O3 H3B 103.5 . . ? P1 O4 Co1 141.1(4) . . ? C13 O7 P2 116.8(5) . . ? C15 O8 H8 109.5 . . ? C17 O9 C14 110.1(7) . . ? C22 O14 P1 117.6(5) . . ? C24 O15 H15 109.5 . . ? C26 O16 C23 109.9(7) . . ? H28A O28 H28B 104.4 . . ? C1 N1 Co1 116.3(5) . . ? C5 N1 Co1 125.1(6) . . ? C5 N1 C1 118.3(7) . . ? C7 N2 Co1 121.6(5) . 1_556 ? C11 N2 Co1 120.7(5) . 1_556 ? C11 N2 C7 117.1(7) . . ? C12 N3 N4 113.3(8) . . ? C6 N4 N3 111.2(8) . . ? C18 N5 C17 118.2(7) . . ? C18 N5 C21 120.9(7) . . ? C21 N5 C17 120.7(7) . . ? C18 N6 H6 116.5 . . ? C19 N6 H6 116.5 . . ? C19 N6 C18 127.1(8) . . ? C27 N7 C26 120.1(7) . . ? C30 N7 C26 119.1(7) . . ? C30 N7 C27 120.7(8) . . ? C29 N8 H8A 116.6 . . ? C30 N8 H8A 116.6 . . ? C30 N8 C29 126.7(8) . . ? N1 C1 H1 118.8 . . ? N1 C1 C2 122.3(8) . . ? C2 C1 H1 118.8 . . ? C1 C2 H2 120.2 . . ? C1 C2 C3 119.5(8) . . ? C3 C2 H2 120.2 . . ? C2 C3 C6 123.2(8) . . ? C4 C3 C2 117.5(8) . . ? C4 C3 C6 119.3(8) . . ? C3 C4 H4 120.0 . . ? C3 C4 C5 120.1(9) . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 122.2(9) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N4 C6 C3 122.2(9) . . ? N4 C6 H6A 118.9 . . ? C3 C6 H6A 118.9 . . ? N2 C7 H7 118.3 . . ? N2 C7 C8 123.4(8) . . ? C8 C7 H7 118.3 . . ? C7 C8 H8B 120.8 . . ? C7 C8 C9 118.5(8) . . ? C9 C8 H8B 120.8 . . ? C8 C9 C12 119.6(8) . . ? C10 C9 C8 117.9(7) . . ? C10 C9 C12 122.5(8) . . ? C9 C10 H10 120.4 . . ? C11 C10 C9 119.2(8) . . ? C11 C10 H10 120.4 . . ? N2 C11 C10 124.0(8) . . ? N2 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? N3 C12 C9 121.9(9) . . ? N3 C12 H12 119.0 . . ? C9 C12 H12 119.0 . . ? O7 C13 H13A 109.9 . . ? O7 C13 H13B 109.9 . . ? O7 C13 C14 109.0(7) . . ? H13A C13 H13B 108.3 . . ? C14 C13 H13A 109.9 . . ? C14 C13 H13B 109.9 . . ? O9 C14 C13 111.2(7) . . ? O9 C14 H14 108.1 . . ? O9 C14 C15 105.5(7) . . ? C13 C14 H14 108.1 . . ? C13 C14 C15 115.6(7) . . ? C15 C14 H14 108.1 . . ? O8 C15 C14 107.0(7) . . ? O8 C15 H15A 111.7 . . ? O8 C15 C16 110.8(7) . . ? C14 C15 H15A 111.7 . . ? C16 C15 C14 103.7(7) . . ? C16 C15 H15A 111.7 . . ? C15 C16 H16A 111.7 . . ? C15 C16 H16B 111.7 . . ? C15 C16 C17 100.4(7) . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16A 111.7 . . ? C17 C16 H16B 111.7 . . ? O9 C17 N5 107.7(7) . . ? O9 C17 C16 105.3(7) . . ? O9 C17 H17 109.1 . . ? N5 C17 C16 116.2(7) . . ? N5 C17 H17 109.1 . . ? C16 C17 H17 109.1 . . ? O10 C18 N5 123.2(8) . . ? O10 C18 N6 121.7(8) . . ? N5 C18 N6 115.2(8) . . ? O11 C19 N6 120.3(8) . . ? O11 C19 C20 125.9(8) . . ? N6 C19 C20 113.8(8) . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.4(8) . . ? C21 C20 H20 119.8 . . ? N5 C21 H21 118.7 . . ? C20 C21 N5 122.6(8) . . ? C20 C21 H21 118.7 . . ? O14 C22 H22A 109.8 . . ? O14 C22 H22B 109.8 . . ? O14 C22 C23 109.4(7) . . ? H22A C22 H22B 108.2 . . ? C23 C22 H22A 109.8 . . ? C23 C22 H22B 109.8 . . ? O16 C23 C22 111.1(7) . . ? O16 C23 H23 108.3 . . ? O16 C23 C24 105.7(7) . . ? C22 C23 H23 108.3 . . ? C24 C23 C22 114.9(8) . . ? C24 C23 H23 108.3 . . ? O15 C24 C23 107.1(7) . . ? O15 C24 H24 111.6 . . ? O15 C24 C25 111.3(7) . . ? C23 C24 H24 111.6 . . ? C25 C24 C23 103.1(7) . . ? C25 C24 H24 111.6 . . ? C24 C25 H25A 111.5 . . ? C24 C25 H25B 111.5 . . ? C24 C25 C26 101.5(8) . . ? H25A C25 H25B 109.3 . . ? C26 C25 H25A 111.5 . . ? C26 C25 H25B 111.5 . . ? O16 C26 N7 107.7(7) . . ? O16 C26 C25 106.2(7) . . ? O16 C26 H26 109.3 . . ? N7 C26 C25 114.8(8) . . ? N7 C26 H26 109.3 . . ? C25 C26 H26 109.3 . . ? N7 C27 H27 118.3 . . ? C28 C27 N7 123.4(8) . . ? C28 C27 H27 118.3 . . ? C27 C28 H28 120.7 . . ? C27 C28 C29 118.6(9) . . ? C29 C28 H28 120.7 . . ? O18 C29 N8 119.2(8) . . ? O18 C29 C28 126.3(9) . . ? N8 C29 C28 114.5(8) . . ? O17 C30 N7 122.0(8) . . ? O17 C30 N8 122.1(8) . . ? N8 C30 N7 115.9(8) . . ? O19 Co2 O20 89.1(3) . . ? O19 Co2 O21 94.8(3) . . ? O19 Co2 O22 85.3(3) . . ? O19 Co2 O23 90.5(3) . . ? O19 Co2 O24 173.0(4) . . ? O20 Co2 O21 87.4(3) . . ? O20 Co2 O22 172.8(3) . . ? O20 Co2 O23 90.4(3) . . ? O20 Co2 O24 95.6(3) . . ? O21 Co2 O22 88.5(3) . . ? O21 Co2 O23 174.2(3) . . ? O21 Co2 O24 90.5(3) . . ? O22 Co2 O23 94.2(3) . . ? O24 Co2 O22 90.3(3) . . ? O24 Co2 O23 84.3(3) . . ? Co2 O19 H19A 109.7 . . ? Co2 O19 H19B 109.6 . . ? H19A O19 H19B 104.5 . . ? Co2 O20 H20A 112.2 . . ? Co2 O20 H20B 112.6 . . ? H20A O20 H20B 101.2 . . ? Co2 O21 H21A 128.1 . . ? Co2 O21 H21B 126.3 . . ? H21A O21 H21B 104.5 . . ? Co2 O22 H22C 110.1 . . ? Co2 O22 H22D 110.0 . . ? H22C O22 H22D 104.1 . . ? Co2 O23 H23A 112.9 . . ? Co2 O23 H23B 112.8 . . ? H23A O23 H23B 101.0 . . ? Co2 O24 H24A 123.1 . . ? Co2 O24 H24B 122.4 . . ? H24A O24 H24B 104.6 . . ? H25C O25 H25D 104.5 . . ? H26A O26 H26B 104.3 . . ? H27A O27 H27B 104.4 . . ? C32 N9 C31 111.7(14) . . ? C33 N9 C31 119.3(15) . . ? C33 N9 C32 127.9(17) . . ? N9 C31 H31A 109.5 . . ? N9 C31 H31B 109.5 . . ? N9 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N9 C32 H32A 109.5 . . ? N9 C32 H32B 109.5 . . ? N9 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O32 C33 H33 120.0 . . ? N9 C33 O32 120.1(15) . . ? N9 C33 H33 120.0 . . ? 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 Co1 O1 2.110(6) . ? Co1 O2 2.114(6) . ? Co1 O3 2.127(6) . ? Co1 O4 2.048(6) . ? Co1 N1 2.213(7) . ? Co1 N2 2.188(7) 1_554 ? P1 O4 1.514(7) . ? P1 O12 1.522(6) . ? P1 O13 1.539(6) . ? P1 O14 1.626(6) . ? P2 O2 1.522(6) . ? P2 O5 1.507(6) . ? P2 O6 1.509(6) . ? P2 O7 1.626(6) . ? O1 H1A 0.8674 . ? O1 H1B 0.8691 . ? O3 H3A 0.8704 . ? O3 H3B 0.8685 . ? O7 C13 1.437(9) . ? O8 H8 0.8200 . ? O8 C15 1.444(10) . ? O9 C14 1.442(10) . ? O9 C17 1.426(11) . ? O10 C18 1.215(11) . ? O11 C19 1.218(11) . ? O14 C22 1.425(10) . ? O15 H15 0.8200 . ? O15 C24 1.455(10) . ? O16 C23 1.448(10) . ? O16 C26 1.409(10) . ? O17 C30 1.244(11) . ? O18 C29 1.226(11) . ? O28 H28A 0.8513 . ? O28 H28B 0.8511 . ? N1 C1 1.353(11) . ? N1 C5 1.326(11) . ? N2 C7 1.349(10) . ? N2 C11 1.333(11) . ? N3 N4 1.418(8) . ? N3 C12 1.253(12) . ? N4 C6 1.256(12) . ? N5 C17 1.449(11) . ? N5 C18 1.379(11) . ? N5 C21 1.389(10) . ? N6 H6 0.8600 . ? N6 C18 1.389(12) . ? N6 C19 1.381(11) . ? N7 C26 1.479(12) . ? N7 C27 1.368(11) . ? N7 C30 1.363(11) . ? N8 H8A 0.8600 . ? N8 C29 1.387(11) . ? N8 C30 1.355(12) . ? C1 H1 0.9300 . ? C1 C2 1.380(11) . ? C2 H2 0.9300 . ? C2 C3 1.389(12) . ? C3 C4 1.384(13) . ? C3 C6 1.473(12) . ? C4 H4 0.9300 . ? C4 C5 1.387(12) . ? C5 H5 0.9300 . ? C6 H6A 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.380(11) . ? C8 H8B 0.9300 . ? C8 C9 1.404(12) . ? C9 C10 1.392(12) . ? C9 C12 1.468(12) . ? C10 H10 0.9300 . ? C10 C11 1.369(12) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.502(11) . ? C14 H14 0.9800 . ? C14 C15 1.539(12) . ? C15 H15A 0.9800 . ? C15 C16 1.509(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.549(13) . ? C17 H17 0.9800 . ? C19 C20 1.452(12) . ? C20 H20 0.9300 . ? C20 C21 1.327(12) . ? C21 H21 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.524(11) . ? C23 H23 0.9800 . ? C23 C24 1.507(13) . ? C24 H24 0.9800 . ? C24 C25 1.504(12) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 C26 1.531(15) . ? C26 H26 0.9800 . ? C27 H27 0.9300 . ? C27 C28 1.338(13) . ? C28 H28 0.9300 . ? C28 C29 1.437(13) . ? Co2 O19 2.069(7) . ? Co2 O20 2.085(6) . ? Co2 O21 2.093(6) . ? Co2 O22 2.128(6) . ? Co2 O23 2.147(7) . ? Co2 O24 2.095(7) . ? O19 H19A 0.8521 . ? O19 H19B 0.8519 . ? O20 H20A 0.9030 . ? O20 H20B 0.9044 . ? O21 H21A 0.8494 . ? O21 H21B 0.8501 . ? O22 H22C 0.8604 . ? O22 H22D 0.8596 . ? O23 H23A 0.9150 . ? O23 H23B 0.9158 . ? O24 H24A 0.8503 . ? O24 H24B 0.8501 . ? O25 H25C 0.8486 . ? O25 H25D 0.8512 . ? O26 H26A 0.8491 . ? O26 H26B 0.8508 . ? O27 H27A 0.8502 . ? O27 H27B 0.8514 . ? O32 C33 1.35(2) . ? N9 C31 1.50(2) . ? N9 C32 1.378(19) . ? N9 C33 1.250(16) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33 0.9300 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H1A O13 0.87 1.92 2.697(8) 149.2 1_455 yes O1 H1B O5 0.87 1.95 2.758(8) 154.6 . yes O3 H3A O5 0.87 1.86 2.653(8) 149.9 1_655 yes O3 H3B O13 0.87 1.99 2.820(8) 159.4 . yes O8 H8 O26 0.82 1.90 2.698(14) 164.9 1_464 yes O15 H15 O8 0.82 1.93 2.746(10) 176.2 1_646 yes O28 H28A O5 0.85 2.07 2.831(9) 147.8 1_655 yes O28 H28B O2 0.85 2.05 2.789(9) 145.1 . yes N6 H6 O17 0.86 1.98 2.829(10) 170.8 1_454 yes N8 H8A O10 0.86 1.97 2.825(9) 172.5 1_656 yes O19 H19A O12 0.85 1.84 2.679(9) 167.0 1_565 yes O19 H19B O32 0.85 1.95 2.713(13) 148.0 . yes O20 H20A O25 0.90 1.99 2.710(9) 135.3 . yes O21 H21A O13 0.85 2.12 2.730(8) 128.4 1_465 yes O22 H22C O27 0.86 2.02 2.731(10) 139.2 . yes O22 H22D O12 0.86 2.05 2.883(9) 164.3 1_565 yes O23 H23A O25 0.92 1.97 2.865(11) 164.8 1_655 yes O23 H23B O28 0.92 1.98 2.857(11) 160.9 . yes O24 H24A O31 0.85 1.95 2.782(16) 167.6 . yes O24 H24B O6 0.85 1.95 2.725(9) 151.3 . yes O25 H25C O18 0.85 1.91 2.732(10) 162.4 1_455 yes O25 H25D O6 0.85 2.11 2.788(9) 136.4 . yes O26 H26A O30 0.85 2.00 2.773(17) 151.2 . yes O26 H26B O15 0.85 1.98 2.817(13) 167.1 1_455 yes O27 H27A O28 0.85 2.09 2.826(10) 145.0 . yes O27 H27B O6 0.85 2.03 2.867(9) 166.0 1_655 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co1 N1 C1 C2 -173.5(6) . . . . ? Co1 N1 C5 C4 173.5(7) . . . . ? Co1 N2 C7 C8 -172.2(7) 1_556 . . . ? Co1 N2 C11 C10 172.2(7) 1_556 . . . ? P1 O14 C22 C23 -168.8(6) . . . . ? P2 O7 C13 C14 179.4(5) . . . . ? O2 P2 O7 C13 -69.4(6) . . . . ? O4 P1 O14 C22 -179.7(6) . . . . ? O5 P2 O2 Co1 9.0(7) . . . . ? O5 P2 O7 C13 171.1(6) . . . . ? O6 P2 O2 Co1 138.3(5) . . . . ? O6 P2 O7 C13 51.7(6) . . . . ? O7 P2 O2 Co1 -104.1(5) . . . . ? O7 C13 C14 O9 -63.7(9) . . . . ? O7 C13 C14 C15 56.6(9) . . . . ? O8 C15 C16 C17 77.9(8) . . . . ? O9 C14 C15 O8 -92.0(8) . . . . ? O9 C14 C15 C16 25.1(8) . . . . ? O11 C19 C20 C21 177.1(10) . . . . ? O12 P1 O4 Co1 -131.0(6) . . . . ? O12 P1 O14 C22 59.3(7) . . . . ? O13 P1 O4 Co1 -1.9(7) . . . . ? O13 P1 O14 C22 -59.7(7) . . . . ? O14 P1 O4 Co1 112.8(6) . . . . ? O14 C22 C23 O16 -74.5(10) . . . . ? O14 C22 C23 C24 45.4(10) . . . . ? O15 C24 C25 C26 78.3(9) . . . . ? O16 C23 C24 O15 -88.4(8) . . . . ? O16 C23 C24 C25 29.1(9) . . . . ? N1 C1 C2 C3 -1.3(13) . . . . ? N2 C7 C8 C9 0.5(15) . . . . ? N3 N4 C6 C3 179.5(9) . . . . ? N4 N3 C12 C9 -179.6(9) . . . . ? N6 C19 C20 C21 -2.4(13) . . . . ? N7 C27 C28 C29 1.8(15) . . . . ? C1 N1 C5 C4 0.2(14) . . . . ? C1 C2 C3 C4 1.5(13) . . . . ? C1 C2 C3 C6 -179.1(9) . . . . ? C2 C3 C4 C5 -1.0(15) . . . . ? C2 C3 C6 N4 -1.3(16) . . . . ? C3 C4 C5 N1 0.1(16) . . . . ? C4 C3 C6 N4 178.0(10) . . . . ? C5 N1 C1 C2 0.4(13) . . . . ? C6 C3 C4 C5 179.6(9) . . . . ? C7 N2 C11 C10 0.4(13) . . . . ? C7 C8 C9 C10 -0.4(14) . . . . ? C7 C8 C9 C12 -179.5(9) . . . . ? C8 C9 C10 C11 0.4(14) . . . . ? C8 C9 C12 N3 179.8(10) . . . . ? C9 C10 C11 N2 -0.4(14) . . . . ? C10 C9 C12 N3 0.8(15) . . . . ? C11 N2 C7 C8 -0.4(13) . . . . ? C12 N3 N4 C6 -172.7(10) . . . . ? C12 C9 C10 C11 179.4(9) . . . . ? C13 C14 C15 O8 144.6(7) . . . . ? C13 C14 C15 C16 -98.2(8) . . . . ? C14 O9 C17 N5 -146.5(6) . . . . ? C14 O9 C17 C16 -21.9(9) . . . . ? C14 C15 C16 C17 -36.5(8) . . . . ? C15 C16 C17 O9 36.4(8) . . . . ? C15 C16 C17 N5 155.5(7) . . . . ? C17 O9 C14 C13 124.4(7) . . . . ? C17 O9 C14 C15 -1.7(8) . . . . ? C17 N5 C18 O10 -4.3(14) . . . . ? C17 N5 C18 N6 175.7(8) . . . . ? C17 N5 C21 C20 -176.3(9) . . . . ? C18 N5 C17 O9 -108.5(9) . . . . ? C18 N5 C17 C16 133.7(8) . . . . ? C18 N5 C21 C20 -0.5(14) . . . . ? C18 N6 C19 O11 -177.6(10) . . . . ? C18 N6 C19 C20 1.9(14) . . . . ? C19 N6 C18 O10 179.3(10) . . . . ? C19 N6 C18 N5 -0.7(14) . . . . ? C19 C20 C21 N5 1.9(15) . . . . ? C21 N5 C17 O9 67.3(10) . . . . ? C21 N5 C17 C16 -50.4(11) . . . . ? C21 N5 C18 O10 179.9(9) . . . . ? C21 N5 C18 N6 -0.1(13) . . . . ? C22 C23 C24 O15 148.7(7) . . . . ? C22 C23 C24 C25 -93.7(9) . . . . ? C23 O16 C26 N7 -137.5(7) . . . . ? C23 O16 C26 C25 -14.0(9) . . . . ? C23 C24 C25 C26 -36.2(9) . . . . ? C24 C25 C26 O16 31.6(9) . . . . ? C24 C25 C26 N7 150.4(7) . . . . ? C26 O16 C23 C22 115.9(8) . . . . ? C26 O16 C23 C24 -9.4(9) . . . . ? C26 N7 C27 C28 -175.6(9) . . . . ? C26 N7 C30 O17 -6.7(15) . . . . ? C26 N7 C30 N8 175.4(8) . . . . ? C27 N7 C26 O16 39.5(11) . . . . ? C27 N7 C26 C25 -78.6(11) . . . . ? C27 N7 C30 O17 177.0(10) . . . . ? C27 N7 C30 N8 -0.9(14) . . . . ? C27 C28 C29 O18 176.3(10) . . . . ? C27 C28 C29 N8 -3.6(14) . . . . ? C29 N8 C30 O17 -179.3(10) . . . . ? C29 N8 C30 N7 -1.4(15) . . . . ? C30 N7 C26 O16 -136.8(9) . . . . ? C30 N7 C26 C25 105.2(10) . . . . ? C30 N7 C27 C28 0.6(15) . . . . ? C30 N8 C29 O18 -176.3(10) . . . . ? C30 N8 C29 C28 3.6(15) . . . . ? C31 N9 C33 O32 172.0(14) . . . . ? C32 N9 C33 O32 5(2) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.97(2) 2 0.03(2)