#------------------------------------------------------------------------------ #$Date: 2024-02-04 13:41:47 +0200 (Sun, 04 Feb 2024) $ #$Revision: 289457 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247824.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_7247824 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 O20 P2, Co H12 O6, H2 O' _chemical_formula_sum 'C30 H50 Co2 N8 O27 P2' _chemical_formula_weight 1134.58 _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 115.138(4) _cell_angle_beta 93.184(4) _cell_angle_gamma 96.631(5) _cell_formula_units_Z 1 _cell_length_a 6.9314(10) _cell_length_b 13.624(2) _cell_length_c 15.739(2) _cell_measurement_reflns_used 3160 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 28.50 _cell_measurement_theta_min 2.63 _cell_volume 1327.4(3) _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_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.1724 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9661 _diffrn_reflns_point_group_measured_fraction_full 0.912 _diffrn_reflns_point_group_measured_fraction_max 0.912 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.671 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 35.0 _diffrn_source_power 1.575 _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.4982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0971 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.6681. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour pink _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.419 _exptl_crystal_description block _exptl_crystal_F_000 586 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.946 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.130 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.11(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 584 _refine_ls_number_reflns 8522 _refine_ls_number_restraints 466 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.1442 _refine_ls_R_factor_gt 0.0821 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1723 _refine_ls_wR_factor_ref 0.2002 _reflns_Friedel_coverage 0.879 _reflns_Friedel_fraction_full 0.853 _reflns_Friedel_fraction_max 0.853 _reflns_number_gt 5080 _reflns_number_total 8522 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01056b2.cif _cod_data_source_block 1_a_CCDC2 _cod_depositor_comments 'Adding full bibliography for 7247822--7247826.cif.' _cod_original_cell_volume 1327.5(3) _cod_database_code 7247824 _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 0.941 _shelx_estimated_absorpt_t_min 0.920 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.89(5) 0.11(5) 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 O(H) groups, All O(H,H) groups, All O(H,H,H,H) groups 3. Restrained distances H4b-O4 0.85 with sigma of 0.02 O2-H2b 0.85 with sigma of 0.02 H24b-O24 0.85 with sigma of 0.02 O24-H24a 0.85 with sigma of 0.02 O27-H27a 0.85 with sigma of 0.02 O27-H27b 0.85 with sigma of 0.02 O19-C25 1.4 with sigma of 0.02 H2b-H4b_$4 2.12 with sigma of 0.02 H2a-O13_$4 1.9 with sigma of 0.02 O13-H4b 2.08 with sigma of 0.02 O5_$1-H4a 2.07 with sigma of 0.02 O5-H2b 1.9 with sigma of 0.02 H4b-O13 1.9 with sigma of 0.02 H4a-O5_$1 1.9 with sigma of 0.02 O1-H27a 1.85 with sigma of 0.02 H9-H19_$7 2.12 with sigma of 0.02 4. Uiso/Uaniso restraints and constraints O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim O27: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A Uanis(C12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(Co2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(O2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5. Others Fixed X: Co2(0.08473) Fixed Y: Co2(-0.02316) Fixed Z: Co1(0.65621) 6.a Free rotating group: O27(H24a,H24b,H27a,H27b) 6.b Rotating group: O2(H2a,H2b), O4(H4a,H4b), O21(H21a,H21b), O22(H22c,H22d), O23(H23a,H23b), O25(H25a,H25b), O26(H26a,H26b) 6.c Ternary CH refined with riding coordinates: C14(H14), C15(H15), C16(H16), C17(H17), C23(H23), C24(H24), C25(H25), C26(H26) 6.d Secondary CH2 refined with riding coordinates: C13(H13a,H13b), C22(H22a,H22b) 6.e Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C5(H5), C1(H1), C6(H6), C7(H7), C8(H8), C12(H12), C11(H11), C9(H9a), N6(H6a), C19(H19a), C18(H18), C28(H28), C27(H27), N8(H8a) 6.f Fitted hexagon refined as free rotating group: C2(C3,C4,C5,N1,C1), C8(N4,C12,C11,C10,C9), N6(C20,C19,C18,N5,C21), C28(C27,N7, C30,N8,C29) 6.g Tetrahedral OH refined with riding coordinates: O19(H19), O20(H20) 6.h Idealised tetrahedral OH refined as rotating group: O9(H9), O10(H10) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 1_a.res in P1 1_a.res created by SHELXL-2018/3 at 11:42:42 on 27-Jun-2023 REM Old TITL 1 in P2 REM SHELXT solution in P2 REM R1 0.200, Rweak 0.154, Alpha 0.000, Orientation as input REM Flack x = 0.163 ( 0.017 ) from Parsons' quotients REM Formula found by SHELXT: C25 N16 O27 P1 Co2 CELL 0.71073 6.9314 13.6243 15.7393 115.138 93.184 96.631 ZERR 1 0.001 0.002 0.0024 0.004 0.004 0.005 LATT -1 SFAC C H Co N O P UNIT 30 50 2 8 27 2 EQIV $1 -1+X,+Y,+Z EQIV $2 1+X,+Y,-1+Z EQIV $3 -1+X,+Y,1+Z EQIV $4 1+X,+Y,+Z EQIV $5 +X,-1+Y,+Z EQIV $6 -1+X,-1+Y,+Z EQIV $7 1+X,-1+Y,-1+Z ISOR 0.001 0.002 C12 C12 N3 Co2 ISOR 0.01 0.02 C1 C3 N3 C19 N1 N5 C27 C26 O3 O1 C17 C21 O13 C23 ISOR 0.005 0.01 C3 C1 N7 C5 O20 O11 O18 ISOR 0.005 0.01 O2 N2 C30 O19 SIMU 0.01 0.02 3.8 O1 > O20 O21 > O27 DFIX 0.85 H4b O4 DFIX 0.85 O2 H2b DFIX 0.85 H24b O24 DFIX 0.85 O24 H24a DFIX 0.85 O27 H27a DFIX 0.85 O27 H27b DFIX 1.4 O19 C25 DFIX 2.12 H2b H4b_$4 DFIX 1.9 H2a O13_$4 DFIX 2.08 O13 H4b DFIX 2.07 O5_$1 H4a DFIX 1.9 O5 H2b DFIX 1.9 H4b O13 DFIX 1.9 H4a O5_$1 DFIX 1.85 O1 H27a DFIX 2.12 H9 H19_$7 ISOR 0.005 0.01 C14 L.S. 10 PLAN 25 SIZE 0.11 0.11 0.08 TEMP 23 CONF HTAB O2 O5 HTAB O4 O5_$1 HTAB O4 O13 HTAB N6 O18_$2 HTAB N8 O11_$3 HTAB O22 O14_$5 HTAB O23 O12_$6 HTAB O23 O14_$5 HTAB O25 O6 HTAB O26 O6_$1 HTAB O26 O17 HTAB O27 O24 BOND $H LIST 4 MORE -1 ABIN fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT -2 50 REM REM REM WGHT 0.081600 BASF 0.11039 FVAR 0.58574 CO1 3 0.477685 0.468449 10.656210 11.00000 0.02449 0.02168 = 0.01759 0.01140 0.00280 0.00094 P1 6 0.681750 0.237131 0.578745 11.00000 0.01509 0.02445 = 0.02271 0.01390 0.00433 0.00342 P2 6 0.276992 0.699490 0.747530 11.00000 0.03489 0.02195 = 0.01938 0.01438 0.00652 0.00567 O1 5 0.518311 0.303531 0.586896 11.00000 0.02242 0.02097 = 0.01737 0.01298 0.00360 0.01306 O2 5 0.777769 0.510148 0.708215 11.00000 0.02736 0.02918 = 0.02939 0.01385 0.00104 0.00457 AFIX 7 H2A 2 0.845150 0.559095 0.706119 11.00000 -1.50000 H2B 2 0.837709 0.450788 0.698784 11.00000 -1.50000 AFIX 0 O3 5 0.442355 0.631732 0.727649 11.00000 0.04601 0.02384 = 0.02733 0.01717 0.00543 0.00649 O4 5 0.175142 0.427903 0.607897 11.00000 0.03605 0.02411 = 0.03912 0.01277 0.00361 0.00154 AFIX 7 H4A 2 0.123296 0.368241 0.612445 11.00000 -1.50000 H4B 2 0.108371 0.478017 0.644545 11.00000 -1.50000 AFIX 0 O5 5 0.866266 0.303292 0.632347 11.00000 0.01002 0.03713 = 0.03257 0.02070 0.00492 0.00798 O6 5 0.626063 0.137898 0.597105 11.00000 0.02136 0.02918 = 0.04101 0.02598 0.01451 0.00488 O7 5 0.734262 0.194149 0.472042 11.00000 0.03518 0.03142 = 0.02643 0.01385 0.00586 -0.00302 O8 5 0.689217 0.188564 0.285824 11.00000 0.04340 0.03784 = 0.03742 0.02402 0.00631 0.00725 O9 5 0.891556 -0.029551 0.205753 11.00000 0.09151 0.03515 = 0.04264 -0.00410 0.00290 0.02075 AFIX 147 H9 2 0.894216 -0.088137 0.208536 11.00000 -1.50000 AFIX 0 O10 5 1.184063 0.134601 0.270915 11.00000 0.06255 0.08049 = 0.06258 0.03571 0.02107 0.02286 AFIX 147 H10 2 1.167860 0.076311 0.223062 11.00000 -1.50000 AFIX 0 O11 5 0.934194 0.324738 0.158014 11.00000 0.08339 0.04775 = 0.02820 0.02522 0.01235 0.00367 O12 5 1.051275 0.656828 0.408858 11.00000 0.07375 0.05199 = 0.02807 0.01766 0.00314 0.00708 O13 5 0.083775 0.633537 0.683734 11.00000 0.04095 0.03794 = 0.03906 0.02561 -0.00272 0.00475 O14 5 0.329552 0.808880 0.742173 11.00000 0.05615 0.02870 = 0.02489 0.02310 0.00104 0.00431 O15 5 0.244488 0.726715 0.854456 11.00000 0.08376 0.03257 = 0.02504 0.02124 0.01610 0.01837 O16 5 0.012255 0.753902 1.006604 11.00000 0.10526 0.05088 = 0.04339 0.03497 0.02188 0.03126 O17 5 -0.081991 0.256132 0.892618 11.00000 0.05665 0.02523 = 0.05184 0.00417 -0.00305 -0.01398 O18 5 0.012020 0.580693 1.162365 11.00000 0.10008 0.04434 = 0.03131 0.03016 0.00392 0.00470 O19 5 0.264713 0.842945 1.208845 11.00000 0.12820 0.07855 = 0.05148 0.02879 0.01006 0.00796 AFIX 83 H19 2 0.186505 0.881087 1.203012 11.00000 -1.50000 AFIX 0 O20 5 0.521187 0.866301 1.085292 11.00000 0.12815 0.10319 = 0.07439 0.04349 0.00205 -0.01342 AFIX 83 H20 2 0.614752 0.838937 1.060477 11.00000 -1.50000 AFIX 0 N2 4 0.470870 0.444820 0.189790 11.00000 0.05952 0.05311 = 0.03760 0.03031 0.00331 -0.00321 N3 4 0.478340 0.476646 0.114228 11.00000 0.04337 0.04290 = 0.04201 0.01908 0.00500 0.00615 AFIX 66 C2 1 0.468349 0.409569 0.354909 11.00000 0.03345 0.03592 = 0.02673 0.01327 0.00219 0.00311 AFIX 43 H2 2 0.445178 0.347973 0.296922 11.00000 -1.20000 AFIX 65 C3 1 0.501823 0.513784 0.358229 11.00000 0.01333 0.02247 = 0.02081 0.01053 0.00399 -0.00012 C4 1 0.536454 0.605847 0.444897 11.00000 0.07433 0.01473 = 0.00967 0.00231 0.01194 -0.00076 AFIX 43 H4 2 0.558850 0.675574 0.447118 11.00000 -1.20000 AFIX 65 C5 1 0.537611 0.593697 0.528246 11.00000 0.02899 0.03248 = 0.02465 0.00964 0.00936 -0.00787 AFIX 43 H5 2 0.560781 0.655294 0.586233 11.00000 -1.20000 AFIX 65 N1 4 0.504137 0.489482 0.524928 11.00000 0.04506 0.02968 = 0.01957 0.02020 0.01191 0.02385 C1 1 0.469506 0.397418 0.438260 11.00000 0.03094 0.03055 = 0.02430 0.01703 0.00322 0.00057 AFIX 43 H1 2 0.447109 0.327692 0.436040 11.00000 -1.20000 AFIX 0 C6 1 0.501406 0.529018 0.269646 11.00000 0.04529 0.05439 = 0.02237 0.02695 0.00399 -0.00173 AFIX 43 H6 2 0.523170 0.599127 0.272652 11.00000 -1.20000 AFIX 0 C7 1 0.455190 0.397709 0.034662 11.00000 0.07357 0.03210 = 0.04108 0.02798 0.01168 0.01099 AFIX 43 H7 2 0.435221 0.326471 0.029160 11.00000 -1.20000 AFIX 66 C8 1 0.388529 0.341076 -0.221502 11.00000 0.08730 0.02678 = 0.02300 0.01593 0.00824 0.00208 AFIX 43 H8 2 0.344726 0.281490 -0.279367 11.00000 -1.20000 AFIX 65 N4 4 0.448818 0.443945 -0.217637 11.00000 0.02491 0.02849 = 0.01845 0.00750 -0.00640 -0.00241 C12 1 0.514286 0.533003 -0.131150 11.00000 0.02372 0.02365 = 0.02281 0.00998 0.00305 0.00392 AFIX 43 H12 2 0.554623 0.601829 -0.128565 11.00000 -1.20000 AFIX 65 C11 1 0.519465 0.519192 -0.048527 11.00000 0.02675 0.03830 = 0.02558 0.01936 0.01074 0.00452 AFIX 43 H11 2 0.563267 0.578778 0.009338 11.00000 -1.20000 AFIX 65 C10 1 0.459176 0.416323 -0.052390 11.00000 0.04370 0.08172 = 0.02947 0.03928 0.01739 0.02210 C9 1 0.393708 0.327265 -0.138876 11.00000 0.08505 0.04836 = 0.04725 0.03532 0.02459 0.00691 AFIX 43 H9A 2 0.353371 0.258438 -0.141461 11.00000 -1.20000 AFIX 0 C13 1 0.590780 0.114061 0.394960 11.00000 0.05646 0.01791 = 0.01771 0.00652 0.00778 0.00238 AFIX 23 H13A 2 0.470312 0.143884 0.394908 11.00000 -1.20000 H13B 2 0.561875 0.047748 0.403624 11.00000 -1.20000 AFIX 0 C14 1 0.673438 0.087501 0.301590 11.00000 0.04033 0.03922 = 0.02561 0.01807 -0.00136 0.00337 AFIX 13 H14 2 0.580369 0.029950 0.251019 11.00000 -1.20000 AFIX 0 C15 1 0.866739 0.051234 0.294980 11.00000 0.06128 0.02499 = 0.02027 0.00130 0.01144 0.02644 AFIX 13 H15 2 0.896672 0.027489 0.344270 11.00000 -1.20000 AFIX 0 C16 1 1.012293 0.151238 0.308332 11.00000 0.03861 0.06096 = 0.05875 0.04367 0.00762 0.02238 AFIX 13 H16 2 1.042844 0.197799 0.376359 11.00000 -1.20000 AFIX 0 C17 1 0.880921 0.209250 0.266819 11.00000 0.03946 0.02115 = 0.02792 0.00826 -0.00400 0.00222 AFIX 13 H17 2 0.883647 0.178142 0.198244 11.00000 -1.20000 AFIX 66 N6 4 0.994698 0.492283 0.285314 11.00000 0.03793 0.02610 = 0.02514 0.02143 0.00438 -0.00081 AFIX 43 H6A 2 1.010365 0.524261 0.248843 11.00000 -1.20000 AFIX 65 C20 1 1.011248 0.554344 0.382634 11.00000 0.08986 0.02074 = 0.01317 0.00372 0.00264 0.00370 C19 1 0.985925 0.502658 0.441581 11.00000 0.04632 0.02173 = 0.01731 0.01213 0.00711 -0.00360 AFIX 43 H19A 2 0.996999 0.544181 0.506695 11.00000 -1.20000 AFIX 65 C18 1 0.944052 0.388911 0.403208 11.00000 0.02517 0.04749 = 0.03549 0.02655 -0.00904 -0.00392 AFIX 43 H18 2 0.927109 0.354330 0.442648 11.00000 -1.20000 AFIX 65 N5 4 0.927501 0.326849 0.305888 11.00000 0.03755 0.04433 = 0.01747 0.01326 0.01179 0.00981 C21 1 0.952823 0.378534 0.246940 11.00000 0.03651 0.03497 = 0.02633 0.01528 0.00318 0.00418 AFIX 0 C22 1 0.201261 0.830118 0.918597 11.00000 0.06544 0.03823 = 0.02802 0.01517 0.02791 0.02480 AFIX 23 H22A 2 0.078814 0.844110 0.896305 11.00000 -1.20000 H22B 2 0.304284 0.888492 0.925517 11.00000 -1.20000 AFIX 0 C23 1 0.186519 0.823707 1.011584 11.00000 0.08574 0.04859 = 0.03754 0.01735 0.02015 0.00978 AFIX 13 H23 2 0.175767 0.897588 1.058943 11.00000 -1.20000 AFIX 0 C24 1 0.350168 0.787105 1.048640 11.00000 0.11436 0.05655 = 0.01074 0.00478 -0.00201 -0.00792 AFIX 13 H24 2 0.383374 0.722221 0.996440 11.00000 -1.20000 AFIX 0 C25 1 0.270066 0.751667 1.118708 11.00000 0.13810 0.05575 = 0.01993 0.01336 0.02343 0.02003 AFIX 13 H25 2 0.335216 0.694238 1.124368 11.00000 -1.20000 AFIX 0 C26 1 0.053717 0.709439 1.073476 11.00000 0.09836 0.06794 = 0.05351 0.04440 0.01363 0.02525 AFIX 13 H26 2 -0.034048 0.732344 1.122790 11.00000 -1.20000 AFIX 66 C28 1 -0.041376 0.417125 0.874709 11.00000 0.01960 0.08918 = 0.03621 0.03874 0.01151 0.01969 AFIX 43 H28 2 -0.055019 0.380107 0.809116 11.00000 -1.20000 AFIX 65 C27 1 -0.006074 0.531141 0.918968 11.00000 0.04561 0.03990 = 0.02755 0.02181 0.00746 0.01378 AFIX 43 H27 2 0.003903 0.570408 0.882987 11.00000 -1.20000 AFIX 65 N7 4 0.014317 0.586470 1.017005 11.00000 0.04872 0.04224 = 0.03334 0.02589 0.00683 0.00215 C30 1 -0.000595 0.527782 1.070783 11.00000 0.05249 0.04535 = 0.03549 0.02590 0.00967 0.00968 N8 4 -0.035897 0.413766 1.026525 11.00000 0.06786 0.04518 = 0.01599 0.00669 0.00737 0.01125 AFIX 43 H8A 2 -0.045122 0.377456 1.059798 11.00000 -1.20000 AFIX 65 C29 1 -0.056288 0.358436 0.928489 11.00000 0.00712 0.05037 = 0.03917 0.02502 0.00101 0.00255 AFIX 0 CO2 3 10.084729 9.976839 0.647578 11.00000 0.03689 0.03125 = 0.02994 0.01818 0.00350 0.00315 O21 5 -0.173180 -0.134682 0.603722 11.00000 0.05833 0.04679 = 0.05384 0.02655 -0.00613 -0.00698 AFIX 7 H21A 2 -0.216170 -0.181314 0.628723 11.00000 -1.50000 H21B 2 -0.270060 -0.148156 0.556820 11.00000 -1.50000 AFIX 0 O22 5 0.106309 -0.031151 0.777750 11.00000 0.05596 0.03391 = 0.03973 0.02017 0.00537 0.01143 AFIX 7 H22C 2 0.172951 0.030701 0.822833 11.00000 -1.50000 H22D 2 0.179224 -0.080456 0.779380 11.00000 -1.50000 AFIX 0 O23 5 0.225771 -0.166335 0.587065 11.00000 0.07146 0.02599 = 0.02805 0.01813 -0.01040 -0.00029 AFIX 7 H23A 2 0.287749 -0.177191 0.631593 11.00000 -1.50000 H23B 2 0.139235 -0.225979 0.558553 11.00000 -1.50000 AFIX 0 O24 5 0.063336 -0.018887 0.518486 11.00000 0.08105 0.03608 = 0.03151 0.01978 0.00196 0.00091 O25 5 0.355571 0.075808 0.692268 11.00000 0.04989 0.02914 = 0.03792 0.01645 0.00495 -0.01031 AFIX 7 H25A 2 0.423543 0.066122 0.644451 11.00000 -1.50000 H25B 2 0.429614 0.056450 0.728129 11.00000 -1.50000 AFIX 0 O26 5 -0.061757 0.112261 0.701371 11.00000 0.06389 0.04338 = 0.04311 0.01935 -0.00916 0.01508 AFIX 7 H26A 2 -0.063957 0.138046 0.764339 11.00000 -1.50000 H26B 2 -0.191320 0.095926 0.680933 11.00000 -1.50000 AFIX 6 O27 5 0.161255 0.176101 0.523729 11.00000 0.05084 0.02269 = 0.04373 0.01358 -0.00423 -0.00081 H24A 2 -0.050480 -0.049588 0.488150 11.00000 -1.50000 H24B 2 0.118207 -0.064855 0.474174 11.00000 -1.50000 H27A 2 0.270834 0.228180 0.575340 11.00000 -1.50000 H27B 2 0.134163 0.108096 0.509800 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1_a.res in P1 REM wR2 = 0.2002, GooF = S = 1.019, Restrained GooF = 1.030 for all data REM R1 = 0.0821 for 5080 Fo > 4sig(Fo) and 0.1442 for all 8522 data REM 584 parameters refined using 466 restraints END WGHT 0.0816 0.0000 REM Highest difference peak 0.946, deepest hole -0.905, 1-sigma level 0.130 Q1 1 0.3251 0.4587 0.6448 11.00000 0.05 0.95 Q2 1 0.6288 0.4760 0.6727 11.00000 0.05 0.91 Q3 1 0.2635 -0.0716 0.4411 11.00000 0.05 0.71 Q4 1 0.6009 0.3969 0.6711 11.00000 0.05 0.70 Q5 1 0.4482 0.3667 0.5817 11.00000 0.05 0.67 Q6 1 0.6881 0.3175 0.6291 11.00000 0.05 0.67 Q7 1 0.2263 -0.0166 0.6376 11.00000 0.05 0.66 Q8 1 0.3007 0.6175 0.6924 11.00000 0.05 0.66 Q9 1 0.1813 0.7799 0.7278 11.00000 0.05 0.65 Q10 1 -0.1676 0.6411 1.1576 11.00000 0.05 0.64 Q11 1 0.7797 0.1435 0.5721 11.00000 0.05 0.62 Q12 1 0.0909 -0.1135 0.5812 11.00000 0.05 0.61 Q13 1 -0.0618 -0.0218 0.6582 11.00000 0.05 0.58 Q14 1 0.3424 0.5396 0.6520 11.00000 0.05 0.57 Q15 1 0.1277 -0.1692 0.4062 11.00000 0.05 0.51 Q16 1 0.3549 0.8615 1.2131 11.00000 0.05 0.50 Q17 1 0.5229 0.1584 0.6211 11.00000 0.05 0.50 Q18 1 0.0871 0.8387 1.2108 11.00000 0.05 0.50 Q19 1 0.2879 -0.2604 0.5573 11.00000 0.05 0.49 Q20 1 0.4774 0.5628 0.7249 11.00000 0.05 0.49 Q21 1 0.9763 0.3003 0.5925 11.00000 0.05 0.48 Q22 1 0.4512 0.4808 -0.2471 11.00000 0.05 0.48 Q23 1 -0.0569 0.4560 1.0328 11.00000 0.05 0.47 Q24 1 0.2287 0.8000 0.8171 11.00000 0.05 0.47 Q25 1 0.0443 -0.2025 0.7238 11.00000 0.05 0.46 ; _shelx_res_checksum 22416 _shelx_fab_file ; -9 -2 1 17.5284 -10.5036 -9 -2 2 27.8189 -19.3874 -9 -2 3 10.9323 18.1850 -9 -2 4 -4.7280 -16.8510 -9 -2 5 42.0574 -14.2768 -9 -1 1 23.6997 18.6459 -9 -1 2 12.9247 -13.3056 -9 -1 3 52.7007 28.1551 -9 -1 4 -9.3708 26.4815 -9 -1 5 16.2509 -36.5418 -9 -1 6 29.4706 14.1636 -9 0 1 32.5253 39.2162 -9 0 2 -21.2083 23.3718 -9 0 3 47.2298 -14.6978 -9 0 4 26.2840 44.7566 -9 0 5 -16.1728 -6.9372 -9 0 6 32.2099 -3.2192 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5 6 -0.2240 1.6431 7 6 0 9.1564 -6.1732 7 6 1 -7.5119 -11.2513 7 6 2 -0.7226 -15.9229 7 6 3 0.4109 -4.9786 7 6 4 1.2002 -1.3697 7 6 5 0.6041 0.6769 7 7 0 8.4378 -12.1413 7 7 1 4.0160 -1.5698 7 7 2 1.9689 -7.2886 7 7 3 3.5207 -2.5895 7 8 0 1.4035 -7.5692 7 8 1 9.4794 0.5370 8 -11 2 -0.1677 3.0039 8 -11 3 0.4761 -2.3708 8 -11 4 2.1631 -0.6643 8 -11 5 0.3347 -0.9345 8 -10 0 -3.3545 2.9861 8 -10 1 -0.2851 -1.0642 8 -10 2 2.1474 3.8814 8 -10 3 -1.1411 0.9253 8 -10 4 1.2499 -0.1785 8 -10 5 -0.1094 -0.1038 8 -10 6 0.9387 0.6720 8 -10 7 -0.3528 -1.3612 8 -9 0 -3.3256 3.5223 8 -9 1 -6.1035 -0.5747 8 -9 2 0.2384 -0.3960 8 -9 3 0.5105 1.4044 8 -9 4 -0.1782 -0.5939 8 -9 5 -0.4733 -0.0082 8 -9 6 -0.0605 2.1107 8 -9 7 -0.4854 -1.4626 8 -9 8 3.7533 1.0586 8 -8 0 -5.7483 -2.1511 8 -8 1 -6.5559 -0.6573 8 -8 2 -2.9238 -3.5056 8 -8 3 1.6836 -2.4706 8 -8 4 -2.6135 -0.7647 8 -8 5 -0.8822 -0.9760 8 -8 6 0.5888 5.8454 8 -8 7 -3.8384 0.7796 8 -8 8 3.0418 -0.6639 8 -8 9 -3.4126 -2.5623 8 -7 0 -5.4570 -2.4200 8 -7 1 -1.4751 -0.7773 8 -7 2 -3.5007 -1.1486 8 -7 3 0.1049 -3.2465 8 -7 4 -5.7393 2.4582 8 -7 5 -6.7221 -4.8494 8 -7 6 1.3379 3.6232 8 -7 7 -6.4567 3.1198 8 -7 8 2.7171 -4.5050 8 -7 9 -2.8003 -3.8474 8 -6 0 -2.1252 3.2680 8 -6 1 -2.0065 1.9413 8 -6 2 -6.7233 1.6916 8 -6 3 -0.2974 -7.7153 8 -6 4 -1.3644 1.9860 8 -6 5 -14.9272 -5.7562 8 -6 6 -0.8557 -3.7755 8 -6 7 -3.8801 4.0357 8 -6 8 1.2286 -6.9888 8 -6 9 -1.2939 -2.7584 8 -5 0 -8.2040 3.3026 8 -5 1 -4.0105 2.4253 8 -5 2 -7.4635 3.8004 8 -5 3 -3.2270 -17.8082 8 -5 4 6.9238 -7.8506 8 -5 5 -12.8959 0.3376 8 -5 6 -4.8179 -6.4759 8 -5 7 0.2066 2.1740 8 -5 8 -1.9178 -3.3482 8 -5 9 -2.0363 -1.0480 8 -4 0 -17.2602 -1.2805 8 -4 1 3.8160 -9.0021 8 -4 2 6.1987 6.2715 8 -4 3 -9.1300 -12.0485 8 -4 4 5.4013 -12.9931 8 -4 5 -2.7225 2.9253 8 -4 6 -6.8447 -3.2960 8 -4 7 -1.2626 -1.8613 8 -4 8 -0.8827 -0.0366 8 -4 9 -2.7925 -0.2062 8 -3 0 -10.3642 2.7945 8 -3 1 4.0428 -21.5160 8 -3 2 20.0046 4.6469 8 -3 3 -6.2553 6.6483 8 -3 4 0.6583 -7.5424 8 -3 5 1.2216 -3.2228 8 -3 6 -3.6672 -0.9381 8 -3 7 -4.4179 -2.0347 8 -3 8 1.7893 -3.5937 8 -3 9 -1.9224 -0.0497 8 -2 0 10.0659 14.6143 8 -2 1 -13.8665 -10.3239 8 -2 2 18.0691 -0.8055 8 -2 3 3.7017 9.2306 8 -2 4 3.0425 -7.4073 8 -2 5 -0.9811 -5.8243 8 -2 6 1.9261 -1.8161 8 -2 7 -1.6708 1.0070 8 -2 8 -0.5406 -6.8949 8 -1 0 24.5017 13.0994 8 -1 1 -18.6127 14.6938 8 -1 2 15.9239 -8.8803 8 -1 3 10.5917 0.6723 8 -1 4 2.5399 -9.7780 8 -1 5 -0.6012 -0.0902 8 -1 6 2.4221 -3.0393 8 -1 7 1.6343 -0.0114 8 -1 8 -3.6582 -4.3040 8 0 0 23.6215 -3.9969 8 0 1 2.6257 25.7108 8 0 2 14.4369 -16.3170 8 0 3 14.2918 -0.1519 8 0 4 -2.4830 0.1777 8 0 5 -0.0829 3.1642 8 0 6 -1.3170 -3.1083 8 0 7 -0.0684 -2.7014 8 1 0 12.3508 -15.0244 8 1 1 22.7258 23.8303 8 1 2 -2.0962 -5.2403 8 1 3 7.3135 0.2717 8 1 4 -1.5468 8.4211 8 1 5 -2.4520 1.3067 8 1 6 -1.9962 -2.9704 8 2 0 -8.5021 -9.9202 8 2 1 19.7299 12.1510 8 2 2 -14.3858 16.6770 8 2 3 -11.5221 1.3133 8 2 4 0.2617 2.0165 8 2 5 -1.6481 1.3263 8 2 6 -0.0832 -2.2526 8 3 0 -26.4921 3.7133 8 3 1 -6.5297 -7.4990 8 3 2 -10.0065 12.5276 8 3 3 -18.1119 8.6582 8 3 4 -3.3548 -3.0683 8 4 0 -19.3657 4.4275 8 4 1 -28.6166 -13.6492 8 4 2 -11.2832 -8.4355 8 4 3 -5.7033 9.9340 8 5 0 -3.3680 -14.0162 8 5 1 -20.6407 -5.2745 8 5 2 -16.4656 -9.1441 8 6 0 -3.3460 -20.8086 9 -6 0 2.6002 -2.3212 9 -6 1 4.1464 0.3417 9 -6 2 1.3415 2.3040 9 -6 3 -4.7286 -0.3151 9 -5 0 5.3705 4.3860 9 -5 1 2.1075 -2.6751 9 -5 2 14.6744 -3.2711 9 -5 3 -2.0123 9.3534 9 -5 4 -9.0026 -5.7825 9 -4 0 25.3149 7.2209 9 -4 1 -0.5866 14.5125 9 -4 2 4.9513 -15.2989 9 -4 3 10.9776 12.7265 9 -4 4 -12.9047 8.0060 9 -3 0 19.2597 -12.0919 9 -3 1 8.6323 27.0224 9 -3 2 -24.3305 -5.2995 9 -3 3 10.8553 -4.3380 9 -3 4 -2.2404 11.8767 9 -2 0 -22.2640 -25.1909 9 -2 1 17.9623 -0.4073 9 -2 2 -20.9508 11.1956 9 -2 3 -4.7806 -15.4437 9 -1 0 -29.1692 -10.7115 9 -1 1 12.8337 -33.7572 9 -1 2 5.8591 -0.0520 9 -1 3 -8.9393 -8.9722 9 0 0 14.6172 1.4896 9 0 1 8.6743 -28.4484 9 0 2 8.9422 -12.2871 9 1 0 35.6264 -1.4789 9 1 1 10.5204 -8.4213 0 0 0 0.0 0.0 ; _shelx_fab_checksum 71964 _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 0.4777(4) 0.4684(2) 0.656210 0.0205(5) Uani 1 1 d . . . . . P1 P 0.6817(7) 0.2371(4) 0.5787(3) 0.0193(10) Uani 1 1 d . . . . . P2 P 0.2770(7) 0.6995(4) 0.7475(3) 0.0232(11) Uani 1 1 d . . . . . O1 O 0.5183(15) 0.3035(9) 0.5869(7) 0.018(2) Uani 1 1 d D U . . . O2 O 0.7778(15) 0.5101(9) 0.7082(8) 0.028(3) Uani 1 1 d D U . . . H2A H 0.845150 0.559095 0.706119 0.042 Uiso 1 1 d DR U . . . H2B H 0.837709 0.450788 0.698784 0.042 Uiso 1 1 d DR U . . . O3 O 0.4424(18) 0.6317(9) 0.7276(8) 0.030(3) Uani 1 1 d . U . . . O4 O 0.1751(16) 0.4279(9) 0.6079(9) 0.034(3) Uani 1 1 d D U . . . H4A H 0.123296 0.368241 0.612445 0.051 Uiso 1 1 d DR U . . . H4B H 0.108371 0.478017 0.644545 0.051 Uiso 1 1 d DR U . . . O5 O 0.8663(14) 0.3033(9) 0.6323(8) 0.024(3) Uani 1 1 d D U . . . O6 O 0.6261(15) 0.1379(9) 0.5971(8) 0.026(3) Uani 1 1 d . U . . . O7 O 0.7343(17) 0.1941(9) 0.4720(8) 0.031(3) Uani 1 1 d . U . . . O8 O 0.6892(18) 0.1886(10) 0.2858(8) 0.037(3) Uani 1 1 d . U . . . O9 O 0.892(2) -0.0296(11) 0.2058(9) 0.063(4) Uani 1 1 d . U . . . H9 H 0.894216 -0.088137 0.208536 0.095 Uiso 1 1 calc DR U . . . O10 O 1.184(2) 0.1346(13) 0.2709(11) 0.065(4) Uani 1 1 d . U . . . H10 H 1.167860 0.076311 0.223062 0.098 Uiso 1 1 calc R U . . . O11 O 0.934(2) 0.3247(11) 0.1580(9) 0.050(4) Uani 1 1 d . U . . . O12 O 1.051(2) 0.6568(12) 0.4089(9) 0.052(4) Uani 1 1 d . . . . . O13 O 0.0838(17) 0.6335(10) 0.6837(9) 0.037(3) Uani 1 1 d D U . . . O14 O 0.3296(18) 0.8089(9) 0.7422(8) 0.033(3) Uani 1 1 d . U . . . O15 O 0.244(2) 0.7267(10) 0.8545(8) 0.043(3) Uani 1 1 d . U . . . O16 O 0.012(2) 0.7539(12) 1.0066(10) 0.059(4) Uani 1 1 d . U . . . O17 O -0.082(2) 0.2561(11) 0.8926(10) 0.051(4) Uani 1 1 d . U . . . O18 O 0.012(2) 0.5807(11) 1.1624(9) 0.054(4) Uani 1 1 d . U . . . O19 O 0.265(3) 0.8429(13) 1.2088(10) 0.087(5) Uani 1 1 d D U . . . H19 H 0.186505 0.881087 1.203012 0.130 Uiso 1 1 calc R U . . . O20 O 0.521(3) 0.8663(15) 1.0853(12) 0.103(5) Uani 1 1 d . U . . . H20 H 0.614752 0.838937 1.060477 0.155 Uiso 1 1 calc R U . . . N2 N 0.471(3) 0.4448(14) 0.1898(12) 0.047(5) Uani 1 1 d . U . . . N3 N 0.478(2) 0.4766(14) 0.1142(12) 0.043(4) Uani 1 1 d . U . . . C2 C 0.4683(17) 0.4096(7) 0.3549(6) 0.032(4) Uani 1 1 d G . . . . H2 H 0.445178 0.347973 0.296922 0.039 Uiso 1 1 calc R U . . . C3 C 0.5018(16) 0.5138(8) 0.3582(6) 0.019(4) Uani 1 1 d G U . . . C4 C 0.5365(17) 0.6058(7) 0.4449(7) 0.034(5) Uani 1 1 d G . . . . H4 H 0.558850 0.675574 0.447118 0.041 Uiso 1 1 calc R U . . . C5 C 0.5376(17) 0.5937(7) 0.5282(5) 0.031(4) Uani 1 1 d G U . . . H5 H 0.560781 0.655294 0.586233 0.037 Uiso 1 1 calc R U . . . N1 N 0.5041(15) 0.4895(8) 0.5249(6) 0.026(4) Uani 1 1 d G U . . . C1 C 0.4695(16) 0.3974(7) 0.4383(7) 0.027(4) Uani 1 1 d G U . . . H1 H 0.447109 0.327692 0.436040 0.033 Uiso 1 1 calc R U . . . C6 C 0.501(3) 0.5290(17) 0.2696(13) 0.038(5) Uani 1 1 d . . . . . H6 H 0.523170 0.599127 0.272652 0.045 Uiso 1 1 calc R U . . . C7 C 0.455(3) 0.3977(17) 0.0347(14) 0.044(6) Uani 1 1 d . . . . . H7 H 0.435221 0.326471 0.029160 0.053 Uiso 1 1 calc R U . . . C8 C 0.3885(18) 0.3411(7) -0.2215(7) 0.044(5) Uani 1 1 d G . . . . H8 H 0.344726 0.281490 -0.279367 0.053 Uiso 1 1 calc R U . . . N4 N 0.4488(15) 0.4439(8) -0.2176(6) 0.026(4) Uani 1 1 d G . . . . C12 C 0.5143(15) 0.5330(7) -0.1312(7) 0.023(4) Uani 1 1 d G U . . . H12 H 0.554623 0.601829 -0.128565 0.028 Uiso 1 1 calc R U . . . C11 C 0.5195(17) 0.5192(9) -0.0485(5) 0.028(4) Uani 1 1 d G . . . . H11 H 0.563267 0.578778 0.009338 0.034 Uiso 1 1 calc R U . . . C10 C 0.4592(18) 0.4163(11) -0.0524(7) 0.045(6) Uani 1 1 d G . . . . C9 C 0.394(2) 0.3273(8) -0.1389(9) 0.055(6) Uani 1 1 d G . . . . H9A H 0.353371 0.258438 -0.141461 0.066 Uiso 1 1 calc R U . . . C13 C 0.591(3) 0.1141(13) 0.3950(11) 0.031(4) Uani 1 1 d . . . . . H13A H 0.470312 0.143884 0.394908 0.038 Uiso 1 1 calc R U . . . H13B H 0.561875 0.047748 0.403624 0.038 Uiso 1 1 calc R U . . . C14 C 0.673(3) 0.0875(15) 0.3016(12) 0.034(4) Uani 1 1 d . U . . . H14 H 0.580369 0.029950 0.251019 0.041 Uiso 1 1 calc R U . . . C15 C 0.867(3) 0.0512(14) 0.2950(11) 0.037(5) Uani 1 1 d . . . . . H15 H 0.896672 0.027489 0.344270 0.044 Uiso 1 1 calc R U . . . C16 C 1.012(3) 0.1512(17) 0.3083(15) 0.045(5) Uani 1 1 d . . . . . H16 H 1.042844 0.197799 0.376359 0.054 Uiso 1 1 calc R U . . . C17 C 0.881(3) 0.2093(14) 0.2668(13) 0.031(4) Uani 1 1 d . U . . . H17 H 0.883647 0.178142 0.198244 0.037 Uiso 1 1 calc R U . . . N6 N 0.9947(16) 0.4923(8) 0.2853(6) 0.027(3) Uani 1 1 d G . . . . H6A H 1.010365 0.524261 0.248843 0.032 Uiso 1 1 calc R U . . . C20 C 1.0112(19) 0.5543(6) 0.3826(7) 0.043(6) Uani 1 1 d G . . . . C19 C 0.9859(19) 0.5027(8) 0.4416(5) 0.028(4) Uani 1 1 d G U . . . H19A H 0.996999 0.544181 0.506695 0.033 Uiso 1 1 calc R U . . . C18 C 0.9441(16) 0.3889(8) 0.4032(6) 0.034(5) Uani 1 1 d G . . . . H18 H 0.927109 0.354330 0.442648 0.041 Uiso 1 1 calc R U . . . N5 N 0.9275(16) 0.3268(6) 0.3059(7) 0.033(4) Uani 1 1 d G U . . . C21 C 0.9528(16) 0.3785(8) 0.2469(5) 0.032(4) Uani 1 1 d G U . . . C22 C 0.201(3) 0.8301(14) 0.9186(12) 0.041(5) Uani 1 1 d . . . . . H22A H 0.078814 0.844110 0.896305 0.049 Uiso 1 1 calc R U . . . H22B H 0.304284 0.888492 0.925517 0.049 Uiso 1 1 calc R U . . . C23 C 0.187(4) 0.8237(19) 1.0116(15) 0.057(6) Uani 1 1 d . U . . . H23 H 0.175767 0.897588 1.058943 0.069 Uiso 1 1 calc R U . . . C24 C 0.350(4) 0.7871(19) 1.0486(13) 0.066(8) Uani 1 1 d . . . . . H24 H 0.383374 0.722221 0.996440 0.079 Uiso 1 1 calc R U . . . C25 C 0.270(4) 0.7517(17) 1.1187(12) 0.071(8) Uani 1 1 d D . . . . H25 H 0.335216 0.694238 1.124368 0.086 Uiso 1 1 calc R U . . . C26 C 0.054(4) 0.7094(19) 1.0735(16) 0.066(7) Uani 1 1 d . U . . . H26 H -0.034048 0.732344 1.122790 0.079 Uiso 1 1 calc R U . . . C28 C -0.0414(18) 0.4171(9) 0.8747(5) 0.043(5) Uani 1 1 d G . . . . H28 H -0.055019 0.380107 0.809116 0.052 Uiso 1 1 calc R U . . . C27 C -0.0061(18) 0.5311(9) 0.9190(7) 0.034(5) Uani 1 1 d G U . . . H27 H 0.003903 0.570408 0.882987 0.041 Uiso 1 1 calc R U . . . N7 N 0.0143(17) 0.5865(7) 1.0170(7) 0.038(4) Uani 1 1 d G U . . . C30 C -0.0006(17) 0.5278(8) 1.0708(5) 0.041(5) Uani 1 1 d G U . . . N8 N -0.0359(17) 0.4138(8) 1.0265(7) 0.045(4) Uani 1 1 d G . . . . H8A H -0.045122 0.377456 1.059798 0.054 Uiso 1 1 calc R U . . . C29 C -0.0563(16) 0.3584(7) 0.9285(7) 0.030(5) Uani 1 1 d G . . . . Co2 Co 0.084729 -0.023161 0.6476(2) 0.0312(6) Uani 1 1 d . U . . . O21 O -0.173(2) -0.1347(11) 0.6037(9) 0.053(3) Uani 1 1 d . U . . . H21A H -0.216170 -0.181314 0.628723 0.080 Uiso 1 1 d R U . . . H21B H -0.270060 -0.148156 0.556820 0.080 Uiso 1 1 d R U . . . O22 O 0.1063(18) -0.0312(10) 0.7777(8) 0.041(3) Uani 1 1 d . U . . . H22C H 0.172951 0.030701 0.822833 0.062 Uiso 1 1 d R U . . . H22D H 0.179224 -0.080456 0.779380 0.062 Uiso 1 1 d R U . . . O23 O 0.2258(19) -0.1663(10) 0.5871(8) 0.041(3) Uani 1 1 d . U . . . H23A H 0.287749 -0.177191 0.631593 0.061 Uiso 1 1 d R U . . . H23B H 0.139235 -0.225979 0.558553 0.061 Uiso 1 1 d R U . . . O24 O 0.063(2) -0.0189(11) 0.5185(8) 0.049(3) Uani 1 1 d D U . . . O25 O 0.3556(18) 0.0758(9) 0.6923(9) 0.040(3) Uani 1 1 d . U . . . H25A H 0.423543 0.066122 0.644451 0.060 Uiso 1 1 d R U . . . H25B H 0.429614 0.056450 0.728129 0.060 Uiso 1 1 d R U . . . O26 O -0.0618(19) 0.1123(10) 0.7014(9) 0.050(3) Uani 1 1 d . U . . . H26A H -0.063957 0.138046 0.764339 0.075 Uiso 1 1 d R U . . . H26B H -0.191320 0.095926 0.680933 0.075 Uiso 1 1 d R U . . . O27 O 0.1613(18) 0.1761(9) 0.5237(8) 0.040(3) Uani 1 1 d DG U . . . H24A H -0.050480 -0.049588 0.488150 0.061 Uiso 1 1 d DG U . . . H24B H 0.118207 -0.064855 0.474174 0.061 Uiso 1 1 d DG U . . . H27A H 0.270834 0.228180 0.575340 0.061 Uiso 1 1 d DG U . . . H27B H 0.134163 0.108096 0.509800 0.061 Uiso 1 1 d DG 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 0.0245(11) 0.0217(11) 0.0176(11) 0.0114(9) 0.0028(9) 0.0009(9) P1 0.015(2) 0.024(3) 0.023(2) 0.014(2) 0.0043(19) 0.0034(19) P2 0.035(3) 0.022(3) 0.019(2) 0.014(2) 0.007(2) 0.006(2) O1 0.022(5) 0.021(5) 0.017(4) 0.013(4) 0.004(4) 0.013(4) O2 0.027(6) 0.029(6) 0.029(6) 0.014(5) 0.001(5) 0.005(5) O3 0.046(6) 0.024(5) 0.027(5) 0.017(4) 0.005(5) 0.006(5) O4 0.036(7) 0.024(6) 0.039(6) 0.013(5) 0.004(6) 0.002(5) O5 0.010(5) 0.037(7) 0.033(6) 0.021(5) 0.005(5) 0.008(5) O6 0.021(6) 0.029(6) 0.041(6) 0.026(5) 0.015(5) 0.005(5) O7 0.035(6) 0.031(6) 0.026(5) 0.014(5) 0.006(5) -0.003(5) O8 0.043(6) 0.038(6) 0.037(6) 0.024(5) 0.006(5) 0.007(5) O9 0.092(10) 0.035(8) 0.043(8) -0.004(6) 0.003(7) 0.021(7) O10 0.063(9) 0.080(11) 0.063(10) 0.036(8) 0.021(8) 0.023(8) O11 0.083(8) 0.048(7) 0.028(6) 0.025(6) 0.012(6) 0.004(6) O12 0.074(11) 0.052(10) 0.028(7) 0.018(7) 0.003(7) 0.007(8) O13 0.041(7) 0.038(7) 0.039(6) 0.026(5) -0.003(6) 0.005(6) O14 0.056(8) 0.029(6) 0.025(6) 0.023(5) 0.001(5) 0.004(6) O15 0.084(7) 0.033(6) 0.025(5) 0.021(5) 0.016(5) 0.018(5) O16 0.105(9) 0.051(7) 0.043(7) 0.035(6) 0.022(7) 0.031(7) O17 0.057(9) 0.025(8) 0.052(9) 0.004(7) -0.003(7) -0.014(7) O18 0.100(9) 0.044(7) 0.031(6) 0.030(6) 0.004(6) 0.005(7) O19 0.128(10) 0.079(8) 0.051(7) 0.029(6) 0.010(7) 0.008(8) O20 0.128(10) 0.103(9) 0.074(8) 0.043(7) 0.002(8) -0.013(8) N2 0.060(7) 0.053(7) 0.038(7) 0.030(6) 0.003(5) -0.003(5) N3 0.043(5) 0.043(4) 0.042(4) 0.019(2) 0.0050(15) 0.0062(16) C2 0.033(11) 0.036(12) 0.027(10) 0.013(9) 0.002(8) 0.003(9) C3 0.013(6) 0.022(6) 0.021(6) 0.011(5) 0.004(5) 0.000(5) C4 0.074(15) 0.015(10) 0.010(8) 0.002(7) 0.012(9) -0.001(9) C5 0.029(7) 0.032(7) 0.025(6) 0.010(5) 0.009(5) -0.008(5) N1 0.045(8) 0.030(8) 0.020(7) 0.020(6) 0.012(6) 0.024(7) C1 0.031(7) 0.031(7) 0.024(6) 0.017(5) 0.003(5) 0.001(5) C6 0.045(13) 0.054(14) 0.022(10) 0.027(10) 0.004(9) -0.002(11) C7 0.074(16) 0.032(12) 0.041(12) 0.028(11) 0.012(11) 0.011(11) C8 0.087(16) 0.027(11) 0.023(10) 0.016(8) 0.008(10) 0.002(10) N4 0.025(8) 0.028(9) 0.018(8) 0.007(7) -0.006(7) -0.002(7) C12 0.024(4) 0.024(4) 0.023(4) 0.010(2) 0.0030(15) 0.0039(15) C11 0.027(10) 0.038(12) 0.026(10) 0.019(9) 0.011(8) 0.005(9) C10 0.044(13) 0.082(17) 0.029(11) 0.039(11) 0.017(10) 0.022(12) C9 0.085(17) 0.048(14) 0.047(14) 0.035(12) 0.025(13) 0.007(12) C13 0.056(12) 0.018(9) 0.018(9) 0.007(7) 0.008(9) 0.002(9) C14 0.040(7) 0.039(7) 0.026(7) 0.018(5) -0.001(5) 0.003(6) C15 0.061(13) 0.025(10) 0.020(9) 0.001(8) 0.011(9) 0.026(10) C16 0.039(12) 0.061(15) 0.059(13) 0.044(12) 0.008(10) 0.022(11) C17 0.039(9) 0.021(8) 0.028(8) 0.008(7) -0.004(7) 0.002(7) N6 0.038(9) 0.026(8) 0.025(8) 0.021(7) 0.004(7) -0.001(7) C20 0.090(17) 0.021(11) 0.013(9) 0.004(8) 0.003(10) 0.004(10) C19 0.046(9) 0.022(8) 0.017(8) 0.012(7) 0.007(7) -0.004(7) C18 0.025(10) 0.047(13) 0.035(11) 0.027(10) -0.009(8) -0.004(9) N5 0.038(8) 0.044(8) 0.017(7) 0.013(6) 0.012(6) 0.010(7) C21 0.037(9) 0.035(9) 0.026(8) 0.015(7) 0.003(7) 0.004(7) C22 0.065(14) 0.038(11) 0.028(10) 0.015(9) 0.028(10) 0.025(10) C23 0.086(12) 0.049(11) 0.038(10) 0.017(8) 0.020(9) 0.010(10) C24 0.11(2) 0.057(15) 0.011(10) 0.005(10) -0.002(12) -0.008(15) C25 0.14(2) 0.056(15) 0.020(11) 0.013(10) 0.023(13) 0.020(15) C26 0.098(13) 0.068(12) 0.054(11) 0.044(9) 0.014(9) 0.025(10) C28 0.020(10) 0.089(17) 0.036(12) 0.039(12) 0.012(9) 0.020(11) C27 0.046(10) 0.040(10) 0.028(9) 0.022(8) 0.007(7) 0.014(8) N7 0.049(7) 0.042(6) 0.033(6) 0.026(5) 0.007(5) 0.002(5) C30 0.052(8) 0.045(7) 0.035(7) 0.026(6) 0.010(6) 0.010(6) N8 0.068(12) 0.045(11) 0.016(8) 0.007(7) 0.007(8) 0.011(9) C29 0.007(9) 0.050(13) 0.039(12) 0.025(10) 0.001(8) 0.003(8) Co2 0.0369(11) 0.0312(11) 0.0299(11) 0.0182(9) 0.0035(8) 0.0031(9) O21 0.058(8) 0.047(8) 0.054(8) 0.027(6) -0.006(6) -0.007(6) O22 0.056(7) 0.034(7) 0.040(7) 0.020(6) 0.005(6) 0.011(6) O23 0.071(8) 0.026(6) 0.028(6) 0.018(5) -0.010(6) 0.000(6) O24 0.081(8) 0.036(7) 0.032(6) 0.020(5) 0.002(6) 0.001(6) O25 0.050(7) 0.029(6) 0.038(6) 0.016(5) 0.005(5) -0.010(5) O26 0.064(8) 0.043(7) 0.043(7) 0.019(6) -0.009(6) 0.015(6) O27 0.051(6) 0.023(5) 0.044(6) 0.014(5) -0.004(5) -0.001(5) 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 88.8(4) . . ? O1 Co1 O4 91.8(4) . . ? O1 Co1 N1 91.2(4) . . ? O1 Co1 N4 88(2) . 1_556 ? O2 Co1 O4 178.4(5) . . ? O2 Co1 N1 97.3(4) . . ? O2 Co1 N4 83(2) . 1_556 ? O3 Co1 O1 178.5(5) . . ? O3 Co1 O2 90.1(4) . . ? O3 Co1 O4 89.3(5) . . ? O3 Co1 N1 89.9(4) . . ? O3 Co1 N4 91(2) . 1_556 ? O4 Co1 N1 84.1(4) . . ? O4 Co1 N4 95(2) . 1_556 ? N4 Co1 N1 179(2) 1_556 . ? O1 P1 O6 113.3(6) . . ? O1 P1 O7 106.9(6) . . ? O5 P1 O1 113.3(6) . . ? O5 P1 O6 112.9(6) . . ? O5 P1 O7 101.7(6) . . ? O6 P1 O7 107.7(6) . . ? O3 P2 O13 112.1(7) . . ? O3 P2 O14 113.1(7) . . ? O3 P2 O15 104.4(7) . . ? O13 P2 O15 108.2(7) . . ? O14 P2 O13 111.1(6) . . ? O14 P2 O15 107.5(7) . . ? P1 O1 Co1 137.7(7) . . ? Co1 O2 H2A 122.6 . . ? Co1 O2 H2B 113.4 . . ? H2A O2 H2B 114.3 . . ? P2 O3 Co1 138.2(8) . . ? Co1 O4 H4A 111.2 . . ? Co1 O4 H4B 111.8 . . ? H4A O4 H4B 102.6 . . ? C13 O7 P1 119.2(10) . . ? C17 O8 C14 107.2(12) . . ? C15 O9 H9 109.5 . . ? C16 O10 H10 109.5 . . ? C22 O15 P2 122.3(10) . . ? C23 O16 C26 106.0(17) . . ? C25 O19 H19 109.5 . . ? C24 O20 H20 109.5 . . ? C6 N2 N3 110.7(15) . . ? C7 N3 N2 113.5(16) . . ? C3 C2 H2 120.0 . . ? C3 C2 C1 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 C6 121.0(10) . . ? C4 C3 C6 119.0(10) . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 120.0 . . ? N1 C5 C4 120.0 . . ? N1 C5 H5 120.0 . . ? C5 N1 Co1 120.6(5) . . ? C5 N1 C1 120.0 . . ? C1 N1 Co1 119.1(5) . . ? C2 C1 H1 120.0 . . ? N1 C1 C2 120.0 . . ? N1 C1 H1 120.0 . . ? N2 C6 C3 119.3(17) . . ? N2 C6 H6 120.3 . . ? C3 C6 H6 120.3 . . ? N3 C7 H7 119.7 . . ? N3 C7 C10 120.6(17) . . ? C10 C7 H7 119.7 . . ? N4 C8 H8 120.0 . . ? N4 C8 C9 120.0 . . ? C9 C8 H8 120.0 . . ? C8 N4 Co1 122.2(5) . 1_554 ? C12 N4 Co1 117.5(5) . 1_554 ? C12 N4 C8 120.0 . . ? N4 C12 H12 120.0 . . ? C11 C12 N4 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C11 H11 120.0 . . ? C12 C11 C10 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C10 C7 122.2(11) . . ? C9 C10 C7 117.8(11) . . ? C9 C10 C11 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9A 120.0 . . ? O7 C13 H13A 109.9 . . ? O7 C13 H13B 109.9 . . ? O7 C13 C14 109.1(14) . . ? H13A C13 H13B 108.3 . . ? C14 C13 H13A 109.9 . . ? C14 C13 H13B 109.9 . . ? O8 C14 C13 107.5(14) . . ? O8 C14 H14 108.4 . . ? C13 C14 H14 108.4 . . ? C15 C14 O8 108.2(14) . . ? C15 C14 C13 115.8(14) . . ? C15 C14 H14 108.4 . . ? O9 C15 C14 114.6(15) . . ? O9 C15 H15 110.7 . . ? O9 C15 C16 104.4(15) . . ? C14 C15 H15 110.7 . . ? C14 C15 C16 105.4(14) . . ? C16 C15 H15 110.7 . . ? O10 C16 C15 118.4(17) . . ? O10 C16 H16 107.8 . . ? O10 C16 C17 114.1(16) . . ? C15 C16 H16 107.8 . . ? C15 C16 C17 100.3(14) . . ? C17 C16 H16 107.8 . . ? O8 C17 C16 107.9(14) . . ? O8 C17 H17 109.1 . . ? O8 C17 N5 105.2(13) . . ? C16 C17 H17 109.1 . . ? N5 C17 C16 116.3(15) . . ? N5 C17 H17 109.1 . . ? C20 N6 H6A 120.0 . . ? C20 N6 C21 120.0 . . ? C21 N6 H6A 120.0 . . ? O12 C20 N6 114.0(9) . . ? O12 C20 C19 126.0(9) . . ? C19 C20 N6 120.0 . . ? C20 C19 H19A 120.0 . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C18 H18 120.0 . . ? C19 C18 N5 120.0 . . ? N5 C18 H18 120.0 . . ? C18 N5 C17 119.5(9) . . ? C21 N5 C17 120.5(9) . . ? C21 N5 C18 120.0 . . ? O11 C21 N6 118.3(9) . . ? O11 C21 N5 121.6(9) . . ? N5 C21 N6 120.0 . . ? O15 C22 H22A 110.5 . . ? O15 C22 H22B 110.5 . . ? O15 C22 C23 106.0(15) . . ? H22A C22 H22B 108.7 . . ? C23 C22 H22A 110.5 . . ? C23 C22 H22B 110.5 . . ? O16 C23 C22 110.5(18) . . ? O16 C23 H23 107.0 . . ? O16 C23 C24 107.2(18) . . ? C22 C23 H23 107.0 . . ? C24 C23 C22 117.5(19) . . ? C24 C23 H23 107.0 . . ? O20 C24 C23 114(2) . . ? O20 C24 H24 107.7 . . ? O20 C24 C25 113.8(18) . . ? C23 C24 H24 107.7 . . ? C23 C24 C25 105(2) . . ? C25 C24 H24 107.7 . . ? O19 C25 C24 112.4(18) . . ? O19 C25 H25 112.6 . . ? O19 C25 C26 106.0(19) . . ? C24 C25 H25 112.6 . . ? C24 C25 C26 99.9(18) . . ? C26 C25 H25 112.6 . . ? O16 C26 C25 109.3(19) . . ? O16 C26 H26 109.9 . . ? O16 C26 N7 105.6(16) . . ? C25 C26 H26 109.9 . . ? N7 C26 C25 112.3(17) . . ? N7 C26 H26 109.9 . . ? C27 C28 H28 120.0 . . ? C27 C28 C29 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C27 H27 120.0 . . ? C28 C27 N7 120.0 . . ? N7 C27 H27 120.0 . . ? C27 N7 C26 125.2(10) . . ? C27 N7 C30 120.0 . . ? C30 N7 C26 114.8(10) . . ? O18 C30 N7 119.3(9) . . ? O18 C30 N8 120.6(9) . . ? N8 C30 N7 120.0 . . ? C30 N8 H8A 120.0 . . ? C30 N8 C29 120.0 . . ? C29 N8 H8A 120.0 . . ? O17 C29 C28 122.7(10) . . ? O17 C29 N8 117.3(10) . . ? N8 C29 C28 120.0 . . ? O21 Co2 O22 90.2(5) . . ? O21 Co2 O23 84.9(5) . . ? O21 Co2 O26 93.1(5) . . ? O22 Co2 O23 90.0(5) . . ? O24 Co2 O21 89.2(5) . . ? O24 Co2 O22 178.8(6) . . ? O24 Co2 O23 89.0(5) . . ? O24 Co2 O25 93.4(5) . . ? O24 Co2 O26 89.5(5) . . ? O25 Co2 O21 174.3(5) . . ? O25 Co2 O22 87.2(5) . . ? O25 Co2 O23 90.1(5) . . ? O25 Co2 O26 92.0(5) . . ? O26 Co2 O22 91.6(5) . . ? O26 Co2 O23 177.5(5) . . ? Co2 O21 H21A 127.0 . . ? Co2 O21 H21B 129.4 . . ? H21A O21 H21B 103.6 . . ? Co2 O22 H22C 110.8 . . ? Co2 O22 H22D 113.5 . . ? H22C O22 H22D 101.2 . . ? Co2 O23 H23A 110.5 . . ? Co2 O23 H23B 110.9 . . ? H23A O23 H23B 103.1 . . ? Co2 O24 H24A 110.5 . . ? Co2 O24 H24B 117.9 . . ? H24A O24 H24B 91.2 . . ? Co2 O25 H25A 111.3 . . ? Co2 O25 H25B 111.1 . . ? H25A O25 H25B 102.8 . . ? Co2 O26 H26A 111.9 . . ? Co2 O26 H26B 113.4 . . ? H26A O26 H26B 101.0 . . ? H27A O27 H27B 123.1 . . ? 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 2.101(10) . ? Co1 O2 2.112(11) . ? Co1 O3 2.075(11) . ? Co1 O4 2.116(11) . ? Co1 N1 2.218(7) . ? Co1 N4 2.165(15) 1_556 ? P1 O1 1.507(10) . ? P1 O5 1.459(11) . ? P1 O6 1.511(11) . ? P1 O7 1.605(12) . ? P2 O3 1.517(12) . ? P2 O13 1.554(13) . ? P2 O14 1.532(11) . ? P2 O15 1.597(12) . ? O2 H2A 0.7826 . ? O2 H2B 0.9117 . ? O4 H4A 0.8831 . ? O4 H4B 0.8838 . ? O7 C13 1.464(19) . ? O8 C14 1.493(19) . ? O8 C17 1.40(2) . ? O9 H9 0.8200 . ? O9 C15 1.404(18) . ? O10 H10 0.8200 . ? O10 C16 1.36(2) . ? O11 C21 1.265(14) . ? O12 C20 1.267(15) . ? O15 C22 1.420(19) . ? O16 C23 1.42(3) . ? O16 C26 1.45(2) . ? O17 C29 1.247(14) . ? O18 C30 1.301(14) . ? O19 H19 0.8200 . ? O19 C25 1.442(18) . ? O20 H20 0.8200 . ? O20 C24 1.41(3) . ? N2 N3 1.430(17) . ? N2 C6 1.28(2) . ? N3 C7 1.24(2) . ? C2 H2 0.9300 . ? C2 C3 1.3900 . ? C2 C1 1.3900 . ? C3 C4 1.3900 . ? C3 C6 1.494(17) . ? C4 H4 0.9300 . ? C4 C5 1.3900 . ? C5 H5 0.9300 . ? C5 N1 1.3900 . ? N1 C1 1.3900 . ? C1 H1 0.9300 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C7 C10 1.50(2) . ? C8 H8 0.9300 . ? C8 N4 1.3900 . ? C8 C9 1.3900 . ? N4 C12 1.3900 . ? C12 H12 0.9300 . ? C12 C11 1.3900 . ? C11 H11 0.9300 . ? C11 C10 1.3900 . ? C10 C9 1.3900 . ? C9 H9A 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.52(2) . ? C14 H14 0.9800 . ? C14 C15 1.47(2) . ? C15 H15 0.9800 . ? C15 C16 1.53(3) . ? C16 H16 0.9800 . ? C16 C17 1.56(2) . ? C17 H17 0.9800 . ? C17 N5 1.439(18) . ? N6 H6A 0.8600 . ? N6 C20 1.3900 . ? N6 C21 1.3900 . ? C20 C19 1.3900 . ? C19 H19A 0.9300 . ? C19 C18 1.3900 . ? C18 H18 0.9300 . ? C18 N5 1.3900 . ? N5 C21 1.3900 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.51(2) . ? C23 H23 0.9800 . ? C23 C24 1.48(3) . ? C24 H24 0.9800 . ? C24 C25 1.49(3) . ? C25 H25 0.9800 . ? C25 C26 1.56(3) . ? C26 H26 0.9800 . ? C26 N7 1.51(2) . ? C28 H28 0.9300 . ? C28 C27 1.3900 . ? C28 C29 1.3900 . ? C27 H27 0.9300 . ? C27 N7 1.3900 . ? N7 C30 1.3900 . ? C30 N8 1.3900 . ? N8 H8A 0.8600 . ? N8 C29 1.3900 . ? Co2 O21 2.080(13) . ? Co2 O22 2.095(12) . ? Co2 O23 2.153(12) . ? Co2 O24 2.055(12) . ? Co2 O25 2.074(12) . ? Co2 O26 2.086(12) . ? O21 H21A 0.9105 . ? O21 H21B 0.9115 . ? O22 H22C 0.8903 . ? O22 H22D 0.8938 . ? O23 H23A 0.8757 . ? O23 H23B 0.8770 . ? O24 H24A 0.8588 . ? O24 H24B 0.8583 . ? O25 H25A 0.8804 . ? O25 H25B 0.8815 . ? O26 H26A 0.9017 . ? O26 H26B 0.9058 . ? O27 H27A 1.0284 . ? O27 H27B 0.8511 . ? 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 O2 H2B O5 0.91 1.87 2.714(14) 152.8 . yes O4 H4A O5 0.88 2.00 2.724(13) 138.8 1_455 yes O4 H4B O13 0.88 1.97 2.707(16) 139.8 . yes N6 H6A O18 0.86 1.83 2.680(13) 172.2 1_654 yes N8 H8A O11 0.86 1.97 2.814(14) 168.0 1_456 yes O22 H22D O14 0.89 1.84 2.701(17) 161.3 1_545 yes O23 H23A O14 0.88 1.84 2.674(14) 158.5 1_545 yes O23 H23B O12 0.88 2.21 2.889(18) 133.7 1_445 yes O25 H25A O6 0.88 1.97 2.738(15) 144.2 . yes O26 H26A O17 0.90 2.00 2.832(18) 153.0 . yes O26 H26B O6 0.91 2.07 2.786(16) 134.9 1_455 yes O27 H27B O24 0.85 1.81 2.630(17) 162.1 . 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 174.3(6) . . . . ? Co1 N4 C12 C11 -172.9(6) 1_554 . . . ? P1 O7 C13 C14 179.4(11) . . . . ? P2 O15 C22 C23 -178.6(14) . . . . ? O1 P1 O7 C13 -67.2(12) . . . . ? O3 P2 O15 C22 141.4(14) . . . . ? O5 P1 O1 Co1 -0.8(12) . . . . ? O5 P1 O7 C13 173.7(11) . . . . ? O6 P1 O1 Co1 129.5(9) . . . . ? O6 P1 O7 C13 54.9(13) . . . . ? O7 P1 O1 Co1 -112.0(9) . . . . ? O7 C13 C14 O8 -67.1(17) . . . . ? O7 C13 C14 C15 54(2) . . . . ? O8 C14 C15 O9 -95.5(18) . . . . ? O8 C14 C15 C16 18.7(18) . . . . ? O8 C17 N5 C18 66.9(14) . . . . ? O8 C17 N5 C21 -112.0(11) . . . . ? O9 C15 C16 O10 -34(2) . . . . ? O9 C15 C16 C17 91.2(16) . . . . ? O10 C16 C17 O8 160.4(16) . . . . ? O10 C16 C17 N5 -82(2) . . . . ? O12 C20 C19 C18 -179.4(15) . . . . ? O13 P2 O3 Co1 -13.4(12) . . . . ? O13 P2 O15 C22 -99.1(15) . . . . ? O14 P2 O3 Co1 -140.0(9) . . . . ? O14 P2 O15 C22 21.0(16) . . . . ? O15 P2 O3 Co1 103.4(10) . . . . ? O15 C22 C23 O16 -72(2) . . . . ? O15 C22 C23 C24 52(3) . . . . ? O16 C23 C24 O20 -161.3(17) . . . . ? O16 C23 C24 C25 -36(2) . . . . ? O16 C26 N7 C27 15(2) . . . . ? O16 C26 N7 C30 -165.2(12) . . . . ? O18 C30 N8 C29 177.6(13) . . . . ? O19 C25 C26 O16 98.6(19) . . . . ? O19 C25 C26 N7 -144.6(16) . . . . ? O20 C24 C25 O19 45(3) . . . . ? O20 C24 C25 C26 157(2) . . . . ? N2 N3 C7 C10 -179.9(14) . . . . ? N3 N2 C6 C3 -179.4(13) . . . . ? N3 C7 C10 C11 11(3) . . . . ? N3 C7 C10 C9 -167.2(16) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C2 C3 C6 N2 0(2) . . . . ? C3 C2 C1 N1 0.0 . . . . ? C3 C4 C5 N1 0.0 . . . . ? C4 C3 C6 N2 179.6(15) . . . . ? C4 C5 N1 Co1 -174.2(7) . . . . ? C4 C5 N1 C1 0.0 . . . . ? C5 N1 C1 C2 0.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C6 180.0(12) . . . . ? C6 N2 N3 C7 178(2) . . . . ? C6 C3 C4 C5 -180.0(11) . . . . ? C7 C10 C9 C8 177.9(13) . . . . ? C8 N4 C12 C11 0.0 . . . . ? N4 C8 C9 C10 0.0 . . . . ? N4 C12 C11 C10 0.0 . . . . ? C12 C11 C10 C7 -177.8(13) . . . . ? C12 C11 C10 C9 0.0 . . . . ? C11 C10 C9 C8 0.0 . . . . ? C9 C8 N4 Co1 172.6(7) . . . 1_554 ? C9 C8 N4 C12 0.0 . . . . ? C13 C14 C15 O9 143.9(16) . . . . ? C13 C14 C15 C16 -102.0(18) . . . . ? C14 O8 C17 C16 -22.2(18) . . . . ? C14 O8 C17 N5 -147.0(12) . . . . ? C14 C15 C16 O10 -154.8(16) . . . . ? C14 C15 C16 C17 -30.0(18) . . . . ? C15 C16 C17 O8 32.6(18) . . . . ? C15 C16 C17 N5 150.5(15) . . . . ? C16 C17 N5 C18 -52.4(18) . . . . ? C16 C17 N5 C21 128.6(13) . . . . ? C17 O8 C14 C13 128.0(15) . . . . ? C17 O8 C14 C15 2.3(18) . . . . ? C17 N5 C21 O11 0.7(14) . . . . ? C17 N5 C21 N6 179.0(12) . . . . ? N6 C20 C19 C18 0.0 . . . . ? C20 N6 C21 O11 178.3(12) . . . . ? C20 N6 C21 N5 0.0 . . . . ? C20 C19 C18 N5 0.0 . . . . ? C19 C18 N5 C17 -179.0(12) . . . . ? C19 C18 N5 C21 0.0 . . . . ? C18 N5 C21 O11 -178.3(13) . . . . ? C18 N5 C21 N6 0.0 . . . . ? C21 N6 C20 O12 179.5(13) . . . . ? C21 N6 C20 C19 0.0 . . . . ? C22 C23 C24 O20 74(3) . . . . ? C22 C23 C24 C25 -160.9(19) . . . . ? C23 O16 C26 C25 -2(2) . . . . ? C23 O16 C26 N7 -123.4(18) . . . . ? C23 C24 C25 O19 -81(2) . . . . ? C23 C24 C25 C26 31(2) . . . . ? C24 C25 C26 O16 -18(2) . . . . ? C24 C25 C26 N7 98.5(19) . . . . ? C25 C26 N7 C27 -103.9(15) . . . . ? C25 C26 N7 C30 75.8(18) . . . . ? C26 O16 C23 C22 152.2(16) . . . . ? C26 O16 C23 C24 23(2) . . . . ? C26 N7 C30 O18 2.7(16) . . . . ? C26 N7 C30 N8 -179.7(14) . . . . ? C28 C27 N7 C26 179.7(16) . . . . ? C28 C27 N7 C30 0.0 . . . . ? C27 C28 C29 O17 -177.8(13) . . . . ? C27 C28 C29 N8 0.0 . . . . ? C27 N7 C30 O18 -177.6(13) . . . . ? C27 N7 C30 N8 0.0 . . . . ? N7 C30 N8 C29 0.0 . . . . ? C30 N8 C29 O17 177.9(12) . . . . ? C30 N8 C29 C28 0.0 . . . . ? C29 C28 C27 N7 0.0 . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.89(5) 2 0.11(5) loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.081 0.036 -0.035 173.5 58.8 ? 2 -0.104 0.807 0.339 83.2 37.0 ?