#------------------------------------------------------------------------------ #$Date: 2023-12-04 20:16:21 +0200 (Mon, 04 Dec 2023) $ #$Revision: 288017 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247820.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_7247820 loop_ _publ_author_name 'Ahmed, Naushad' 'Sahu, Prem Prakash' _publ_section_title ; Ferromagnetically coupled CoII2LnIII2 complexes (where LnIII = Ho, Er, Yb): experimental and theoretical investigations ; _journal_issue 47 _journal_name_full CrystEngComm _journal_page_first 6592 _journal_page_last 6601 _journal_paper_doi 10.1039/D3CE00827D _journal_volume 25 _journal_year 2023 _chemical_formula_moiety 'C66 H69 Co2 Ho2 N4 O20, 8(C H4 O), 3(N O3)' _chemical_formula_sum 'C74 H101 Co2 Ho2 N7 O37' _chemical_formula_weight 2128.33 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2022-08-30 _audit_creation_method ; Olex2 1.5-alpha (compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535) ; _audit_update_record ; 2023-10-16 deposited with the CCDC. 2023-10-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.761(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 26.692(7) _cell_length_b 15.981(4) _cell_length_c 19.803(5) _cell_measurement_reflns_used 11661 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.2 _cell_measurement_theta_min 3.1 _cell_volume 8389(4) _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type ; Rigaku Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_unetI/netI 0.0505 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 41581 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 3.074 _exptl_absorpt_coefficient_mu 2.350 _exptl_absorpt_correction_T_max 0.638 _exptl_absorpt_correction_T_min 0.384 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Red _exptl_crystal_density_diffrn 1.685 _exptl_crystal_description Block _exptl_crystal_F_000 4312 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.29 _refine_diff_density_max 1.134 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 602 _refine_ls_number_reflns 7366 _refine_ls_number_restraints 75 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0456 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+63.6302P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.0930 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6799 _reflns_number_total 7366 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00827d2.cif _cod_data_source_block Co2Ho2 _cod_database_code 7247820 _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 0.549 _shelx_estimated_absorpt_t_min 0.418 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2. Restrained distances O33-H33 0.87 with sigma of 0.01 Co1-H33 2.803457 with sigma of 0.02 C44-H33 1.910224 with sigma of 0.02 N1-O5 \\sim N1A-O5A with sigma of 0.02 N1-O1 \\sim N1A-O1A with sigma of 0.02 N1-O4 \\sim N1A-O4A with sigma of 0.02 O1-O5 \\sim O1A-O5A with sigma of 0.04 O1-O4 \\sim O1A-O4A with sigma of 0.04 O4-O5 \\sim O4A-O5A with sigma of 0.04 3. Uiso/Uaniso restraints and constraints N1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O4A \\sim O4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O5 \\sim O5A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O1 \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002 4. Rigid body (RIGU) restrains O4A, O5A, O1A, N1A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N1, O4, O5, O1 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(O4A)=Sof(N1A)=Sof(O5A)=Sof(O1A)=1-FVAR(1) Sof(N1)=Sof(O1)=Sof(O4)=Sof(O5)=FVAR(1) Fixed Sof: H62A(0.5) H62B(0.5) H62C(0.5) 6.a Rotating group: O1W(H1WA,H1WB) 6.b Secondary CH2 refined with riding coordinates: C24(H24A,H24B), C44(H44A,H44B) 6.c Me refined with riding coordinates: C52(H52A,H52B,H52C), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C62(H62A,H62B, H62C) 6.d Aromatic/amide H refined with riding coordinates: C33(H33A), C13(H13A), C12(H12), C42(H42), C17(H17), C41(H41), C14(H14), C37(H37), C19(H19), C39(H39), C20(H20), C40(H40), C34(H34), C22(H22), C21(H21), C32(H32) 6.e Idealised Me refined as rotating group: C4S(H4SA,H4SB,H4SC), C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC), C1(H1A,H1B,H1C) 6.f Idealised tetrahedral OH refined as rotating group: O13(H13), O3S(H3S), O2S(H2S), O4S(H4S), O6(H6) ; _shelx_res_file ; TITL MS-NA-H0-CO co2ho2.res created by SHELXL-2018/3 at 18:57:46 on 30-Aug-2022 CELL 0.7107 26.692 15.981 19.803 90 96.761 90 ZERR 4 0.007 0.004 0.005 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Co Ho N O UNIT 296 404 8 8 28 148 SADI N1 O5 N1A O5A SADI N1 O1 N1A O1A SADI N1 O4 N1A O4A SADI 0.04 O1 O5 O1A O5A SADI 0.04 O1 O4 O1A O4A SADI 0.04 O4 O5 O4A O5A RIGU O4A O5A O1A N1A RIGU N1 O4 O5 O1 SIMU N1A N1 SIMU O4A O4 SIMU O5 O5A SIMU O1 O1A ISOR 0.01 0.002 C1 DFIX 0.87 0.01 O33 H33 DANG 2.803457 0.02 Co1 H33 DANG 1.910224 0.02 C44 H33 L.S. 10 PLAN 5 SIZE 0.29 0.33 0.45 TEMP -173(2) CONF WPDB -2 HTAB BOND $H LIST 4 MORE -1 fmap 2 acta SHEL 99999 0 OMIT -3 50 OMIT 21 3 4 OMIT -11 7 13 OMIT 6 0 16 OMIT 20 4 5 OMIT -1 3 1 OMIT -16 10 3 OMIT 2 12 8 OMIT -9 5 15 OMIT 22 0 2 REM REM REM WGHT 0.020100 63.630196 FVAR 0.33923 0.50847 HO1 4 0.556088 0.330267 0.845073 11.00000 0.01675 0.01560 = 0.02278 -0.00094 0.00372 0.00247 CO1 3 0.607533 0.176682 0.959132 11.00000 0.01478 0.01573 = 0.01904 -0.00080 0.00581 -0.00064 O11 6 0.615502 0.228094 0.866502 11.00000 0.01381 0.01829 = 0.02135 0.00003 0.00428 0.00227 C52 1 0.577303 0.152599 0.700555 11.00000 0.02769 0.03104 = 0.03754 -0.01047 -0.00369 0.00959 AFIX 33 H52A 2 0.564163 0.107570 0.669847 11.00000 -1.50000 H52B 2 0.609520 0.172409 0.687396 11.00000 -1.50000 H52C 2 0.582427 0.131473 0.747317 11.00000 -1.50000 AFIX 0 O31 6 0.561777 0.280594 0.956726 11.00000 0.01735 0.02455 = 0.02346 -0.00514 0.00636 0.00306 O61 6 0.532807 0.450982 0.790083 11.00000 0.02529 0.01603 = 0.03720 0.00074 -0.00135 0.00790 O12 6 0.641005 0.354323 0.796589 11.00000 0.02021 0.01334 = 0.03008 0.00405 0.00835 0.00024 O32 6 0.488697 0.382922 0.915554 11.00000 0.02141 0.03777 = 0.03182 -0.00200 0.00482 0.01219 O33 6 0.676891 0.237943 0.997025 11.00000 0.01848 0.01577 = 0.02533 0.00120 0.00273 -0.00381 H33 2 0.677586 0.290611 1.011394 11.00000 -1.50000 O1W 6 0.599923 0.433514 0.912357 11.00000 0.03764 0.02085 = 0.03215 -0.00094 -0.00123 -0.00301 AFIX 7 H1WA 2 0.616113 0.410784 0.950077 11.00000 -1.50000 H1WB 2 0.624933 0.454884 0.891327 11.00000 -1.50000 AFIX 0 O13 6 0.539146 0.106125 0.938062 11.00000 0.01693 0.02446 = 0.02817 -0.00030 0.00109 -0.00379 AFIX 147 H13 2 0.521724 0.134825 0.908482 11.00000 -1.50000 AFIX 0 O3S 6 0.656622 0.554846 0.866906 11.00000 0.04233 0.02735 = 0.05269 0.00077 -0.00440 -0.00933 AFIX 147 H3S 2 0.648105 0.579868 0.830036 11.00000 -1.50000 AFIX 0 O2S 6 0.744006 0.603290 1.130369 11.00000 0.06071 0.04105 = 0.06444 -0.00110 0.00944 0.00436 AFIX 147 H2S 2 0.722303 0.565883 1.120289 11.00000 -1.50000 AFIX 0 O4S 6 0.599858 0.206319 1.274126 11.00000 0.05488 0.05004 = 0.04311 0.00945 0.00663 -0.00070 AFIX 147 H4S 2 0.571019 0.185308 1.274209 11.00000 -1.50000 AFIX 0 N31 5 0.604420 0.167078 1.062209 11.00000 0.01584 0.02107 = 0.01969 -0.00046 0.00489 -0.00440 N11 5 0.643166 0.071892 0.926295 11.00000 0.01344 0.01647 = 0.02076 -0.00033 0.00353 -0.00338 C25 1 0.647622 0.417758 0.746291 11.00000 0.02699 0.01847 = 0.03894 0.01160 0.00421 -0.00025 AFIX 33 H25A 2 0.623212 0.462932 0.749660 11.00000 -1.50000 H25B 2 0.681934 0.440364 0.754379 11.00000 -1.50000 H25C 2 0.642204 0.392953 0.700758 11.00000 -1.50000 AFIX 0 C33 1 0.453046 0.328255 1.085026 11.00000 0.03257 0.10441 = 0.03455 -0.00635 0.01378 0.03149 AFIX 43 H33A 2 0.427668 0.339692 1.113593 11.00000 -1.20000 AFIX 0 C35 1 0.487614 0.348664 0.980189 11.00000 0.02122 0.03971 = 0.02297 -0.00777 0.00150 0.00356 O71 6 0.549927 0.287258 0.731422 11.00000 0.02768 0.01804 = 0.02885 -0.00154 0.01067 -0.00321 C16 1 0.658227 0.218700 0.838199 11.00000 0.01082 0.01756 = 0.01561 -0.00415 0.00183 -0.00163 C36 1 0.527788 0.292390 0.999877 11.00000 0.01668 0.02751 = 0.02557 -0.01083 0.00555 -0.00181 C51 1 0.540878 0.222345 0.696199 11.00000 0.01481 0.02103 = 0.02372 0.00122 0.00737 -0.00095 C13 1 0.744847 0.207780 0.770491 11.00000 0.02273 0.02713 = 0.03083 0.00147 0.01648 -0.00045 AFIX 43 H13A 2 0.774243 0.203853 0.747896 11.00000 -1.20000 AFIX 0 C12 1 0.731147 0.141946 0.809067 11.00000 0.02031 0.02145 = 0.02898 -0.00228 0.00791 0.00319 AFIX 43 H12 2 0.750973 0.092425 0.811923 11.00000 -1.20000 AFIX 0 C42 1 0.729649 0.075150 1.120845 11.00000 0.01294 0.02124 = 0.02973 -0.00137 0.00754 -0.00486 AFIX 43 H42 2 0.763848 0.080973 1.112709 11.00000 -1.20000 AFIX 0 C17 1 0.675704 0.072858 0.882614 11.00000 0.01546 0.01690 = 0.02267 -0.00366 0.00325 0.00131 AFIX 43 H17 2 0.692526 0.021963 0.874915 11.00000 -1.20000 AFIX 0 C11 1 0.688345 0.146144 0.844527 11.00000 0.01682 0.01449 = 0.01935 -0.00340 0.00490 -0.00107 C41 1 0.716897 0.013454 1.165400 11.00000 0.02360 0.02128 = 0.03199 0.00061 -0.00285 -0.00138 AFIX 43 H41 2 0.742255 -0.022308 1.187214 11.00000 -1.20000 AFIX 0 C14 1 0.715501 0.280622 0.764482 11.00000 0.02399 0.02338 = 0.02092 0.00079 0.00798 -0.00352 AFIX 43 H14 2 0.724623 0.326104 0.737556 11.00000 -1.20000 AFIX 0 C15 1 0.673259 0.285541 0.798070 11.00000 0.01808 0.01387 = 0.02168 -0.00116 0.00068 -0.00217 C38 1 0.643126 0.117320 1.099360 11.00000 0.02025 0.02430 = 0.01672 -0.00299 0.00125 -0.00353 C37 1 0.570336 0.200796 1.094304 11.00000 0.02255 0.03685 = 0.01797 -0.00047 0.00643 -0.00506 AFIX 43 H37 2 0.571802 0.189138 1.141537 11.00000 -1.20000 AFIX 0 C4S 1 0.635644 0.157645 1.315989 11.00000 0.08998 0.05888 = 0.05064 0.01539 0.00872 0.02082 AFIX 137 H4SA 2 0.669774 0.177169 1.310738 11.00000 -1.50000 H4SB 2 0.632285 0.098725 1.302497 11.00000 -1.50000 H4SC 2 0.629559 0.163466 1.363609 11.00000 -1.50000 AFIX 0 C24 1 0.539875 0.020385 0.915897 11.00000 0.02496 0.02705 = 0.04988 -0.00913 0.00942 -0.01163 AFIX 23 H24A 2 0.544862 0.018672 0.867163 11.00000 -1.20000 H24B 2 0.506983 -0.006068 0.920933 11.00000 -1.20000 AFIX 0 C43 1 0.693118 0.129001 1.087633 11.00000 0.02137 0.01832 = 0.01949 -0.00324 0.00449 -0.00299 C19 1 0.670709 -0.054301 0.990985 11.00000 0.03303 0.01934 = 0.02713 -0.00103 0.01038 0.00146 AFIX 43 H19 2 0.704931 -0.037456 0.992132 11.00000 -1.20000 AFIX 0 C44 1 0.713035 0.195827 1.044886 11.00000 0.02257 0.03003 = 0.02957 0.01011 0.00109 -0.00263 AFIX 23 H44A 2 0.730191 0.238418 1.075725 11.00000 -1.20000 H44B 2 0.738920 0.170369 1.019385 11.00000 -1.20000 AFIX 0 C39 1 0.630460 0.055502 1.143778 11.00000 0.02179 0.03262 = 0.02571 0.00177 0.00510 -0.01110 AFIX 43 H39 2 0.596180 0.048083 1.150994 11.00000 -1.20000 AFIX 0 C18 1 0.632354 -0.005495 0.957791 11.00000 0.02620 0.01423 = 0.02774 -0.00336 0.01321 -0.00221 C23 1 0.581363 -0.028133 0.956501 11.00000 0.03248 0.01938 = 0.03250 -0.00405 0.01280 -0.00382 C20 1 0.658481 -0.128121 1.022539 11.00000 0.05630 0.01974 = 0.03587 0.00581 0.00925 0.00544 AFIX 43 H20 2 0.684474 -0.162177 1.044983 11.00000 -1.20000 AFIX 0 C31 1 0.529701 0.255230 1.064781 11.00000 0.01819 0.04437 = 0.02313 -0.00628 0.00515 0.00453 C40 1 0.667485 0.004257 1.177865 11.00000 0.03207 0.02854 = 0.02515 0.00910 0.00293 -0.01271 AFIX 43 H40 2 0.658728 -0.036545 1.209335 11.00000 -1.20000 AFIX 0 C34 1 0.450771 0.365858 1.021342 11.00000 0.03008 0.07860 = 0.02859 -0.00829 0.00244 0.02655 AFIX 43 H34 2 0.424004 0.403098 1.006389 11.00000 -1.20000 AFIX 0 C3S 1 0.685497 0.609783 0.912928 11.00000 0.04539 0.03921 = 0.06240 -0.00786 0.00141 -0.00897 AFIX 137 H3SA 2 0.693790 0.581672 0.956801 11.00000 -1.50000 H3SB 2 0.665859 0.660404 0.919262 11.00000 -1.50000 H3SC 2 0.716702 0.625060 0.894375 11.00000 -1.50000 AFIX 0 C22 1 0.570320 -0.103258 0.988720 11.00000 0.04336 0.02286 = 0.05890 0.00086 0.02892 -0.01420 AFIX 43 H22 2 0.536269 -0.120807 0.988163 11.00000 -1.20000 AFIX 0 C21 1 0.608966 -0.151846 1.021317 11.00000 0.06704 0.01849 = 0.05374 0.00524 0.02819 -0.01191 AFIX 43 H21 2 0.601020 -0.202284 1.043110 11.00000 -1.20000 AFIX 0 C32 1 0.491930 0.274574 1.106740 11.00000 0.03236 0.08519 = 0.02671 -0.00001 0.01359 0.02493 AFIX 43 H32 2 0.493428 0.250098 1.150650 11.00000 -1.20000 AFIX 0 C45 1 0.453119 0.449475 0.897821 11.00000 0.05637 0.07066 = 0.06576 0.02675 0.02750 0.05166 AFIX 33 H45A 2 0.456672 0.469420 0.851830 11.00000 -1.50000 H45B 2 0.418753 0.428594 0.899379 11.00000 -1.50000 H45C 2 0.459745 0.495658 0.930199 11.00000 -1.50000 AFIX 0 O54 6 0.499849 0.216101 0.655971 11.00000 0.02004 0.02951 = 0.02603 -0.00239 0.00047 0.00584 C61 1 0.500000 0.488233 0.750000 10.50000 0.02311 0.00687 = 0.04060 0.00000 0.00353 0.00000 C62 1 0.500000 0.582598 0.750000 10.50000 0.04641 0.01500 = 0.08243 0.00000 -0.02139 0.00000 PART -1 AFIX 33 H62A 2 0.527295 0.603039 0.783350 10.50000 -1.50000 H62B 2 0.505128 0.603039 0.704664 10.50000 -1.50000 H62C 2 0.467577 0.603039 0.761985 10.50000 -1.50000 AFIX 0 PART 0 C2S 1 0.730585 0.676067 1.091835 11.00000 0.12294 0.04368 = 0.05355 0.00892 0.01678 0.01749 AFIX 137 H2SA 2 0.707197 0.709784 1.115118 11.00000 -1.50000 H2SB 2 0.714283 0.660012 1.046762 11.00000 -1.50000 H2SC 2 0.760971 0.708850 1.086915 11.00000 -1.50000 AFIX 0 N3 5 0.500000 0.070657 1.250000 10.50000 0.06842 0.04015 = 0.02241 0.00000 0.01815 0.00000 O2 6 0.540299 0.033808 1.248954 11.00000 0.11827 0.05064 = 0.11313 0.03023 0.08843 0.03942 O3 6 0.500000 0.147975 1.250000 10.50000 0.05390 0.03026 = 0.15489 0.00000 -0.01685 0.00000 PART 1 N1 5 0.675267 0.447641 1.051124 21.00000 0.01833 0.01924 = 0.04002 -0.00699 0.00290 -0.00161 O1 6 0.642897 0.388470 1.036708 21.00000 0.03228 0.02163 = 0.04597 -0.00640 -0.00400 -0.00683 O4 6 0.719600 0.433628 1.046029 21.00000 0.01986 0.05239 = 0.07862 -0.00505 0.00620 0.00469 O5 6 0.663060 0.514500 1.071604 21.00000 0.06287 0.02751 = 0.11895 -0.02945 0.03708 -0.00489 PART 2 O4A 6 0.681506 0.435972 1.026711 -21.00000 0.10379 0.13149 = 0.04327 0.01583 0.01820 0.01582 N1A 5 0.664173 0.425575 1.081692 -21.00000 0.03891 0.02763 = 0.03224 -0.00865 -0.01163 0.01069 O5A 6 0.665651 0.478585 1.125650 -21.00000 0.04207 0.03360 = 0.06097 -0.02644 -0.00666 0.00777 O1A 6 0.646241 0.354533 1.092494 -21.00000 0.05696 0.03477 = 0.08729 -0.01780 0.01080 -0.00483 PART 0 O6 6 0.629354 0.639377 0.753108 11.00000 0.06019 0.05411 = 0.04921 0.01532 0.01073 0.00515 AFIX 147 H6 2 0.619048 0.687258 0.762239 11.00000 -1.50000 AFIX 0 C1 1 0.630733 0.633534 0.692650 11.00000 0.11964 0.11911 = 0.12152 0.00010 0.01293 -0.00031 AFIX 137 H1A 2 0.596265 0.632227 0.669307 11.00000 -1.50000 H1B 2 0.648311 0.581895 0.682840 11.00000 -1.50000 H1C 2 0.648742 0.681733 0.676666 11.00000 -1.50000 AFIX 0 HKLF 4 REM MS-NA-H0-CO REM wR2 = 0.0930, GooF = S = 1.106, Restrained GooF = 1.104 for all data REM R1 = 0.0456 for 6799 Fo > 4sig(Fo) and 0.0517 for all 7366 data REM 602 parameters refined using 75 restraints END WGHT 0.0201 63.6271 REM Instructions for potential hydrogen bonds HTAB O33 N1 HTAB O33 O1 HTAB O33 O4 HTAB O33 O4A HTAB O33 N1A HTAB O33 O1A HTAB O1W N1 HTAB O1W O1 HTAB O1W O4A HTAB O1W O3S EQIV $1 -x+1, y, -z+3/2 HTAB O13 O54_$1 HTAB O3S O6 HTAB O2S N1 HTAB O2S O4 HTAB O2S O5 HTAB O2S O5A HTAB O4S N3 HTAB O4S O2 HTAB O4S O3 HTAB C25 O61 EQIV $3 -x+3/2, -y+1/2, -z+2 HTAB C17 O2S_$3 EQIV $4 x, -y+1, z-1/2 HTAB C14 O2S_$4 HTAB C37 O4S EQIV $5 x, -y, z-1/2 HTAB C24 O2_$5 HTAB C44 O4_$3 HTAB C39 O2 HTAB C45 O61 EQIV $6 -x+1, -y+1, -z+2 HTAB C45 O5_$6 HTAB C62 O6_$1 HTAB O6 O4S_$4 HTAB C1 N1A_$4 HTAB C1 O5A_$4 REM Highest difference peak 1.134, deepest hole -0.910, 1-sigma level 0.117 Q1 1 0.5634 0.3356 0.8897 11.00000 0.05 1.13 Q2 1 0.5502 0.3321 0.7929 11.00000 0.05 0.83 Q3 1 0.5899 0.3257 0.8258 11.00000 0.05 0.72 Q4 1 0.5218 0.3278 0.8707 11.00000 0.05 0.72 Q5 1 0.5000 0.1701 0.7500 10.50000 0.05 0.67 ; _shelx_res_checksum 40466 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.55609(2) 0.33027(2) 0.84507(2) 0.01827(8) Uani 1 1 d . . . . . Co1 Co 0.60753(2) 0.17668(4) 0.95913(3) 0.01621(15) Uani 1 1 d D . . . . O11 O 0.61550(12) 0.2281(2) 0.86650(16) 0.0176(7) Uani 1 1 d . . . . . C52 C 0.5773(2) 0.1526(4) 0.7006(3) 0.0327(14) Uani 1 1 d . . . . . H52A H 0.564163 0.107570 0.669847 0.049 Uiso 1 1 calc R U . . . H52B H 0.609520 0.172409 0.687396 0.049 Uiso 1 1 calc R U . . . H52C H 0.582427 0.131473 0.747317 0.049 Uiso 1 1 calc R U . . . O31 O 0.56178(12) 0.2806(2) 0.95673(17) 0.0215(8) Uani 1 1 d . . . . . O61 O 0.53281(13) 0.4510(2) 0.79008(18) 0.0266(8) Uani 1 1 d . . . . . O12 O 0.64100(12) 0.3543(2) 0.79659(17) 0.0208(8) Uani 1 1 d . . . . . O32 O 0.48870(13) 0.3829(3) 0.91555(18) 0.0302(9) Uani 1 1 d . . . . . O33 O 0.67689(12) 0.2379(2) 0.99702(17) 0.0198(7) Uani 1 1 d D . . . . H33 H 0.6776(10) 0.2906(8) 1.0114(18) 0.030 Uiso 1 1 d D U . . . O1W O 0.59992(14) 0.4335(2) 0.91236(19) 0.0306(9) Uani 1 1 d . . . . . H1WA H 0.616113 0.410784 0.950077 0.046 Uiso 1 1 d R U . . . H1WB H 0.624933 0.454884 0.891327 0.046 Uiso 1 1 d R U . . . O13 O 0.53915(13) 0.1061(2) 0.93806(17) 0.0233(8) Uani 1 1 d . . . . . H13 H 0.521724 0.134825 0.908482 0.035 Uiso 1 1 calc R U . . . O3S O 0.65662(16) 0.5548(3) 0.8669(2) 0.0416(11) Uani 1 1 d . . . . . H3S H 0.648105 0.579868 0.830036 0.062 Uiso 1 1 calc R U . . . O2S O 0.74401(19) 0.6033(3) 1.1304(3) 0.0552(13) Uani 1 1 d . . . . . H2S H 0.722303 0.565883 1.120289 0.083 Uiso 1 1 calc R U . . . O4S O 0.59986(17) 0.2063(3) 1.2741(2) 0.0493(12) Uani 1 1 d . . . . . H4S H 0.571019 0.185308 1.274209 0.074 Uiso 1 1 calc R U . . . N31 N 0.60442(14) 0.1671(3) 1.0622(2) 0.0186(9) Uani 1 1 d . . . . . N11 N 0.64317(14) 0.0719(3) 0.92629(19) 0.0168(9) Uani 1 1 d . . . . . C25 C 0.6476(2) 0.4178(3) 0.7463(3) 0.0281(12) Uani 1 1 d . . . . . H25A H 0.623212 0.462932 0.749660 0.042 Uiso 1 1 calc R U . . . H25B H 0.681934 0.440364 0.754379 0.042 Uiso 1 1 calc R U . . . H25C H 0.642204 0.392953 0.700758 0.042 Uiso 1 1 calc R U . . . C33 C 0.4530(2) 0.3283(5) 1.0850(3) 0.056(2) Uani 1 1 d . . . . . H33A H 0.427668 0.339692 1.113593 0.068 Uiso 1 1 calc R U . . . C35 C 0.48761(19) 0.3487(4) 0.9802(3) 0.0281(13) Uani 1 1 d . . . . . O71 O 0.54993(13) 0.2873(2) 0.73142(18) 0.0243(8) Uani 1 1 d . . . . . C16 C 0.65823(17) 0.2187(3) 0.8382(2) 0.0146(10) Uani 1 1 d . . . . . C36 C 0.52779(18) 0.2924(3) 0.9999(3) 0.0230(11) Uani 1 1 d . . . . . C51 C 0.54088(18) 0.2223(3) 0.6962(2) 0.0194(11) Uani 1 1 d . . . . . C13 C 0.7448(2) 0.2078(3) 0.7705(3) 0.0258(12) Uani 1 1 d . . . . . H13A H 0.774243 0.203853 0.747896 0.031 Uiso 1 1 calc R U . . . C12 C 0.73115(19) 0.1419(3) 0.8091(3) 0.0232(11) Uani 1 1 d . . . . . H12 H 0.750973 0.092425 0.811923 0.028 Uiso 1 1 calc R U . . . C42 C 0.72965(18) 0.0751(3) 1.1208(3) 0.0209(11) Uani 1 1 d . . . . . H42 H 0.763848 0.080973 1.112709 0.025 Uiso 1 1 calc R U . . . C17 C 0.67570(17) 0.0729(3) 0.8826(2) 0.0183(10) Uani 1 1 d . . . . . H17 H 0.692526 0.021963 0.874915 0.022 Uiso 1 1 calc R U . . . C11 C 0.68834(18) 0.1461(3) 0.8445(2) 0.0167(10) Uani 1 1 d . . . . . C41 C 0.71690(19) 0.0135(3) 1.1654(3) 0.0261(12) Uani 1 1 d . . . . . H41 H 0.742255 -0.022308 1.187214 0.031 Uiso 1 1 calc R U . . . C14 C 0.71550(19) 0.2806(3) 0.7645(2) 0.0223(11) Uani 1 1 d . . . . . H14 H 0.724623 0.326104 0.737556 0.027 Uiso 1 1 calc R U . . . C15 C 0.67326(18) 0.2855(3) 0.7981(2) 0.0180(10) Uani 1 1 d . . . . . C38 C 0.64313(18) 0.1173(3) 1.0994(2) 0.0205(11) Uani 1 1 d . . . . . C37 C 0.57034(19) 0.2008(4) 1.0943(3) 0.0255(12) Uani 1 1 d . . . . . H37 H 0.571802 0.189138 1.141537 0.031 Uiso 1 1 calc R U . . . C4S C 0.6356(3) 0.1576(5) 1.3160(4) 0.066(2) Uani 1 1 d . . . . . H4SA H 0.669774 0.177169 1.310738 0.100 Uiso 1 1 calc R U . . . H4SB H 0.632285 0.098725 1.302497 0.100 Uiso 1 1 calc R U . . . H4SC H 0.629559 0.163466 1.363609 0.100 Uiso 1 1 calc R U . . . C24 C 0.5399(2) 0.0204(4) 0.9159(3) 0.0336(14) Uani 1 1 d . . . . . H24A H 0.544862 0.018672 0.867163 0.040 Uiso 1 1 calc R U . . . H24B H 0.506983 -0.006068 0.920933 0.040 Uiso 1 1 calc R U . . . C43 C 0.69312(18) 0.1290(3) 1.0876(2) 0.0196(11) Uani 1 1 d . . . . . C19 C 0.6707(2) -0.0543(3) 0.9910(3) 0.0260(12) Uani 1 1 d . . . . . H19 H 0.704931 -0.037456 0.992132 0.031 Uiso 1 1 calc R U . . . C44 C 0.71303(19) 0.1958(4) 1.0449(3) 0.0275(12) Uani 1 1 d D . . . . H44A H 0.730191 0.238418 1.075725 0.033 Uiso 1 1 calc R U . . . H44B H 0.738920 0.170369 1.019385 0.033 Uiso 1 1 calc R U . . . C39 C 0.6305(2) 0.0555(4) 1.1438(3) 0.0265(12) Uani 1 1 d . . . . . H39 H 0.596180 0.048083 1.150994 0.032 Uiso 1 1 calc R U . . . C18 C 0.63235(19) -0.0055(3) 0.9578(3) 0.0219(11) Uani 1 1 d . . . . . C23 C 0.5814(2) -0.0281(3) 0.9565(3) 0.0274(12) Uani 1 1 d . . . . . C20 C 0.6585(2) -0.1281(4) 1.0225(3) 0.0370(15) Uani 1 1 d . . . . . H20 H 0.684474 -0.162177 1.044983 0.044 Uiso 1 1 calc R U . . . C31 C 0.52970(19) 0.2552(4) 1.0648(3) 0.0283(13) Uani 1 1 d . . . . . C40 C 0.6675(2) 0.0043(4) 1.1779(3) 0.0286(13) Uani 1 1 d . . . . . H40 H 0.658728 -0.036545 1.209335 0.034 Uiso 1 1 calc R U . . . C34 C 0.4508(2) 0.3659(5) 1.0213(3) 0.0458(18) Uani 1 1 d . . . . . H34 H 0.424004 0.403098 1.006389 0.055 Uiso 1 1 calc R U . . . C3S C 0.6855(3) 0.6098(4) 0.9129(4) 0.0494(18) Uani 1 1 d . . . . . H3SA H 0.693790 0.581672 0.956801 0.074 Uiso 1 1 calc R U . . . H3SB H 0.665859 0.660404 0.919262 0.074 Uiso 1 1 calc R U . . . H3SC H 0.716702 0.625060 0.894375 0.074 Uiso 1 1 calc R U . . . C22 C 0.5703(2) -0.1033(4) 0.9887(3) 0.0399(16) Uani 1 1 d . . . . . H22 H 0.536269 -0.120807 0.988163 0.048 Uiso 1 1 calc R U . . . C21 C 0.6090(3) -0.1518(4) 1.0213(3) 0.0447(17) Uani 1 1 d . . . . . H21 H 0.601020 -0.202284 1.043110 0.054 Uiso 1 1 calc R U . . . C32 C 0.4919(2) 0.2746(5) 1.1067(3) 0.0473(19) Uani 1 1 d . . . . . H32 H 0.493428 0.250098 1.150650 0.057 Uiso 1 1 calc R U . . . C45 C 0.4531(3) 0.4495(5) 0.8978(4) 0.063(2) Uani 1 1 d . . . . . H45A H 0.456672 0.469420 0.851830 0.094 Uiso 1 1 calc R U . . . H45B H 0.418753 0.428594 0.899379 0.094 Uiso 1 1 calc R U . . . H45C H 0.459745 0.495658 0.930199 0.094 Uiso 1 1 calc R U . . . O54 O 0.49985(13) 0.2161(2) 0.65597(17) 0.0254(8) Uani 1 1 d . . . . . C61 C 0.500000 0.4882(4) 0.750000 0.0235(16) Uani 1 2 d S T P . . C62 C 0.500000 0.5826(5) 0.750000 0.050(3) Uani 1 2 d S T P . . H62A H 0.527295 0.603039 0.783350 0.075 Uiso 0.5 1 calc R U P A -1 H62B H 0.505128 0.603039 0.704664 0.075 Uiso 0.5 1 calc R U P A -1 H62C H 0.467577 0.603039 0.761985 0.075 Uiso 0.5 1 calc R U P A -1 C2S C 0.7306(4) 0.6761(5) 1.0918(4) 0.073(3) Uani 1 1 d . . . . . H2SA H 0.707197 0.709784 1.115118 0.109 Uiso 1 1 calc R U . . . H2SB H 0.714283 0.660012 1.046762 0.109 Uiso 1 1 calc R U . . . H2SC H 0.760971 0.708850 1.086915 0.109 Uiso 1 1 calc R U . . . N3 N 0.500000 0.0707(5) 1.250000 0.0426(19) Uani 1 2 d S T P . . O2 O 0.5403(2) 0.0338(3) 1.2490(3) 0.088(2) Uani 1 1 d . . . . . O3 O 0.500000 0.1480(5) 1.250000 0.082(3) Uani 1 2 d S T P . . N1 N 0.6753(4) 0.4476(7) 1.0511(8) 0.026(3) Uani 0.508(10) 1 d D U P B 1 O1 O 0.6429(3) 0.3885(5) 1.0367(5) 0.034(2) Uani 0.508(10) 1 d D U P B 1 O4 O 0.7196(3) 0.4336(6) 1.0460(5) 0.050(3) Uani 0.508(10) 1 d D U P B 1 O5 O 0.6631(4) 0.5145(6) 1.0716(8) 0.068(4) Uani 0.508(10) 1 d D U P B 1 O4A O 0.6815(8) 0.4360(13) 1.0267(7) 0.092(7) Uani 0.492(10) 1 d D U P B 2 N1A N 0.6642(5) 0.4256(7) 1.0817(6) 0.034(3) Uani 0.492(10) 1 d D U P B 2 O5A O 0.6657(3) 0.4786(6) 1.1257(6) 0.047(3) Uani 0.492(10) 1 d D U P B 2 O1A O 0.6462(4) 0.3545(6) 1.0925(6) 0.059(4) Uani 0.492(10) 1 d D U P B 2 O6 O 0.6294(2) 0.6394(3) 0.7531(2) 0.0542(13) Uani 1 1 d . . . . . H6 H 0.619048 0.687258 0.762239 0.081 Uiso 1 1 calc R U . . . C1 C 0.6307(5) 0.6335(8) 0.6927(6) 0.120(4) Uani 1 1 d . U . . . H1A H 0.596265 0.632227 0.669307 0.180 Uiso 1 1 calc R U . . . H1B H 0.648311 0.581895 0.682840 0.180 Uiso 1 1 calc R U . . . H1C H 0.648742 0.681733 0.676666 0.180 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 Ho1 0.01675(13) 0.01560(13) 0.02278(13) -0.00094(10) 0.00372(9) 0.00247(10) Co1 0.0148(3) 0.0157(3) 0.0190(3) -0.0008(3) 0.0058(2) -0.0006(3) O11 0.0138(17) 0.0183(18) 0.0213(18) 0.0000(14) 0.0043(13) 0.0023(14) C52 0.028(3) 0.031(3) 0.038(3) -0.010(3) -0.004(2) 0.010(3) O31 0.0173(18) 0.025(2) 0.0235(19) -0.0051(15) 0.0064(14) 0.0031(15) O61 0.025(2) 0.0160(19) 0.037(2) 0.0007(16) -0.0014(16) 0.0079(16) O12 0.0202(18) 0.0133(18) 0.030(2) 0.0041(15) 0.0084(14) 0.0002(14) O32 0.021(2) 0.038(2) 0.032(2) -0.0020(18) 0.0048(16) 0.0122(17) O33 0.0185(18) 0.0158(18) 0.0253(19) 0.0012(15) 0.0027(14) -0.0038(14) O1W 0.038(2) 0.021(2) 0.032(2) -0.0009(17) -0.0012(17) -0.0030(17) O13 0.0169(19) 0.024(2) 0.028(2) -0.0003(16) 0.0011(14) -0.0038(15) O3S 0.042(3) 0.027(2) 0.053(3) 0.001(2) -0.004(2) -0.009(2) O2S 0.061(3) 0.041(3) 0.064(3) -0.001(3) 0.009(3) 0.004(2) O4S 0.055(3) 0.050(3) 0.043(3) 0.009(2) 0.007(2) -0.001(2) N31 0.016(2) 0.021(2) 0.020(2) -0.0005(18) 0.0049(16) -0.0044(18) N11 0.013(2) 0.016(2) 0.021(2) -0.0003(17) 0.0035(16) -0.0034(17) C25 0.027(3) 0.018(3) 0.039(3) 0.012(2) 0.004(2) 0.000(2) C33 0.033(4) 0.104(7) 0.035(4) -0.006(4) 0.014(3) 0.031(4) C35 0.021(3) 0.040(4) 0.023(3) -0.008(2) 0.001(2) 0.004(2) O71 0.028(2) 0.0180(19) 0.029(2) -0.0015(16) 0.0107(15) -0.0032(16) C16 0.011(2) 0.018(3) 0.016(2) -0.0041(19) 0.0018(18) -0.0016(19) C36 0.017(3) 0.028(3) 0.026(3) -0.011(2) 0.006(2) -0.002(2) C51 0.015(3) 0.021(3) 0.024(3) 0.001(2) 0.007(2) -0.001(2) C13 0.023(3) 0.027(3) 0.031(3) 0.001(2) 0.016(2) 0.000(2) C12 0.020(3) 0.021(3) 0.029(3) -0.002(2) 0.008(2) 0.003(2) C42 0.013(2) 0.021(3) 0.030(3) -0.001(2) 0.008(2) -0.005(2) C17 0.015(2) 0.017(3) 0.023(3) -0.004(2) 0.0032(19) 0.001(2) C11 0.017(2) 0.014(3) 0.019(2) -0.003(2) 0.0049(19) -0.0011(19) C41 0.024(3) 0.021(3) 0.032(3) 0.001(2) -0.003(2) -0.001(2) C14 0.024(3) 0.023(3) 0.021(3) 0.001(2) 0.008(2) -0.004(2) C15 0.018(3) 0.014(3) 0.022(3) -0.001(2) 0.0007(19) -0.002(2) C38 0.020(3) 0.024(3) 0.017(2) -0.003(2) 0.0012(19) -0.004(2) C37 0.023(3) 0.037(3) 0.018(3) 0.000(2) 0.006(2) -0.005(2) C4S 0.090(6) 0.059(5) 0.051(5) 0.015(4) 0.009(4) 0.021(5) C24 0.025(3) 0.027(3) 0.050(4) -0.009(3) 0.009(3) -0.012(2) C43 0.021(3) 0.018(3) 0.019(3) -0.003(2) 0.004(2) -0.003(2) C19 0.033(3) 0.019(3) 0.027(3) -0.001(2) 0.010(2) 0.001(2) C44 0.023(3) 0.030(3) 0.030(3) 0.010(2) 0.001(2) -0.003(2) C39 0.022(3) 0.033(3) 0.026(3) 0.002(2) 0.005(2) -0.011(2) C18 0.026(3) 0.014(3) 0.028(3) -0.003(2) 0.013(2) -0.002(2) C23 0.032(3) 0.019(3) 0.032(3) -0.004(2) 0.013(2) -0.004(2) C20 0.056(4) 0.020(3) 0.036(3) 0.006(3) 0.009(3) 0.005(3) C31 0.018(3) 0.044(4) 0.023(3) -0.006(3) 0.005(2) 0.005(2) C40 0.032(3) 0.029(3) 0.025(3) 0.009(2) 0.003(2) -0.013(3) C34 0.030(3) 0.079(5) 0.029(3) -0.008(3) 0.002(3) 0.027(3) C3S 0.045(4) 0.039(4) 0.062(5) -0.008(3) 0.001(3) -0.009(3) C22 0.043(4) 0.023(3) 0.059(4) 0.001(3) 0.029(3) -0.014(3) C21 0.067(5) 0.018(3) 0.054(4) 0.005(3) 0.028(3) -0.012(3) C32 0.032(3) 0.085(6) 0.027(3) 0.000(3) 0.014(3) 0.025(4) C45 0.056(5) 0.071(6) 0.066(5) 0.027(4) 0.028(4) 0.052(4) O54 0.0200(19) 0.030(2) 0.0260(19) -0.0024(16) 0.0005(15) 0.0058(16) C61 0.023(4) 0.007(3) 0.041(4) 0.000 0.004(3) 0.000 C62 0.046(6) 0.015(4) 0.082(7) 0.000 -0.021(5) 0.000 C2S 0.123(8) 0.044(5) 0.054(5) 0.009(4) 0.017(5) 0.017(5) N3 0.068(6) 0.040(5) 0.022(4) 0.000 0.018(4) 0.000 O2 0.118(5) 0.051(4) 0.113(5) 0.030(3) 0.088(4) 0.039(4) O3 0.054(5) 0.030(4) 0.155(9) 0.000 -0.017(5) 0.000 N1 0.018(4) 0.019(5) 0.040(9) -0.007(5) 0.003(5) -0.002(3) O1 0.032(4) 0.022(4) 0.046(6) -0.006(4) -0.004(4) -0.007(3) O4 0.020(4) 0.052(6) 0.079(7) -0.005(5) 0.006(4) 0.005(4) O5 0.063(7) 0.028(5) 0.119(11) -0.029(6) 0.037(7) -0.005(4) O4A 0.104(15) 0.131(15) 0.043(8) 0.016(8) 0.018(8) 0.016(11) N1A 0.039(7) 0.028(5) 0.032(6) -0.009(4) -0.012(5) 0.011(4) O5A 0.042(5) 0.034(5) 0.061(6) -0.026(5) -0.007(5) 0.008(4) O1A 0.057(7) 0.035(5) 0.087(9) -0.018(5) 0.011(6) -0.005(4) O6 0.060(3) 0.054(3) 0.049(3) 0.015(2) 0.011(2) 0.005(3) C1 0.120(4) 0.119(5) 0.122(4) 0.000(2) 0.013(2) 0.000(2) 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' Ho Ho -0.2175 4.6783 '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' 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 O11 Ho1 O31 67.33(11) . . ? O11 Ho1 O12 63.64(11) . . ? O11 Ho1 O32 130.93(12) . . ? O11 Ho1 O1W 96.23(12) . . ? O11 Ho1 O71 86.40(12) . . ? O11 Ho1 O54 82.72(12) . 2_656 ? O31 Ho1 O12 116.01(11) . . ? O31 Ho1 O32 64.22(11) . . ? O31 Ho1 O1W 74.28(13) . . ? O31 Ho1 O71 143.07(12) . . ? O31 Ho1 O54 73.49(12) . 2_656 ? O61 Ho1 O11 147.59(12) . . ? O61 Ho1 O31 136.67(12) . . ? O61 Ho1 O12 84.15(12) . . ? O61 Ho1 O32 79.08(13) . . ? O61 Ho1 O1W 76.37(13) . . ? O61 Ho1 O71 78.68(13) . . ? O61 Ho1 O54 121.16(13) . 2_656 ? O32 Ho1 O12 149.20(12) . . ? O1W Ho1 O12 72.94(12) . . ? O1W Ho1 O32 78.08(13) . . ? O1W Ho1 O54 145.39(13) . 2_656 ? O71 Ho1 O12 69.69(11) . . ? O71 Ho1 O32 130.54(12) . . ? O71 Ho1 O1W 136.62(13) . . ? O71 Ho1 O54 77.96(12) . 2_656 ? O54 Ho1 O12 133.82(12) 2_656 . ? O54 Ho1 O32 76.87(13) 2_656 . ? O11 Co1 O31 77.24(13) . . ? O11 Co1 O33 87.36(13) . . ? O11 Co1 O13 102.29(13) . . ? O11 Co1 N31 160.16(16) . . ? O11 Co1 N11 86.73(14) . . ? O31 Co1 O33 97.17(14) . . ? O31 Co1 O13 86.02(14) . . ? O31 Co1 N11 159.96(14) . . ? O13 Co1 O33 170.31(13) . . ? N31 Co1 O31 89.43(15) . . ? N31 Co1 O33 79.72(14) . . ? N31 Co1 O13 91.20(14) . . ? N31 Co1 N11 108.97(16) . . ? N11 Co1 O33 93.98(14) . . ? N11 Co1 O13 85.73(15) . . ? Co1 O11 Ho1 108.13(13) . . ? C16 O11 Ho1 127.7(3) . . ? C16 O11 Co1 121.0(3) . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? Co1 O31 Ho1 105.56(13) . . ? C36 O31 Ho1 125.9(3) . . ? C36 O31 Co1 123.1(3) . . ? C61 O61 Ho1 146.7(4) . . ? C25 O12 Ho1 122.8(3) . . ? C15 O12 Ho1 116.1(3) . . ? C15 O12 C25 116.2(4) . . ? C35 O32 Ho1 117.7(3) . . ? C35 O32 C45 115.4(4) . . ? C45 O32 Ho1 126.7(3) . . ? Co1 O33 H33 121.9(17) . . ? C44 O33 Co1 120.0(3) . . ? C44 O33 H33 104.2(16) . . ? Ho1 O1W H1WA 110.4 . . ? Ho1 O1W H1WB 110.7 . . ? H1WA O1W H1WB 103.3 . . ? Co1 O13 H13 103.7 . . ? C24 O13 Co1 121.2(3) . . ? C24 O13 H13 109.5 . . ? C3S O3S H3S 109.5 . . ? C2S O2S H2S 109.5 . . ? C4S O4S H4S 109.5 . . ? C38 N31 Co1 116.0(3) . . ? C37 N31 Co1 124.9(4) . . ? C37 N31 C38 119.1(4) . . ? C17 N11 Co1 124.7(3) . . ? C17 N11 C18 119.1(4) . . ? C18 N11 Co1 116.1(3) . . ? O12 C25 H25A 109.5 . . ? O12 C25 H25B 109.5 . . ? O12 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C32 C33 C34 120.2(5) . . ? O32 C35 C36 113.8(4) . . ? C34 C35 O32 123.9(5) . . ? C34 C35 C36 122.2(5) . . ? C51 O71 Ho1 139.7(3) . . ? O11 C16 C11 124.1(4) . . ? O11 C16 C15 117.5(4) . . ? C11 C16 C15 118.3(4) . . ? O31 C36 C35 117.6(5) . . ? O31 C36 C31 124.8(5) . . ? C31 C36 C35 117.5(4) . . ? O71 C51 C52 120.6(5) . . ? O71 C51 O54 120.3(5) . . ? O54 C51 C52 119.2(5) . . ? C12 C13 H13A 120.0 . . ? C12 C13 C14 120.0(5) . . ? C14 C13 H13A 120.0 . . ? C13 C12 H12 119.2 . . ? C13 C12 C11 121.6(5) . . ? C11 C12 H12 119.2 . . ? C41 C42 H42 119.2 . . ? C41 C42 C43 121.5(5) . . ? C43 C42 H42 119.2 . . ? N11 C17 H17 117.6 . . ? N11 C17 C11 124.8(4) . . ? C11 C17 H17 117.6 . . ? C16 C11 C12 118.8(4) . . ? C16 C11 C17 123.0(4) . . ? C12 C11 C17 118.1(4) . . ? C42 C41 H41 120.0 . . ? C40 C41 C42 120.0(5) . . ? C40 C41 H41 120.0 . . ? C13 C14 H14 120.4 . . ? C15 C14 C13 119.2(5) . . ? C15 C14 H14 120.4 . . ? O12 C15 C16 113.0(4) . . ? C14 C15 O12 125.0(4) . . ? C14 C15 C16 122.0(5) . . ? C43 C38 N31 119.1(4) . . ? C39 C38 N31 120.2(4) . . ? C39 C38 C43 120.6(5) . . ? N31 C37 H37 117.0 . . ? N31 C37 C31 126.0(5) . . ? C31 C37 H37 117.0 . . ? O4S C4S H4SA 109.5 . . ? O4S C4S H4SB 109.5 . . ? O4S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? O13 C24 H24A 109.4 . . ? O13 C24 H24B 109.4 . . ? O13 C24 C23 111.3(4) . . ? H24A C24 H24B 108.0 . . ? C23 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C42 C43 C44 115.4(4) . . ? C38 C43 C42 117.7(5) . . ? C38 C43 C44 126.9(5) . . ? C18 C19 H19 120.3 . . ? C18 C19 C20 119.3(5) . . ? C20 C19 H19 120.3 . . ? O33 C44 C43 116.8(4) . . ? O33 C44 H44A 108.1 . . ? O33 C44 H44B 108.1 . . ? C43 C44 H44A 108.1 . . ? C43 C44 H44B 108.1 . . ? H44A C44 H44B 107.3 . . ? C38 C39 H39 119.6 . . ? C38 C39 C40 120.8(5) . . ? C40 C39 H39 119.6 . . ? C19 C18 N11 121.1(4) . . ? C19 C18 C23 121.5(5) . . ? C23 C18 N11 117.4(5) . . ? C18 C23 C24 121.8(5) . . ? C18 C23 C22 117.7(5) . . ? C22 C23 C24 120.1(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 C19 120.2(6) . . ? C21 C20 H20 119.9 . . ? C36 C31 C37 124.2(4) . . ? C36 C31 C32 119.4(5) . . ? C32 C31 C37 116.3(5) . . ? C41 C40 C39 119.3(5) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C33 C34 H34 120.3 . . ? C35 C34 C33 119.5(6) . . ? C35 C34 H34 120.3 . . ? O3S C3S H3SA 109.5 . . ? O3S C3S H3SB 109.5 . . ? O3S C3S H3SC 109.5 . . ? H3SA C3S H3SB 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? C23 C22 H22 119.9 . . ? C21 C22 C23 120.3(6) . . ? C21 C22 H22 119.9 . . ? C20 C21 C22 121.0(6) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C33 C32 C31 121.1(6) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? O32 C45 H45A 109.5 . . ? O32 C45 H45B 109.5 . . ? O32 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 O54 Ho1 116.1(3) . 2_656 ? O61 C61 O61 123.6(7) 2_656 . ? O61 C61 C62 118.2(3) 2_656 . ? O61 C61 C62 118.2(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O2S C2S H2SA 109.5 . . ? O2S C2S H2SB 109.5 . . ? O2S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O2 N3 O2 122.7(9) 2_657 . ? O2 N3 O3 118.6(5) 2_657 . ? O2 N3 O3 118.6(5) . . ? O4 N1 O1 118.6(10) . . ? O5 N1 O1 121.7(12) . . ? O5 N1 O4 119.7(11) . . ? O4A N1A O1A 117.2(14) . . ? O5A N1A O4A 123.5(17) . . ? O5A N1A O1A 119.3(13) . . ? C1 O6 H6 109.5 . . ? O6 C1 H1A 109.5 . . ? O6 C1 H1B 109.5 . . ? O6 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? 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 Ho1 O11 2.281(3) . ? Ho1 O31 2.337(3) . ? Ho1 O61 2.266(4) . ? Ho1 O12 2.592(3) . ? Ho1 O32 2.546(3) . ? Ho1 O1W 2.345(4) . ? Ho1 O71 2.340(3) . ? Ho1 O54 2.356(4) 2_656 ? Co1 O11 2.044(3) . ? Co1 O31 2.059(3) . ? Co1 O33 2.150(3) . ? Co1 O13 2.144(3) . ? Co1 N31 2.058(4) . ? Co1 N11 2.068(4) . ? O11 C16 1.337(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C52 C51 1.475(7) . ? O31 C36 1.331(6) . ? O61 C61 1.260(5) . ? O12 C25 1.447(6) . ? O12 C15 1.394(6) . ? O32 C35 1.396(6) . ? O32 C45 1.441(7) . ? O33 H33 0.888(10) . ? O33 C44 1.438(6) . ? O1W H1WA 0.8948 . ? O1W H1WB 0.8951 . ? O13 H13 0.8400 . ? O13 C24 1.440(6) . ? O3S H3S 0.8400 . ? O3S C3S 1.425(7) . ? O2S H2S 0.8400 . ? O2S C2S 1.414(8) . ? O4S H4S 0.8400 . ? O4S C4S 1.421(8) . ? N31 C38 1.436(6) . ? N31 C37 1.288(6) . ? N11 C17 1.296(6) . ? N11 C18 1.430(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C33 H33A 0.9500 . ? C33 C34 1.392(9) . ? C33 C32 1.376(9) . ? C35 C36 1.419(7) . ? C35 C34 1.377(7) . ? O71 C51 1.258(6) . ? C16 C11 1.408(7) . ? C16 C15 1.417(7) . ? C36 C31 1.411(7) . ? C51 O54 1.280(6) . ? C13 H13A 0.9500 . ? C13 C12 1.375(7) . ? C13 C14 1.400(7) . ? C12 H12 0.9500 . ? C12 C11 1.411(6) . ? C42 H42 0.9500 . ? C42 C41 1.392(7) . ? C42 C43 1.405(7) . ? C17 H17 0.9500 . ? C17 C11 1.454(7) . ? C41 H41 0.9500 . ? C41 C40 1.378(7) . ? C14 H14 0.9500 . ? C14 C15 1.377(7) . ? C38 C43 1.394(7) . ? C38 C39 1.391(7) . ? C37 H37 0.9500 . ? C37 C31 1.458(7) . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C23 1.505(8) . ? C43 C44 1.499(7) . ? C19 H19 0.9500 . ? C19 C18 1.389(7) . ? C19 C20 1.392(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C39 H39 0.9500 . ? C39 C40 1.395(8) . ? C18 C23 1.406(7) . ? C23 C22 1.407(8) . ? C20 H20 0.9500 . ? C20 C21 1.372(9) . ? C31 C32 1.414(7) . ? C40 H40 0.9500 . ? C34 H34 0.9500 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C22 H22 0.9500 . ? C22 C21 1.388(9) . ? C21 H21 0.9500 . ? C32 H32 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C61 C62 1.508(10) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? N3 O2 1.229(6) 2_657 ? N3 O2 1.229(6) . ? N3 O3 1.236(10) . ? N1 O1 1.290(14) . ? N1 O4 1.220(14) . ? N1 O5 1.201(12) . ? O4A N1A 1.243(16) . ? N1A O5A 1.212(11) . ? N1A O1A 1.260(14) . ? O6 H6 0.8400 . ? O6 C1 1.206(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? 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 Ho1 O11 C16 C11 -167.7(3) . . . . ? Ho1 O11 C16 C15 10.7(6) . . . . ? Ho1 O31 C36 C35 -8.6(6) . . . . ? Ho1 O31 C36 C31 173.7(4) . . . . ? Ho1 O61 C61 O61 -19.3(4) . . . 2_656 ? Ho1 O61 C61 C62 160.7(4) . . . . ? Ho1 O12 C15 C16 -11.8(5) . . . . ? Ho1 O12 C15 C14 167.9(4) . . . . ? Ho1 O32 C35 C36 4.7(6) . . . . ? Ho1 O32 C35 C34 -174.2(5) . . . . ? Ho1 O71 C51 C52 -69.7(7) . . . . ? Ho1 O71 C51 O54 110.4(5) . . . . ? Co1 O11 C16 C11 34.9(6) . . . . ? Co1 O11 C16 C15 -146.6(3) . . . . ? Co1 O31 C36 C35 -158.8(4) . . . . ? Co1 O31 C36 C31 23.5(7) . . . . ? Co1 O33 C44 C43 -24.9(6) . . . . ? Co1 O13 C24 C23 43.6(6) . . . . ? Co1 N31 C38 C43 46.6(6) . . . . ? Co1 N31 C38 C39 -130.1(4) . . . . ? Co1 N31 C37 C31 -3.6(8) . . . . ? Co1 N11 C17 C11 -6.8(7) . . . . ? Co1 N11 C18 C19 -123.0(4) . . . . ? Co1 N11 C18 C23 54.1(5) . . . . ? O11 C16 C11 C12 176.5(4) . . . . ? O11 C16 C11 C17 0.4(7) . . . . ? O11 C16 C15 O12 2.5(6) . . . . ? O11 C16 C15 C14 -177.3(4) . . . . ? C52 C51 O54 Ho1 178.8(4) . . . 2_656 ? O31 C36 C31 C37 2.1(9) . . . . ? O31 C36 C31 C32 178.3(5) . . . . ? O32 C35 C36 O31 1.8(7) . . . . ? O32 C35 C36 C31 179.6(5) . . . . ? O32 C35 C34 C33 179.9(6) . . . . ? O13 C24 C23 C18 -60.2(7) . . . . ? O13 C24 C23 C22 126.6(5) . . . . ? N31 C38 C43 C42 -175.3(4) . . . . ? N31 C38 C43 C44 7.3(8) . . . . ? N31 C38 C39 C40 177.1(5) . . . . ? N31 C37 C31 C36 -13.4(9) . . . . ? N31 C37 C31 C32 170.3(6) . . . . ? N11 C17 C11 C16 -16.1(8) . . . . ? N11 C17 C11 C12 167.8(5) . . . . ? N11 C18 C23 C24 8.0(7) . . . . ? N11 C18 C23 C22 -178.6(5) . . . . ? C25 O12 C15 C16 -167.8(4) . . . . ? C25 O12 C15 C14 11.9(7) . . . . ? C35 C36 C31 C37 -175.6(5) . . . . ? C35 C36 C31 C32 0.5(8) . . . . ? O71 C51 O54 Ho1 -1.2(6) . . . 2_656 ? C36 C35 C34 C33 1.1(10) . . . . ? C36 C31 C32 C33 0.8(10) . . . . ? C13 C12 C11 C16 2.1(7) . . . . ? C13 C12 C11 C17 178.3(5) . . . . ? C13 C14 C15 O12 179.7(5) . . . . ? C13 C14 C15 C16 -0.6(7) . . . . ? C12 C13 C14 C15 0.6(8) . . . . ? C42 C41 C40 C39 2.0(8) . . . . ? C42 C43 C44 O33 164.5(4) . . . . ? C17 N11 C18 C19 53.6(7) . . . . ? C17 N11 C18 C23 -129.2(5) . . . . ? C11 C16 C15 O12 -179.0(4) . . . . ? C11 C16 C15 C14 1.3(7) . . . . ? C41 C42 C43 C38 -1.6(7) . . . . ? C41 C42 C43 C44 176.1(5) . . . . ? C14 C13 C12 C11 -1.4(8) . . . . ? C15 C16 C11 C12 -2.0(7) . . . . ? C15 C16 C11 C17 -178.0(4) . . . . ? C38 N31 C37 C31 177.7(5) . . . . ? C38 C43 C44 O33 -18.0(8) . . . . ? C38 C39 C40 C41 -2.2(8) . . . . ? C37 N31 C38 C43 -134.6(5) . . . . ? C37 N31 C38 C39 48.7(7) . . . . ? C37 C31 C32 C33 177.2(7) . . . . ? C24 C23 C22 C21 174.5(6) . . . . ? C43 C42 C41 C40 -0.1(8) . . . . ? C43 C38 C39 C40 0.4(8) . . . . ? C19 C18 C23 C24 -174.8(5) . . . . ? C19 C18 C23 C22 -1.5(8) . . . . ? C19 C20 C21 C22 0.2(9) . . . . ? C39 C38 C43 C42 1.5(7) . . . . ? C39 C38 C43 C44 -176.0(5) . . . . ? C18 N11 C17 C11 176.8(4) . . . . ? C18 C19 C20 C21 -0.6(8) . . . . ? C18 C23 C22 C21 1.0(9) . . . . ? C23 C22 C21 C20 -0.4(10) . . . . ? C20 C19 C18 N11 178.3(5) . . . . ? C20 C19 C18 C23 1.3(8) . . . . ? C34 C33 C32 C31 -1.2(12) . . . . ? C34 C35 C36 O31 -179.4(5) . . . . ? C34 C35 C36 C31 -1.5(8) . . . . ? C32 C33 C34 C35 0.2(12) . . . . ? C45 O32 C35 C36 -171.1(6) . . . . ? C45 O32 C35 C34 10.0(9) . . . . ?