#------------------------------------------------------------------------------ #$Date: 2023-11-02 01:43:29 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287232 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247648.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_7247648 loop_ _publ_author_name 'Ovcharenko, Victor' 'Fursova, Elena' 'Letyagin, Gleb' 'Morozov, Vitaly' 'Bogomyakov, Artem' 'Romanenko, Galina' _publ_section_title ; Alternating [ML2(MeOH)2] and [ML2(EtOH)2] layers in low-temperature ferromagnets [ML2(MeOH)2][ML2(EtOH)2] (M = CoII, NiII or CoII0.5NiII0.5) ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00912B _journal_year 2023 _chemical_formula_sum 'C23 H36 Co0.5 F6 N4 Ni0.5 O6' _chemical_formula_weight 637.38 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_block_doi 10.5517/ccdc.csd.cc2bjd4f _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2022-03-22 deposited with the CCDC. 2023-10-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 120.036(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.333(4) _cell_length_b 15.836(3) _cell_length_c 11.701(2) _cell_measurement_reflns_used 2665 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 20.98 _cell_measurement_theta_min 2.39 _cell_volume 2940.9(10) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1127 _diffrn_reflns_av_unetI/netI 0.1503 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 27870 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.494 _diffrn_reflns_theta_min 2.182 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_T_max 0.2917 _exptl_absorpt_correction_T_min 0.2479 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour light_brown _exptl_crystal_density_diffrn 1.440 _exptl_crystal_description block _exptl_crystal_F_000 1326 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.402 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 410 _refine_ls_number_reflns 7261 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.838 _refine_ls_R_factor_all 0.1951 _refine_ls_R_factor_gt 0.0592 _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^)+(0.0890P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1539 _refine_ls_wR_factor_ref 0.1958 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2475 _reflns_number_total 7261 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00912b1.cif _cod_data_source_block z44s _cod_original_cell_volume 2940.8(10) _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C23 H36 Co0.50 F6 N4 Ni0.50 O6' _cod_database_code 7247648 _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_res_file ; TITL z44s_a.res in P2(1)/c z44s.res created by SHELXL-2018/3 at 15:14:01 on 27-Jan-2021 REM Old TITL z44s in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.263, Rweak 0.009, Alpha 0.095 REM 0.200 for 220 systematic absences, Orientation as input REM Formula found by SHELXT: C28 N3 O6 F4 Ni CELL 0.71073 18.3329 15.8363 11.7006 90.000 120.036 90.000 ZERR 4.000 0.0036 0.0028 0.0022 0.000 0.008 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O F CO NI UNIT 92 144 16 24 24 2 2 TEMP 23.000 omit 1 1 0 omit -6 0 2 omit -4 7 4 omit 0 6 1 omit -1 2 1 omit -2 4 3 omit -8 3 4 omit -6 7 1 omit -6 3 4 acta htab EQIV $1 x, -y+1/2, z-1/2 eqiv $2 x, -y+3/2, z+1/2 HTAB O21S O13B_$1 HTAB O11S O13x_$2 HTAB O11S O13a_$2 L.S. 20 BOND LIST 4 FMAP 2 exyz ni1 co1 eadp ni1 co1 exyz ni2 co2 eadp ni2 co2 htab PLAN 20 dfix 1. 0.02 o11s h11s o21s h21s WGHT 0.088958 FVAR 0.22581 0.48486 NI1 7 0.500000 0.500000 0.000000 10.25000 0.04125 0.03068 = 0.03655 0.00102 0.01400 -0.00114 CO1 6 0.500000 0.500000 0.000000 10.25000 0.04125 0.03068 = 0.03655 0.00102 0.01400 -0.00114 O1A 4 0.617676 0.520564 0.148643 11.00000 0.04974 0.04580 = 0.04605 0.00574 0.01188 -0.00519 C2A 1 0.666034 0.583654 0.168446 11.00000 0.04354 0.06588 = 0.03883 -0.00025 0.01523 -0.00940 C3A 1 0.751402 0.573336 0.292167 11.00000 0.04331 0.07155 = 0.05674 0.00068 0.01496 -0.01125 F4A 5 0.793106 0.508251 0.284282 11.00000 0.06278 0.14450 = 0.13160 -0.03604 0.01288 0.02747 F5A 5 0.802189 0.638834 0.320274 11.00000 0.07501 0.12541 = 0.07841 0.00706 0.00502 -0.04924 F6A 5 0.743408 0.561336 0.397219 11.00000 0.07539 0.15209 = 0.04325 0.02362 0.01022 -0.01547 C7A 1 0.650806 0.652610 0.092158 11.00000 0.08581 0.07786 = 0.04454 0.00710 0.01016 -0.04607 AFIX 43 H7AA 2 0.692528 0.693731 0.120702 11.00000 -1.20000 AFIX 0 C8A 1 0.575353 0.666303 -0.028546 11.00000 0.09181 0.07691 = 0.05046 0.02563 -0.00203 -0.04570 PART 1 C9A 1 0.590275 0.727430 -0.124070 10.50000 0.06150 0.05022 = 0.06844 0.01493 0.00433 -0.01911 C10A 1 0.662732 0.718917 -0.154998 10.50000 0.08420 0.08165 = 0.09798 0.03142 0.02717 -0.00184 AFIX 33 H10A 2 0.715612 0.729315 -0.076260 10.50000 -1.50000 H10B 2 0.662655 0.662906 -0.186442 10.50000 -1.50000 H10C 2 0.654877 0.759247 -0.221479 10.50000 -1.50000 AFIX 0 C11A 1 0.592819 0.810761 -0.058716 10.50000 0.14297 0.03597 = 0.08604 0.02169 0.02704 -0.00989 AFIX 33 H11A 2 0.648418 0.819835 0.014777 10.50000 -1.50000 H11B 2 0.578619 0.855755 -0.121351 10.50000 -1.50000 H11C 2 0.553034 0.809524 -0.028140 10.50000 -1.50000 AFIX 0 N12A 3 0.506236 0.713137 -0.235588 10.50000 0.11567 0.04093 = 0.05032 0.02505 0.01284 -0.02159 O13A 4 0.478042 0.753285 -0.349475 10.50000 0.10921 0.06932 = 0.07828 0.03268 0.01509 -0.01875 PART 2 C9X 1 0.549985 0.759027 -0.093021 10.50000 0.05016 0.04822 = 0.03867 0.00220 0.01546 -0.01592 C10X 1 0.536731 0.834003 -0.020732 10.50000 0.13904 0.02975 = 0.07247 0.00990 0.03122 0.00955 AFIX 33 H10G 2 0.589452 0.848566 0.055677 10.50000 -1.50000 H10H 2 0.515574 0.881688 -0.079071 10.50000 -1.50000 H10I 2 0.496938 0.818314 0.006088 10.50000 -1.50000 AFIX 0 C11X 1 0.614196 0.779565 -0.134353 10.50000 0.06731 0.15792 = 0.08208 0.05698 0.01972 -0.05060 AFIX 33 H11D 2 0.667517 0.791721 -0.057465 10.50000 -1.50000 H11E 2 0.620124 0.732128 -0.180152 10.50000 -1.50000 H11F 2 0.595633 0.827859 -0.191634 10.50000 -1.50000 AFIX 0 N12X 3 0.466533 0.739831 -0.209483 10.50000 0.05077 0.05529 = 0.05269 0.01159 0.01186 -0.00912 O13X 4 0.429345 0.788045 -0.310543 10.50000 0.09097 0.06747 = 0.05512 0.03042 0.00344 -0.01595 PART 0 C14A 1 0.444241 0.649797 -0.212020 11.00000 0.12883 0.06152 = 0.06049 0.03839 -0.01624 -0.04850 C15A 1 0.363399 0.671672 -0.210647 11.00000 0.09788 0.06721 = 0.17275 0.03449 -0.02872 0.02884 AFIX 33 H15A 2 0.322293 0.693321 -0.295461 11.00000 -1.50000 H15B 2 0.341719 0.621823 -0.191387 11.00000 -1.50000 H15C 2 0.375457 0.713597 -0.144231 11.00000 -1.50000 AFIX 0 C16A 1 0.432395 0.589835 -0.323890 11.00000 0.15907 0.11502 = 0.03405 0.02207 -0.00240 -0.07693 AFIX 33 H16A 2 0.389879 0.612118 -0.407197 11.00000 -1.50000 H16B 2 0.484599 0.584853 -0.323841 11.00000 -1.50000 H16C 2 0.415333 0.535202 -0.310282 11.00000 -1.50000 AFIX 0 N17A 3 0.509211 0.616315 -0.083952 11.00000 0.06872 0.04093 = 0.04841 0.01411 0.00128 -0.01546 O11S 4 0.450127 0.566168 0.106039 11.00000 0.07584 0.08212 = 0.07426 -0.02984 0.04068 -0.00024 AFIX 3 H11S 2 0.476690 0.623480 0.134911 11.00000 -1.20000 AFIX 0 C11S 1 0.373135 0.547673 0.100341 11.00000 0.08375 0.28083 = 0.14393 -0.07617 0.08259 -0.01650 AFIX 33 H11J 2 0.364838 0.586022 0.156372 11.00000 -1.50000 H11K 2 0.327744 0.553611 0.011111 11.00000 -1.50000 H11L 2 0.374406 0.490794 0.129661 11.00000 -1.50000 AFIX 0 NI2 7 1.000000 0.500000 1.000000 10.25000 0.04005 0.03075 = 0.04033 0.00200 0.01325 -0.00051 CO2 6 1.000000 0.500000 1.000000 10.25000 0.04005 0.03075 = 0.04033 0.00200 0.01325 -0.00051 O1B 4 0.883240 0.486155 0.846545 11.00000 0.05073 0.04288 = 0.04710 0.00804 0.01371 -0.00713 C2B 1 0.827722 0.429975 0.829384 11.00000 0.04256 0.03790 = 0.04269 -0.00316 0.01424 0.00000 C3B 1 0.747640 0.441055 0.697872 11.00000 0.04505 0.05849 = 0.04843 0.00267 0.01507 -0.00974 F4B 5 0.709801 0.513236 0.688918 11.00000 0.06646 0.07987 = 0.10557 0.00001 0.00114 0.02060 F5B 5 0.763341 0.439146 0.597589 11.00000 0.06955 0.14489 = 0.04454 0.00732 0.01747 -0.01483 F6B 5 0.689351 0.381655 0.670503 11.00000 0.05860 0.10413 = 0.05990 0.00454 0.00560 -0.03462 C7B 1 0.832341 0.366864 0.910082 11.00000 0.05059 0.03917 = 0.03874 -0.00199 0.01946 -0.00489 AFIX 43 H7BA 2 0.786549 0.330553 0.880815 11.00000 -1.20000 AFIX 0 C8B 1 0.903945 0.352558 1.038613 11.00000 0.04652 0.02671 = 0.04409 0.00032 0.02260 0.00302 C9B 1 0.900392 0.280765 1.121953 11.00000 0.06226 0.03330 = 0.05021 0.00533 0.02104 -0.01104 C10B 1 0.827355 0.289605 1.149946 11.00000 0.07677 0.08123 = 0.07353 0.00753 0.04590 -0.01444 AFIX 33 H10D 2 0.774954 0.279251 1.070337 11.00000 -1.50000 H10E 2 0.834301 0.249400 1.216072 11.00000 -1.50000 H10F 2 0.827158 0.345690 1.180927 11.00000 -1.50000 AFIX 0 C11B 1 0.902496 0.193392 1.064044 11.00000 0.08744 0.04188 = 0.07393 -0.00004 0.03353 -0.01145 AFIX 33 H11G 2 0.849648 0.183470 0.985011 11.00000 -1.50000 H11H 2 0.947143 0.192434 1.043721 11.00000 -1.50000 H11I 2 0.912000 0.150143 1.127526 11.00000 -1.50000 AFIX 0 N12B 3 0.981689 0.296569 1.243907 11.00000 0.07196 0.04595 = 0.05041 0.01457 0.01845 -0.00895 O13B 4 1.005822 0.256174 1.350591 11.00000 0.09920 0.05535 = 0.05875 0.02451 0.02278 -0.01029 C14B 1 1.030370 0.366485 1.230555 11.00000 0.04541 0.04463 = 0.04614 0.01278 0.00843 -0.00542 C15B 1 1.110933 0.328706 1.244094 11.00000 0.05516 0.06376 = 0.09180 0.03558 0.02167 0.01612 AFIX 33 H15D 2 1.146545 0.309610 1.333100 11.00000 -1.50000 H15E 2 1.096897 0.281879 1.184584 11.00000 -1.50000 H15F 2 1.140023 0.370871 1.223113 11.00000 -1.50000 AFIX 0 C16B 1 1.045090 0.433446 1.332175 11.00000 0.07695 0.06003 = 0.04266 -0.00028 0.01748 -0.01140 AFIX 33 H16D 2 1.082297 0.411744 1.418990 11.00000 -1.50000 H16E 2 1.070005 0.482336 1.316913 11.00000 -1.50000 H16F 2 0.992307 0.448741 1.325089 11.00000 -1.50000 AFIX 0 N17B 3 0.973564 0.396748 1.095452 11.00000 0.04508 0.03216 = 0.04026 0.00024 0.01389 0.00175 O21S 4 1.043159 0.410486 0.912736 11.00000 0.05306 0.04888 = 0.09008 -0.01480 0.04152 -0.00887 AFIX 3 H21S 2 1.008969 0.363666 0.873666 11.00000 -1.20000 AFIX 0 C21S 1 1.116797 0.414744 0.906993 11.00000 0.10682 0.06240 = 0.10497 -0.00907 0.06037 -0.00026 AFIX 23 H21A 2 1.105713 0.394751 0.821395 11.00000 -1.20000 H21B 2 1.134827 0.473146 0.915980 11.00000 -1.20000 AFIX 0 C22S 1 1.180067 0.367688 1.003559 11.00000 0.30760 0.28823 = 0.33240 -0.05071 0.19803 -0.08227 AFIX 33 H22A 2 1.229703 0.372385 0.996031 11.00000 -1.50000 H22B 2 1.192036 0.387984 1.088534 11.00000 -1.50000 H22C 2 1.162933 0.309621 0.993988 11.00000 -1.50000 AFIX 0 HKLF 4 REM z44s_a.res in P2(1)/c REM wR2 = 0.1958, GooF = S = 0.837, Restrained GooF = 0.838 for all data REM R1 = 0.0592 for 2475 Fo > 4sig(Fo) and 0.1951 for all 7261 data REM 410 parameters refined using 2 restraints END WGHT 0.0822 0.0000 REM Instructions for potential hydrogen bonds EQIV $3 -x+1, -y+1, -z HTAB C15A O1A_$3 HTAB C16A O1A_$3 HTAB O11S O13A_$2 HTAB O11S O13X_$2 HTAB C11S O13X_$2 EQIV $4 -x+2, -y+1, -z+2 HTAB C15B O1B_$4 HTAB C16B O1B_$4 HTAB O21S O13B_$1 REM Highest difference peak 0.402, deepest hole -0.673, 1-sigma level 0.069 Q1 1 0.4671 0.5032 0.1159 11.00000 0.05 0.40 Q2 1 1.0332 0.5025 0.8865 11.00000 0.05 0.35 Q3 1 1.0634 0.5041 0.9651 11.00000 0.05 0.33 Q4 1 1.0042 0.4601 1.1048 11.00000 0.05 0.33 Q5 1 0.7582 0.4913 0.3711 11.00000 0.05 0.30 Q6 1 0.4971 0.5403 -0.1056 11.00000 0.05 0.30 Q7 1 0.4347 0.4980 0.0254 11.00000 0.05 0.29 Q8 1 1.0180 0.4186 1.0621 11.00000 0.05 0.26 Q9 1 0.4416 0.4498 -0.0056 11.00000 0.05 0.26 Q10 1 0.9458 0.2626 1.1695 11.00000 0.05 0.26 Q11 1 0.7486 0.5045 0.6224 11.00000 0.05 0.26 Q12 1 0.9905 0.4550 0.9010 11.00000 0.05 0.25 Q13 1 0.7679 0.5041 0.7895 11.00000 0.05 0.25 Q14 1 0.4794 0.4297 -0.0744 11.00000 0.05 0.25 Q15 1 1.0812 0.3642 1.2351 11.00000 0.05 0.23 Q16 1 0.9861 0.2863 1.3185 11.00000 0.05 0.23 Q17 1 0.5796 0.6067 -0.1334 11.00000 0.05 0.23 Q18 1 0.4864 0.5796 -0.0568 11.00000 0.05 0.23 Q19 1 0.7706 0.6267 0.4018 11.00000 0.05 0.22 Q20 1 0.4229 0.6258 -0.4073 11.00000 0.05 0.22 ; _shelx_res_checksum 98618 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Ni1 Ni 0.500000 0.500000 0.000000 0.0386(3) Uani 0.5 2 d S . P . . Co1 Co 0.500000 0.500000 0.000000 0.0386(3) Uani 0.5 2 d S . P . . O1A O 0.61768(19) 0.52056(19) 0.1486(3) 0.0526(9) Uani 1 1 d . . . . . C2A C 0.6660(3) 0.5837(3) 0.1684(4) 0.0518(13) Uani 1 1 d . . . . . C3A C 0.7514(3) 0.5733(4) 0.2922(5) 0.0617(15) Uani 1 1 d . . . . . F4A F 0.7931(2) 0.5083(3) 0.2843(4) 0.1289(17) Uani 1 1 d . . . . . F5A F 0.80219(19) 0.6388(2) 0.3203(3) 0.1078(13) Uani 1 1 d . . . . . F6A F 0.74341(18) 0.5613(2) 0.3972(3) 0.0989(12) Uani 1 1 d . . . . . C7A C 0.6508(3) 0.6526(4) 0.0922(5) 0.0794(19) Uani 1 1 d . . . . . H7AA H 0.692528 0.693731 0.120702 0.095 Uiso 1 1 calc R U . . . C8A C 0.5754(4) 0.6663(4) -0.0285(5) 0.090(2) Uani 1 1 d . . . . . C9A C 0.5903(11) 0.7274(9) -0.1241(16) 0.073(5) Uani 0.5 1 d . . P A 1 C10A C 0.6627(8) 0.7189(9) -0.1550(13) 0.096(5) Uani 0.5 1 d . . P A 1 H10A H 0.715612 0.729315 -0.076260 0.144 Uiso 0.5 1 calc R U P A 1 H10B H 0.662655 0.662906 -0.186442 0.144 Uiso 0.5 1 calc R U P A 1 H10C H 0.654877 0.759247 -0.221479 0.144 Uiso 0.5 1 calc R U P A 1 C11A C 0.5928(15) 0.8108(9) -0.0587(16) 0.102(7) Uani 0.5 1 d . . P A 1 H11A H 0.648418 0.819835 0.014777 0.153 Uiso 0.5 1 calc R U P A 1 H11B H 0.578619 0.855755 -0.121351 0.153 Uiso 0.5 1 calc R U P A 1 H11C H 0.553034 0.809524 -0.028140 0.153 Uiso 0.5 1 calc R U P A 1 N12A N 0.5062(8) 0.7131(7) -0.2356(11) 0.082(4) Uani 0.5 1 d . . P A 1 O13A O 0.4780(6) 0.7533(6) -0.3495(9) 0.100(3) Uani 0.5 1 d . . P A 1 C9X C 0.5500(7) 0.7590(11) -0.0930(11) 0.049(3) Uani 0.5 1 d . . P A 2 C10X C 0.5367(9) 0.8340(7) -0.0207(12) 0.090(5) Uani 0.5 1 d . . P A 2 H10G H 0.589452 0.848566 0.055677 0.135 Uiso 0.5 1 calc R U P A 2 H10H H 0.515574 0.881688 -0.079071 0.135 Uiso 0.5 1 calc R U P A 2 H10I H 0.496938 0.818314 0.006088 0.135 Uiso 0.5 1 calc R U P A 2 C11X C 0.6142(9) 0.7796(19) -0.1344(18) 0.110(9) Uani 0.5 1 d . . P A 2 H11D H 0.667517 0.791721 -0.057465 0.165 Uiso 0.5 1 calc R U P A 2 H11E H 0.620124 0.732128 -0.180152 0.165 Uiso 0.5 1 calc R U P A 2 H11F H 0.595633 0.827859 -0.191634 0.165 Uiso 0.5 1 calc R U P A 2 N12X N 0.4665(6) 0.7398(7) -0.2095(11) 0.059(3) Uani 0.5 1 d . . P A 2 O13X O 0.4293(6) 0.7880(5) -0.3105(8) 0.086(3) Uani 0.5 1 d . . P A 2 C14A C 0.4442(5) 0.6498(4) -0.2120(6) 0.112(3) Uani 1 1 d . . . . . C15A C 0.3634(4) 0.6717(4) -0.2106(8) 0.156(4) Uani 1 1 d . . . . . H15A H 0.322293 0.693321 -0.295461 0.233 Uiso 1 1 calc R U . . . H15B H 0.341719 0.621823 -0.191387 0.233 Uiso 1 1 calc R U . . . H15C H 0.375457 0.713597 -0.144231 0.233 Uiso 1 1 calc R U . . . C16A C 0.4324(4) 0.5898(4) -0.3239(5) 0.125(3) Uani 1 1 d . . . . . H16A H 0.389879 0.612118 -0.407197 0.188 Uiso 1 1 calc R U . . . H16B H 0.484599 0.584853 -0.323841 0.188 Uiso 1 1 calc R U . . . H16C H 0.415333 0.535202 -0.310282 0.188 Uiso 1 1 calc R U . . . N17A N 0.5092(2) 0.6163(2) -0.0840(4) 0.0652(13) Uani 1 1 d . . . . . O11S O 0.4501(2) 0.5662(2) 0.1060(3) 0.0760(11) Uani 1 1 d D . . . . H11S H 0.476690 0.623480 0.134911 0.091 Uiso 1 1 d DR U . . . C11S C 0.3731(4) 0.5477(6) 0.1003(8) 0.158(4) Uani 1 1 d . . . . . H11J H 0.364838 0.586022 0.156372 0.237 Uiso 1 1 calc R U . . . H11K H 0.327744 0.553611 0.011111 0.237 Uiso 1 1 calc R U . . . H11L H 0.374406 0.490794 0.129661 0.237 Uiso 1 1 calc R U . . . Ni2 Ni 1.000000 0.500000 1.000000 0.0401(3) Uani 0.5 2 d S . P . . Co2 Co 1.000000 0.500000 1.000000 0.0401(3) Uani 0.5 2 d S . P . . O1B O 0.88324(18) 0.48615(19) 0.8465(3) 0.0517(9) Uani 1 1 d . . . . . C2B C 0.8277(3) 0.4300(3) 0.8294(4) 0.0442(12) Uani 1 1 d . . . . . C3B C 0.7476(3) 0.4411(3) 0.6979(5) 0.0544(14) Uani 1 1 d . . . . . F4B F 0.70980(19) 0.5132(2) 0.6889(3) 0.1026(13) Uani 1 1 d . . . . . F5B F 0.76334(18) 0.4391(2) 0.5976(3) 0.0913(11) Uani 1 1 d . . . . . F6B F 0.68935(17) 0.3817(2) 0.6705(3) 0.0849(10) Uani 1 1 d . . . . . C7B C 0.8323(3) 0.3669(3) 0.9101(4) 0.0441(12) Uani 1 1 d . . . . . H7BA H 0.786549 0.330553 0.880815 0.053 Uiso 1 1 calc R U . . . C8B C 0.9039(3) 0.3526(3) 1.0386(4) 0.0391(11) Uani 1 1 d . . . . . C9B C 0.9004(3) 0.2808(3) 1.1220(5) 0.0518(13) Uani 1 1 d . . . . . C10B C 0.8274(3) 0.2896(4) 1.1499(5) 0.0735(17) Uani 1 1 d . . . . . H10D H 0.774954 0.279251 1.070337 0.110 Uiso 1 1 calc R U . . . H10E H 0.834301 0.249400 1.216072 0.110 Uiso 1 1 calc R U . . . H10F H 0.827158 0.345690 1.180927 0.110 Uiso 1 1 calc R U . . . C11B C 0.9025(3) 0.1934(3) 1.0640(5) 0.0708(17) Uani 1 1 d . . . . . H11G H 0.849648 0.183470 0.985011 0.106 Uiso 1 1 calc R U . . . H11H H 0.947143 0.192434 1.043721 0.106 Uiso 1 1 calc R U . . . H11I H 0.912000 0.150143 1.127526 0.106 Uiso 1 1 calc R U . . . N12B N 0.9817(3) 0.2966(3) 1.2439(4) 0.0615(12) Uani 1 1 d . . . . . O13B O 1.0058(2) 0.2562(2) 1.3506(3) 0.0786(12) Uani 1 1 d . . . . . C14B C 1.0304(3) 0.3665(3) 1.2306(4) 0.0518(13) Uani 1 1 d . . . . . C15B C 1.1109(3) 0.3287(3) 1.2441(5) 0.0770(18) Uani 1 1 d . . . . . H15D H 1.146545 0.309610 1.333100 0.115 Uiso 1 1 calc R U . . . H15E H 1.096897 0.281879 1.184584 0.115 Uiso 1 1 calc R U . . . H15F H 1.140023 0.370871 1.223113 0.115 Uiso 1 1 calc R U . . . C16B C 1.0451(3) 0.4334(3) 1.3322(4) 0.0654(15) Uani 1 1 d . . . . . H16D H 1.082297 0.411744 1.418990 0.098 Uiso 1 1 calc R U . . . H16E H 1.070005 0.482336 1.316913 0.098 Uiso 1 1 calc R U . . . H16F H 0.992307 0.448741 1.325089 0.098 Uiso 1 1 calc R U . . . N17B N 0.9736(2) 0.3967(2) 1.0955(3) 0.0425(9) Uani 1 1 d . . . . . O21S O 1.0432(2) 0.4105(2) 0.9127(3) 0.0615(10) Uani 1 1 d D . . . . H21S H 1.008969 0.363666 0.873666 0.074 Uiso 1 1 d DR U . . . C21S C 1.1168(4) 0.4147(4) 0.9070(7) 0.088(2) Uani 1 1 d . . . . . H21A H 1.105713 0.394751 0.821395 0.106 Uiso 1 1 calc R U . . . H21B H 1.134827 0.473146 0.915980 0.106 Uiso 1 1 calc R U . . . C22S C 1.1801(8) 0.3677(9) 1.0036(13) 0.293(8) Uani 1 1 d . . . . . H22A H 1.229703 0.372385 0.996031 0.439 Uiso 1 1 calc R U . . . H22B H 1.192036 0.387984 1.088534 0.439 Uiso 1 1 calc R U . . . H22C H 1.162933 0.309621 0.993988 0.439 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 Ni1 0.0412(5) 0.0307(5) 0.0365(5) 0.0010(4) 0.0140(4) -0.0011(4) Co1 0.0412(5) 0.0307(5) 0.0365(5) 0.0010(4) 0.0140(4) -0.0011(4) O1A 0.0497(19) 0.046(2) 0.0461(19) 0.0057(15) 0.0119(16) -0.0052(15) C2A 0.044(3) 0.066(4) 0.039(3) 0.000(3) 0.015(2) -0.009(3) C3A 0.043(3) 0.072(4) 0.057(4) 0.001(3) 0.015(3) -0.011(3) F4A 0.063(2) 0.145(4) 0.132(3) -0.036(3) 0.013(2) 0.027(2) F5A 0.075(2) 0.125(3) 0.078(2) 0.007(2) 0.0050(18) -0.049(2) F6A 0.075(2) 0.152(4) 0.0432(18) 0.024(2) 0.0102(17) -0.015(2) C7A 0.086(4) 0.078(4) 0.045(3) 0.007(3) 0.010(3) -0.046(3) C8A 0.092(4) 0.077(4) 0.050(3) 0.026(3) -0.002(3) -0.046(3) C9A 0.061(9) 0.050(9) 0.068(9) 0.015(7) 0.004(8) -0.019(8) C10A 0.084(9) 0.082(11) 0.098(10) 0.031(8) 0.027(9) -0.002(8) C11A 0.143(18) 0.036(9) 0.086(12) 0.022(9) 0.027(12) -0.010(11) N12A 0.116(11) 0.041(7) 0.050(7) 0.025(5) 0.013(7) -0.022(7) O13A 0.109(8) 0.069(7) 0.078(6) 0.033(5) 0.015(6) -0.019(5) C9X 0.050(7) 0.048(9) 0.039(6) 0.002(5) 0.015(5) -0.016(6) C10X 0.139(13) 0.030(7) 0.072(9) 0.010(6) 0.031(9) 0.010(7) C11X 0.067(10) 0.16(2) 0.082(12) 0.057(14) 0.020(9) -0.051(12) N12X 0.051(6) 0.055(8) 0.053(6) 0.012(5) 0.012(5) -0.009(5) O13X 0.091(6) 0.067(6) 0.055(5) 0.030(4) 0.003(5) -0.016(5) C14A 0.129(6) 0.062(4) 0.060(4) 0.038(3) -0.016(4) -0.049(4) C15A 0.098(5) 0.067(5) 0.173(8) 0.034(5) -0.029(5) 0.029(4) C16A 0.159(6) 0.115(6) 0.034(3) 0.022(3) -0.002(4) -0.077(5) N17A 0.069(3) 0.041(3) 0.048(2) 0.0141(19) 0.001(2) -0.015(2) O11S 0.076(2) 0.082(3) 0.074(2) -0.030(2) 0.041(2) 0.000(2) C11S 0.084(5) 0.281(12) 0.144(7) -0.076(7) 0.083(5) -0.017(6) Ni2 0.0401(5) 0.0308(5) 0.0403(5) 0.0020(4) 0.0133(4) -0.0005(4) Co2 0.0401(5) 0.0308(5) 0.0403(5) 0.0020(4) 0.0133(4) -0.0005(4) O1B 0.0507(18) 0.043(2) 0.0471(18) 0.0080(15) 0.0137(15) -0.0071(15) C2B 0.043(3) 0.038(3) 0.043(3) -0.003(2) 0.014(2) 0.000(2) C3B 0.045(3) 0.058(4) 0.048(3) 0.003(3) 0.015(3) -0.010(3) F4B 0.066(2) 0.080(3) 0.106(3) 0.000(2) 0.0011(19) 0.0206(18) F5B 0.070(2) 0.145(3) 0.0445(18) 0.0073(19) 0.0175(17) -0.0148(19) F6B 0.0586(17) 0.104(3) 0.0599(18) 0.0045(17) 0.0056(15) -0.0346(18) C7B 0.051(3) 0.039(3) 0.039(3) -0.002(2) 0.019(2) -0.005(2) C8B 0.047(3) 0.027(2) 0.044(3) 0.000(2) 0.023(2) 0.003(2) C9B 0.062(3) 0.033(3) 0.050(3) 0.005(2) 0.021(3) -0.011(2) C10B 0.077(4) 0.081(4) 0.074(4) 0.008(3) 0.046(3) -0.014(3) C11B 0.087(4) 0.042(3) 0.074(4) 0.000(3) 0.034(3) -0.011(3) N12B 0.072(3) 0.046(3) 0.050(3) 0.015(2) 0.018(2) -0.009(2) O13B 0.099(3) 0.055(2) 0.059(2) 0.0245(19) 0.023(2) -0.010(2) C14B 0.045(3) 0.045(3) 0.046(3) 0.013(2) 0.008(2) -0.005(2) C15B 0.055(3) 0.064(4) 0.092(4) 0.036(3) 0.022(3) 0.016(3) C16B 0.077(4) 0.060(4) 0.043(3) 0.000(3) 0.017(3) -0.011(3) N17B 0.045(2) 0.032(2) 0.040(2) 0.0002(16) 0.0139(18) 0.0017(17) O21S 0.0531(19) 0.049(2) 0.090(3) -0.0148(18) 0.0415(19) -0.0089(17) C21S 0.107(6) 0.062(5) 0.105(5) -0.009(4) 0.060(5) 0.000(4) C22S 0.308(19) 0.29(2) 0.33(2) -0.051(15) 0.198(17) -0.082(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Ni1 O1A 180.00(15) . 3_665 ? O1A Ni1 N17A 87.73(13) . . ? O1A Ni1 N17A 92.27(13) 3_665 . ? O1A Ni1 N17A 92.27(13) . 3_665 ? O1A Ni1 N17A 87.73(13) 3_665 3_665 ? N17A Ni1 N17A 180.0 . 3_665 ? O1A Ni1 O11S 90.23(13) . . ? O1A Ni1 O11S 89.77(13) 3_665 . ? N17A Ni1 O11S 89.97(16) . . ? N17A Ni1 O11S 90.03(16) 3_665 . ? O1A Ni1 O11S 89.77(13) . 3_665 ? O1A Ni1 O11S 90.23(13) 3_665 3_665 ? N17A Ni1 O11S 90.03(16) . 3_665 ? N17A Ni1 O11S 89.97(16) 3_665 3_665 ? O11S Ni1 O11S 180.0 . 3_665 ? C2A O1A Ni1 129.1(3) . . ? O1A C2A C7A 128.2(4) . . ? O1A C2A C3A 112.3(5) . . ? C7A C2A C3A 119.4(5) . . ? F4A C3A F5A 105.7(5) . . ? F4A C3A F6A 107.0(5) . . ? F5A C3A F6A 105.9(5) . . ? F4A C3A C2A 112.1(5) . . ? F5A C3A C2A 114.5(5) . . ? F6A C3A C2A 111.2(4) . . ? C2A C7A C8A 124.1(5) . . ? N17A C8A C7A 126.8(5) . . ? N17A C8A C9A 117.2(6) . . ? C7A C8A C9A 111.5(7) . . ? N17A C8A C9X 109.8(6) . . ? C7A C8A C9X 121.1(6) . . ? N12A C9A C11A 109.9(17) . . ? N12A C9A C10A 115.1(16) . . ? C11A C9A C10A 112.4(19) . . ? N12A C9A C8A 93.3(12) . . ? C11A C9A C8A 98(2) . . ? C10A C9A C8A 125.2(11) . . ? O13A N12A C9A 122.1(13) . . ? O13A N12A C14A 120.5(9) . . ? C9A N12A C14A 117.2(11) . . ? N12X C9X C11X 111.1(12) . . ? N12X C9X C10X 106.7(11) . . ? C11X C9X C10X 111.7(19) . . ? N12X C9X C8A 99.6(9) . . ? C11X C9X C8A 104.9(17) . . ? C10X C9X C8A 122.1(9) . . ? O13X N12X C14A 122.8(9) . . ? O13X N12X C9X 123.6(11) . . ? C14A N12X C9X 111.3(10) . . ? N17A C14A N12X 104.6(6) . . ? N17A C14A C16A 110.0(6) . . ? N12X C14A C16A 122.0(7) . . ? N17A C14A C15A 111.5(6) . . ? N12X C14A C15A 92.3(7) . . ? C16A C14A C15A 115.0(5) . . ? N17A C14A N12A 96.7(6) . . ? C16A C14A N12A 92.8(7) . . ? C15A C14A N12A 128.3(7) . . ? C8A N17A C14A 111.2(4) . . ? C8A N17A Ni1 124.0(3) . . ? C14A N17A Ni1 124.8(3) . . ? C11S O11S Ni1 125.2(4) . . ? O1B Ni2 O1B 180.0 3_767 . ? O1B Ni2 O21S 90.91(12) 3_767 . ? O1B Ni2 O21S 89.09(12) . . ? O1B Ni2 O21S 89.09(12) 3_767 3_767 ? O1B Ni2 O21S 90.91(12) . 3_767 ? O21S Ni2 O21S 180.0 . 3_767 ? O1B Ni2 N17B 88.00(12) 3_767 3_767 ? O1B Ni2 N17B 92.00(12) . 3_767 ? O21S Ni2 N17B 91.30(13) . 3_767 ? O21S Ni2 N17B 88.70(13) 3_767 3_767 ? O1B Ni2 N17B 92.00(12) 3_767 . ? O1B Ni2 N17B 88.00(12) . . ? O21S Ni2 N17B 88.70(13) . . ? O21S Ni2 N17B 91.30(13) 3_767 . ? N17B Ni2 N17B 180.0(2) 3_767 . ? C2B O1B Ni2 128.4(3) . . ? O1B C2B C7B 129.4(4) . . ? O1B C2B C3B 111.5(4) . . ? C7B C2B C3B 119.1(4) . . ? F4B C3B F6B 105.4(4) . . ? F4B C3B F5B 106.6(5) . . ? F6B C3B F5B 105.7(4) . . ? F4B C3B C2B 112.7(4) . . ? F6B C3B C2B 114.5(4) . . ? F5B C3B C2B 111.3(4) . . ? C2B C7B C8B 123.7(4) . . ? N17B C8B C7B 126.6(4) . . ? N17B C8B C9B 114.7(4) . . ? C7B C8B C9B 118.7(4) . . ? N12B C9B C8B 98.4(3) . . ? N12B C9B C10B 110.1(4) . . ? C8B C9B C10B 113.0(4) . . ? N12B C9B C11B 109.8(4) . . ? C8B C9B C11B 111.6(4) . . ? C10B C9B C11B 112.9(4) . . ? O13B N12B C9B 123.4(4) . . ? O13B N12B C14B 123.3(4) . . ? C9B N12B C14B 113.2(4) . . ? N17B C14B N12B 102.6(3) . . ? N17B C14B C16B 111.6(4) . . ? N12B C14B C16B 108.7(4) . . ? N17B C14B C15B 111.5(4) . . ? N12B C14B C15B 107.4(4) . . ? C16B C14B C15B 114.2(4) . . ? C8B N17B C14B 111.0(4) . . ? C8B N17B Ni2 123.7(3) . . ? C14B N17B Ni2 125.4(3) . . ? C21S O21S Ni2 126.8(4) . . ? C22S C21S O21S 112.2(8) . . ? 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 Ni1 O1A 2.007(3) . ? Ni1 O1A 2.007(3) 3_665 ? Ni1 N17A 2.134(4) . ? Ni1 N17A 2.134(4) 3_665 ? Ni1 O11S 2.147(3) . ? Ni1 O11S 2.147(3) 3_665 ? O1A C2A 1.278(5) . ? C2A C7A 1.348(7) . ? C2A C3A 1.518(6) . ? C3A F4A 1.314(6) . ? C3A F5A 1.321(5) . ? C3A F6A 1.322(6) . ? C7A C8A 1.414(6) . ? C8A N17A 1.315(6) . ? C8A C9A 1.60(2) . ? C8A C9X 1.609(16) . ? C9A N12A 1.454(16) . ? C9A C11A 1.51(2) . ? C9A C10A 1.55(3) . ? N12A O13A 1.326(12) . ? N12A C14A 1.639(14) . ? C9X N12X 1.484(14) . ? C9X C11X 1.52(2) . ? C9X C10X 1.55(2) . ? N12X O13X 1.280(12) . ? N12X C14A 1.479(13) . ? C14A N17A 1.469(6) . ? C14A C16A 1.542(10) . ? C14A C15A 1.530(10) . ? O11S C11S 1.410(6) . ? Ni2 O1B 2.002(3) 3_767 ? Ni2 O1B 2.002(3) . ? Ni2 O21S 2.118(3) . ? Ni2 O21S 2.118(3) 3_767 ? Ni2 N17B 2.167(4) 3_767 ? Ni2 N17B 2.167(4) . ? O1B C2B 1.290(5) . ? C2B C7B 1.348(6) . ? C2B C3B 1.514(6) . ? C3B F4B 1.314(6) . ? C3B F6B 1.337(5) . ? C3B F5B 1.341(5) . ? C7B C8B 1.435(5) . ? C8B N17B 1.308(5) . ? C8B C9B 1.520(6) . ? C9B N12B 1.480(5) . ? C9B C10B 1.536(7) . ? C9B C11B 1.550(6) . ? N12B O13B 1.269(4) . ? N12B C14B 1.479(6) . ? C14B N17B 1.471(5) . ? C14B C16B 1.513(6) . ? C14B C15B 1.527(6) . ? O21S C21S 1.387(7) . ? C21S C22S 1.366(13) . ? 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 O21S H21S O13B 0.93 1.91 2.732(5) 145.6 4_565 yes O11S H11S O13X^b 1.01 1.92 2.608(8) 123.2 4_576 yes O11S H11S O13A^a 1.01 1.96 2.905(10) 155.8 4_576 yes