#------------------------------------------------------------------------------ #$Date: 2023-11-02 01:43:29 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287232 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247650.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_7247650 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 F6 N4 Ni O6' _chemical_formula_weight 637.27 _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.cc2bjd5g _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2022-03-22 deposited with the CCDC. 2023-10-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 120.67(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.564(4) _cell_length_b 15.699(3) _cell_length_c 11.768(2) _cell_measurement_reflns_used 5462 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.92 _cell_measurement_theta_min 2.59 _cell_volume 2949.9(13) _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-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _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 0.0658 _diffrn_reflns_av_unetI/netI 0.0940 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 29421 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.209 _diffrn_reflns_theta_min 1.275 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_T_max 0.2901 _exptl_absorpt_correction_T_min 0.2442 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour light_green _exptl_crystal_density_diffrn 1.435 _exptl_crystal_description block _exptl_crystal_F_000 1328 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.501 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 372 _refine_ls_number_reflns 7954 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.872 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0441 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.1341 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3617 _reflns_number_total 7954 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00912b1.cif _cod_data_source_block z700s _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7247650 _shelx_shelxl_version_number 2014/7 _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 ; z700s.res created by SHELXL-2014/7 TITL z700s in P2(1)/c CELL 0.71073 18.5639 15.6993 11.7681 90.000 120.673 90.000 ZERR 4.00 0.0037 0.0031 0.0024 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F NI UNIT 92 144 16 24 24 4 L.S. 20 acta htab EQIV $1 -x, y-1/2, -z+5/2 HTAB O1S O13A_$1 EQIV $2 x, -y+1/2, z+1/2 HTAB O1T O13B_$2 BOND FMAP 2 PLAN 20 WGHT 0.061600 FVAR 0.17218 NI1 6 0.000000 0.500000 1.000000 10.50000 0.03106 0.02325 = 0.02900 -0.00171 0.01358 0.00186 O1S 4 -0.049401 0.448099 1.113146 11.00000 0.06704 0.03257 = 0.06486 0.01509 0.04520 0.00911 H1S 2 -0.041914 0.406071 1.131220 11.00000 0.04024 C1S 1 -0.123654 0.478001 1.111484 11.00000 0.10457 0.06386 = 0.11264 0.03428 0.08922 0.03027 AFIX 33 H1SA 2 -0.132854 0.444223 1.170926 11.00000 -1.50000 H1SB 2 -0.116254 0.536540 1.138774 11.00000 -1.50000 H1SC 2 -0.171123 0.473080 1.023648 11.00000 -1.50000 AFIX 0 O1A 4 -0.117117 0.523179 0.851930 11.00000 0.03631 0.03459 = 0.03567 -0.00564 0.00871 0.00628 C2A 1 -0.161035 0.590433 0.828625 11.00000 0.03031 0.03717 = 0.03218 0.00595 0.01522 0.00737 C3A 1 -0.247549 0.581953 0.709892 11.00000 0.03858 0.04840 = 0.04263 -0.00176 0.01223 0.00559 F4A 5 -0.290437 0.521006 0.726143 11.00000 0.04720 0.10789 = 0.10062 0.01748 0.01139 -0.02404 F5A 5 -0.294816 0.650424 0.679216 11.00000 0.06118 0.07667 = 0.08503 -0.01052 -0.01303 0.03580 F6A 5 -0.245923 0.561415 0.602463 11.00000 0.06061 0.13898 = 0.04215 -0.02594 0.00940 0.00598 C7A 1 -0.139536 0.664183 0.898544 11.00000 0.03821 0.02930 = 0.03672 -0.00005 0.01578 0.00679 AFIX 43 H7AA 2 -0.177867 0.708779 0.866614 11.00000 -1.20000 AFIX 0 C8A 1 -0.061926 0.677433 1.017719 11.00000 0.04013 0.02631 = 0.03514 -0.00130 0.02346 0.00205 C9A 1 -0.046921 0.761356 1.088906 11.00000 0.04852 0.02773 = 0.04325 -0.00686 0.01899 0.00576 C10A 1 -0.035608 0.834672 1.014387 11.00000 0.10319 0.03276 = 0.07998 -0.00062 0.03626 -0.00248 AFIX 33 H10A 2 -0.088355 0.847550 0.936756 11.00000 -1.50000 H10B 2 -0.015546 0.883991 1.070341 11.00000 -1.50000 H10C 2 0.004199 0.818624 0.989154 11.00000 -1.50000 AFIX 0 C11A 1 -0.113045 0.782390 1.124567 11.00000 0.07322 0.07983 = 0.09161 -0.03886 0.04753 0.00647 AFIX 33 H11A 2 -0.164942 0.795759 1.045673 11.00000 -1.50000 H11B 2 -0.120907 0.734219 1.167343 11.00000 -1.50000 H11C 2 -0.094983 0.830458 1.183172 11.00000 -1.50000 AFIX 0 N12A 3 0.032325 0.740869 1.206901 11.00000 0.05892 0.03654 = 0.04871 -0.02132 0.01614 0.00494 O13A 4 0.069074 0.787923 1.308844 11.00000 0.08777 0.05994 = 0.06840 -0.03974 0.00803 0.01169 C14A 1 0.067466 0.657611 1.199924 11.00000 0.04312 0.02984 = 0.04369 -0.01511 0.01181 0.00230 C15A 1 0.146460 0.672004 1.193624 11.00000 0.04562 0.05280 = 0.08639 -0.02721 0.02064 -0.01338 AFIX 33 H15A 2 0.189643 0.694840 1.276269 11.00000 -1.50000 H15B 2 0.164812 0.618825 1.176743 11.00000 -1.50000 H15C 2 0.134735 0.711422 1.123886 11.00000 -1.50000 AFIX 0 C16A 1 0.082188 0.603695 1.317644 11.00000 0.08563 0.05545 = 0.03005 -0.00485 0.01175 0.02124 AFIX 33 H16A 2 0.126904 0.627997 1.397479 11.00000 -1.50000 H16B 2 0.032012 0.602367 1.322178 11.00000 -1.50000 H16C 2 0.096919 0.546769 1.307406 11.00000 -1.50000 AFIX 0 N17A 3 -0.001035 0.622399 1.074647 11.00000 0.03353 0.02363 = 0.03113 -0.00480 0.01286 -0.00024 NI2 6 0.500000 0.500000 2.000000 10.50000 0.02883 0.02564 = 0.03184 -0.00216 0.01233 0.00157 O1T 4 0.456848 0.407349 2.081306 11.00000 0.05431 0.03185 = 0.07274 0.01171 0.04109 0.00430 H1T 2 0.468273 0.358527 2.098313 11.00000 0.06447 C1T 1 0.384113 0.408091 2.093507 11.00000 0.06357 0.04975 = 0.08793 0.00800 0.05197 0.00153 AFIX 23 H1TA 2 0.366847 0.466691 2.091176 11.00000 -1.20000 H1TB 2 0.398827 0.384698 2.178980 11.00000 -1.20000 AFIX 0 C2T 1 0.312097 0.359316 1.989190 11.00000 0.06030 0.07629 = 0.08770 0.01016 0.03515 -0.00620 AFIX 33 H2TA 2 0.265828 0.362723 2.003852 11.00000 -1.50000 H2TB 2 0.295947 0.382901 1.904189 11.00000 -1.50000 H2TC 2 0.327969 0.300801 1.992107 11.00000 -1.50000 AFIX 0 O1B 4 0.615249 0.487488 2.155919 11.00000 0.03288 0.03796 = 0.03710 -0.00686 0.00946 0.00892 C2B 1 0.670643 0.432737 2.174736 11.00000 0.03186 0.03439 = 0.03321 0.00158 0.01413 0.00209 C3B 1 0.749798 0.442209 2.307296 11.00000 0.03833 0.04578 = 0.04043 -0.00402 0.01228 0.00805 F4B 5 0.785619 0.517170 2.319696 11.00000 0.06062 0.06989 = 0.08694 -0.00079 -0.00564 -0.02449 F5B 5 0.734271 0.436843 2.405377 11.00000 0.06001 0.13481 = 0.03307 -0.00311 0.01709 0.01325 F6B 5 0.808783 0.384543 2.333925 11.00000 0.04987 0.09544 = 0.05465 -0.00673 0.00499 0.03244 C7B 1 0.666648 0.369980 2.091936 11.00000 0.03705 0.03802 = 0.04215 0.00139 0.01634 0.01253 AFIX 43 H7BA 2 0.712487 0.333809 2.121848 11.00000 -1.20000 AFIX 0 C8B 1 0.597156 0.355944 1.962791 11.00000 0.03625 0.02553 = 0.03870 -0.00060 0.01930 0.00156 C9B 1 0.601789 0.285901 1.879481 11.00000 0.04422 0.03386 = 0.04677 -0.00875 0.02217 0.00514 C10B 1 0.674278 0.294738 1.854951 11.00000 0.05920 0.07584 = 0.06739 -0.02275 0.03530 0.00291 AFIX 33 H10D 2 0.726076 0.284456 1.935718 11.00000 -1.50000 H10E 2 0.667933 0.254075 1.789530 11.00000 -1.50000 H10F 2 0.674614 0.351265 1.824111 11.00000 -1.50000 AFIX 0 C11B 1 0.599823 0.196753 1.933837 11.00000 0.09297 0.03359 = 0.07666 -0.00459 0.03500 0.00980 AFIX 33 H11D 2 0.651817 0.186683 2.014380 11.00000 -1.50000 H11E 2 0.554516 0.194123 1.950890 11.00000 -1.50000 H11F 2 0.591918 0.154130 1.869973 11.00000 -1.50000 AFIX 0 N12B 3 0.522647 0.301505 1.756707 11.00000 0.04636 0.03756 = 0.04300 -0.01639 0.01698 -0.00091 O13B 4 0.499070 0.261448 1.648832 11.00000 0.06995 0.04785 = 0.05375 -0.02381 0.02809 -0.00388 C14B 1 0.471955 0.370177 1.768075 11.00000 0.04014 0.03480 = 0.04270 -0.01161 0.01608 0.00119 C15B 1 0.392005 0.330460 1.750009 11.00000 0.04581 0.05900 = 0.07733 -0.03164 0.02644 -0.01190 AFIX 33 H15D 2 0.358052 0.373880 1.756996 11.00000 -1.50000 H15E 2 0.361551 0.304204 1.664505 11.00000 -1.50000 H15F 2 0.405967 0.288235 1.817126 11.00000 -1.50000 AFIX 0 C16B 1 0.456136 0.438471 1.668113 11.00000 0.06780 0.05137 = 0.03653 -0.00339 0.01526 0.01168 AFIX 33 H16D 2 0.423288 0.483169 1.675039 11.00000 -1.50000 H16E 2 0.508628 0.461251 1.684688 11.00000 -1.50000 H16F 2 0.426405 0.414537 1.580879 11.00000 -1.50000 AFIX 0 N17B 3 0.528036 0.400231 1.905490 11.00000 0.03514 0.02693 = 0.03250 -0.00705 0.01284 -0.00167 HKLF 4 REM z700s in P2(1)/c REM R1 = 0.0441 for 3617 Fo > 4sig(Fo) and 0.1172 for all 7954 data REM 372 parameters refined using 0 restraints END WGHT 0.0590 0.0000 REM Instructions for potential hydrogen bonds HTAB O1S O13A_$1 EQIV $3 -x, -y+1, -z+2 HTAB C15A O1A_$3 EQIV $4 -x+1, -y+1, -z+4 HTAB C16A F5B_$4 HTAB C16A O1A_$3 HTAB O1T O13B_$2 HTAB C15B O1B_$4 HTAB C16B O1B_$4 REM Highest difference peak 0.501, deepest hole -0.738, 1-sigma level 0.070 Q1 1 -0.1811 0.4387 1.0688 11.00000 0.05 0.50 Q2 1 -0.2608 0.5037 0.6427 11.00000 0.05 0.42 Q3 1 0.4420 0.4584 2.0098 11.00000 0.05 0.35 Q4 1 -0.3089 0.6190 0.6845 11.00000 0.05 0.32 Q5 1 0.6613 0.3999 2.1453 11.00000 0.05 0.31 Q6 1 0.7560 0.5026 2.3663 11.00000 0.05 0.31 Q7 1 -0.1385 0.5315 1.0583 11.00000 0.05 0.31 Q8 1 -0.0936 0.4984 1.2455 11.00000 0.05 0.29 Q9 1 -0.2874 0.4921 0.6669 11.00000 0.05 0.29 Q10 1 -0.1001 0.6639 0.9415 11.00000 0.05 0.28 Q11 1 0.5037 0.4171 1.9494 11.00000 0.05 0.28 Q12 1 -0.2739 0.6222 0.6001 11.00000 0.05 0.28 Q13 1 0.4498 0.2297 1.6784 11.00000 0.05 0.28 Q14 1 -0.2994 0.5768 0.7396 11.00000 0.05 0.28 Q15 1 -0.2572 0.6621 0.6493 11.00000 0.05 0.27 Q16 1 0.5995 0.3210 1.9174 11.00000 0.05 0.27 Q17 1 0.0736 0.6293 1.2571 11.00000 0.05 0.25 Q18 1 -0.0407 0.5900 1.0910 11.00000 0.05 0.25 Q19 1 0.0016 0.5817 1.0446 11.00000 0.05 0.24 Q20 1 0.5550 0.2740 1.8243 11.00000 0.05 0.24 ; _shelx_res_checksum 10868 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 0.0000 0.5000 1.0000 0.02857(13) Uani 1 2 d S . P . . O1S O -0.04940(14) 0.44810(16) 1.1131(2) 0.0495(6) Uani 1 1 d . . . . . H1S H -0.0419(18) 0.4061(18) 1.131(3) 0.040(11) Uiso 1 1 d . . . . . C1S C -0.1237(2) 0.4780(2) 1.1115(4) 0.0781(12) Uani 1 1 d . . . . . H1SA H -0.1329 0.4442 1.1709 0.117 Uiso 1 1 calc R U . . . H1SB H -0.1163 0.5365 1.1388 0.117 Uiso 1 1 calc R U . . . H1SC H -0.1711 0.4731 1.0236 0.117 Uiso 1 1 calc R U . . . O1A O -0.11712(11) 0.52318(12) 0.85193(17) 0.0400(5) Uani 1 1 d . . . . . C2A C -0.16104(15) 0.59043(18) 0.8286(2) 0.0335(6) Uani 1 1 d . . . . . C3A C -0.24755(18) 0.5820(2) 0.7099(3) 0.0471(8) Uani 1 1 d . . . . . F4A F -0.29044(12) 0.52101(15) 0.7261(2) 0.0973(8) Uani 1 1 d . . . . . F5A F -0.29482(11) 0.65042(13) 0.6792(2) 0.0974(8) Uani 1 1 d . . . . . F6A F -0.24592(11) 0.56142(15) 0.60246(17) 0.0883(7) Uani 1 1 d . . . . . C7A C -0.13954(15) 0.66418(18) 0.8985(3) 0.0363(7) Uani 1 1 d . . . . . H7AA H -0.1779 0.7088 0.8666 0.044 Uiso 1 1 calc R U . . . C8A C -0.06193(16) 0.67743(16) 1.0177(2) 0.0319(6) Uani 1 1 d . . . . . C9A C -0.04692(17) 0.76136(18) 1.0889(3) 0.0419(7) Uani 1 1 d . . . . . C10A C -0.0356(2) 0.8347(2) 1.0144(3) 0.0768(11) Uani 1 1 d . . . . . H10A H -0.0884 0.8475 0.9368 0.115 Uiso 1 1 calc R U . . . H10B H -0.0155 0.8840 1.0703 0.115 Uiso 1 1 calc R U . . . H10C H 0.0042 0.8186 0.9892 0.115 Uiso 1 1 calc R U . . . C11A C -0.1130(2) 0.7824(2) 1.1246(3) 0.0790(12) Uani 1 1 d . . . . . H11A H -0.1649 0.7958 1.0457 0.119 Uiso 1 1 calc R U . . . H11B H -0.1209 0.7342 1.1673 0.119 Uiso 1 1 calc R U . . . H11C H -0.0950 0.8305 1.1832 0.119 Uiso 1 1 calc R U . . . N12A N 0.03233(15) 0.74087(16) 1.2069(2) 0.0533(7) Uani 1 1 d . . . . . O13A O 0.06907(15) 0.78792(15) 1.3088(2) 0.0867(8) Uani 1 1 d . . . . . C14A C 0.06747(16) 0.65761(18) 1.1999(3) 0.0436(8) Uani 1 1 d . . . . . C15A C 0.14646(17) 0.6720(2) 1.1936(3) 0.0676(10) Uani 1 1 d . . . . . H15A H 0.1896 0.6948 1.2763 0.101 Uiso 1 1 calc R U . . . H15B H 0.1648 0.6188 1.1767 0.101 Uiso 1 1 calc R U . . . H15C H 0.1347 0.7114 1.1239 0.101 Uiso 1 1 calc R U . . . C16A C 0.0822(2) 0.6037(2) 1.3176(3) 0.0652(10) Uani 1 1 d . . . . . H16A H 0.1269 0.6280 1.3975 0.098 Uiso 1 1 calc R U . . . H16B H 0.0320 0.6024 1.3222 0.098 Uiso 1 1 calc R U . . . H16C H 0.0969 0.5468 1.3074 0.098 Uiso 1 1 calc R U . . . N17A N -0.00104(12) 0.62240(13) 1.07465(19) 0.0311(5) Uani 1 1 d . . . . . Ni2 Ni 0.5000 0.5000 2.0000 0.03022(14) Uani 1 2 d S . P . . O1T O 0.45685(13) 0.40735(15) 2.0813(2) 0.0490(6) Uani 1 1 d . . . . . H1T H 0.4683(19) 0.359(2) 2.098(3) 0.064(12) Uiso 1 1 d . . . . . C1T C 0.38411(19) 0.4081(2) 2.0935(3) 0.0610(9) Uani 1 1 d . . . . . H1TA H 0.3668 0.4667 2.0912 0.073 Uiso 1 1 calc R U . . . H1TB H 0.3988 0.3847 2.1790 0.073 Uiso 1 1 calc R U . . . C2T C 0.31210(19) 0.3593(2) 1.9892(3) 0.0760(11) Uani 1 1 d . . . . . H2TA H 0.2658 0.3627 2.0039 0.114 Uiso 1 1 calc R U . . . H2TB H 0.2959 0.3829 1.9042 0.114 Uiso 1 1 calc R U . . . H2TC H 0.3280 0.3008 1.9921 0.114 Uiso 1 1 calc R U . . . O1B O 0.61525(11) 0.48749(11) 2.15592(17) 0.0398(5) Uani 1 1 d . . . . . C2B C 0.67064(15) 0.43274(18) 2.1747(2) 0.0343(6) Uani 1 1 d . . . . . C3B C 0.74980(17) 0.4422(2) 2.3073(3) 0.0451(8) Uani 1 1 d . . . . . F4B F 0.78562(12) 0.51717(13) 2.3197(2) 0.0924(8) Uani 1 1 d . . . . . F5B F 0.73427(10) 0.43684(15) 2.40538(15) 0.0790(6) Uani 1 1 d . . . . . F6B F 0.80878(10) 0.38454(13) 2.33393(17) 0.0766(6) Uani 1 1 d . . . . . C7B C 0.66665(16) 0.36998(18) 2.0919(3) 0.0409(7) Uani 1 1 d . . . . . H7BA H 0.7125 0.3338 2.1218 0.049 Uiso 1 1 calc R U . . . C8B C 0.59716(16) 0.35594(17) 1.9628(3) 0.0334(6) Uani 1 1 d . . . . . C9B C 0.60179(16) 0.28590(18) 1.8795(3) 0.0421(7) Uani 1 1 d . . . . . C10B C 0.67428(18) 0.2947(2) 1.8550(3) 0.0661(10) Uani 1 1 d . . . . . H10D H 0.7261 0.2845 1.9357 0.099 Uiso 1 1 calc R U . . . H10E H 0.6679 0.2541 1.7895 0.099 Uiso 1 1 calc R U . . . H10F H 0.6746 0.3513 1.8241 0.099 Uiso 1 1 calc R U . . . C11B C 0.5998(2) 0.19675(19) 1.9338(3) 0.0715(11) Uani 1 1 d . . . . . H11D H 0.6518 0.1867 2.0144 0.107 Uiso 1 1 calc R U . . . H11E H 0.5545 0.1941 1.9509 0.107 Uiso 1 1 calc R U . . . H11F H 0.5919 0.1541 1.8700 0.107 Uiso 1 1 calc R U . . . N12B N 0.52265(14) 0.30150(15) 1.7567(2) 0.0450(6) Uani 1 1 d . . . . . O13B O 0.49907(12) 0.26145(13) 1.64883(19) 0.0588(6) Uani 1 1 d . . . . . C14B C 0.47195(16) 0.37018(18) 1.7681(3) 0.0415(7) Uani 1 1 d . . . . . C15B C 0.39201(17) 0.3305(2) 1.7500(3) 0.0630(10) Uani 1 1 d . . . . . H15D H 0.3581 0.3739 1.7570 0.094 Uiso 1 1 calc R U . . . H15E H 0.3616 0.3042 1.6645 0.094 Uiso 1 1 calc R U . . . H15F H 0.4060 0.2882 1.8171 0.094 Uiso 1 1 calc R U . . . C16B C 0.45614(19) 0.4385(2) 1.6681(3) 0.0571(9) Uani 1 1 d . . . . . H16D H 0.4233 0.4832 1.6750 0.086 Uiso 1 1 calc R U . . . H16E H 0.5086 0.4613 1.6847 0.086 Uiso 1 1 calc R U . . . H16F H 0.4264 0.4145 1.5809 0.086 Uiso 1 1 calc R U . . . N17B N 0.52804(13) 0.40023(13) 1.90549(19) 0.0335(5) Uani 1 1 d . . . . . 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 0.0311(2) 0.0232(3) 0.0290(2) -0.0017(2) 0.0136(2) 0.0019(2) O1S 0.0670(16) 0.0326(15) 0.0649(15) 0.0151(13) 0.0452(13) 0.0091(13) C1S 0.105(3) 0.064(2) 0.113(3) 0.034(2) 0.089(3) 0.030(2) O1A 0.0363(10) 0.0346(11) 0.0357(10) -0.0056(9) 0.0087(8) 0.0063(9) C2A 0.0303(14) 0.0372(18) 0.0322(14) 0.0060(14) 0.0152(12) 0.0074(13) C3A 0.0386(17) 0.048(2) 0.0426(18) -0.0018(17) 0.0122(15) 0.0056(16) F4A 0.0472(11) 0.1079(18) 0.1006(17) 0.0175(14) 0.0114(12) -0.0240(12) F5A 0.0612(12) 0.0767(15) 0.0850(14) -0.0105(12) -0.0130(11) 0.0358(11) F6A 0.0606(12) 0.139(2) 0.0421(10) -0.0259(12) 0.0094(9) 0.0060(12) C7A 0.0382(15) 0.0293(16) 0.0367(15) -0.0001(14) 0.0158(13) 0.0068(13) C8A 0.0401(15) 0.0263(15) 0.0351(14) -0.0013(13) 0.0235(13) 0.0021(13) C9A 0.0485(17) 0.0277(17) 0.0433(16) -0.0069(15) 0.0190(15) 0.0058(14) C10A 0.103(3) 0.033(2) 0.080(3) -0.0006(19) 0.036(2) -0.002(2) C11A 0.073(2) 0.080(3) 0.092(3) -0.039(2) 0.048(2) 0.006(2) N12A 0.0589(16) 0.0365(15) 0.0487(15) -0.0213(13) 0.0161(13) 0.0049(13) O13A 0.0878(17) 0.0599(16) 0.0684(15) -0.0397(14) 0.0080(13) 0.0117(13) C14A 0.0431(16) 0.0298(17) 0.0437(17) -0.0151(15) 0.0118(14) 0.0023(14) C15A 0.0456(18) 0.053(2) 0.086(2) -0.027(2) 0.0206(18) -0.0134(17) C16A 0.086(2) 0.055(2) 0.0301(16) -0.0049(17) 0.0117(16) 0.0212(19) N17A 0.0335(11) 0.0236(12) 0.0311(12) -0.0048(10) 0.0129(10) -0.0002(10) Ni2 0.0288(2) 0.0256(3) 0.0318(3) -0.0022(2) 0.0123(2) 0.0016(2) O1T 0.0543(13) 0.0318(13) 0.0727(15) 0.0117(12) 0.0411(12) 0.0043(11) C1T 0.064(2) 0.050(2) 0.088(2) 0.008(2) 0.052(2) 0.0015(18) C2T 0.060(2) 0.076(3) 0.088(3) 0.010(2) 0.035(2) -0.006(2) O1B 0.0329(10) 0.0380(12) 0.0371(10) -0.0069(9) 0.0095(8) 0.0089(9) C2B 0.0319(14) 0.0344(17) 0.0332(14) 0.0016(14) 0.0141(12) 0.0021(13) C3B 0.0383(16) 0.046(2) 0.0404(17) -0.0040(16) 0.0123(15) 0.0081(16) F4B 0.0606(13) 0.0699(14) 0.0869(15) -0.0008(12) -0.0056(11) -0.0245(11) F5B 0.0600(11) 0.1348(19) 0.0331(9) -0.0031(11) 0.0171(9) 0.0133(12) F6B 0.0499(10) 0.0954(16) 0.0547(11) -0.0067(11) 0.0050(9) 0.0324(11) C7B 0.0370(15) 0.0380(18) 0.0422(16) 0.0014(15) 0.0163(13) 0.0125(14) C8B 0.0363(14) 0.0255(15) 0.0387(15) -0.0006(13) 0.0193(13) 0.0016(13) C9B 0.0442(16) 0.0339(18) 0.0468(17) -0.0087(15) 0.0222(15) 0.0051(14) C10B 0.059(2) 0.076(3) 0.067(2) -0.023(2) 0.0353(18) 0.0029(18) C11B 0.093(3) 0.034(2) 0.077(2) -0.0046(19) 0.035(2) 0.0098(19) N12B 0.0464(14) 0.0376(15) 0.0430(14) -0.0164(13) 0.0170(12) -0.0009(12) O13B 0.0699(14) 0.0478(14) 0.0538(13) -0.0238(12) 0.0281(11) -0.0039(11) C14B 0.0401(15) 0.0348(17) 0.0427(17) -0.0116(15) 0.0161(14) 0.0012(14) C15B 0.0458(18) 0.059(2) 0.077(2) -0.0316(19) 0.0264(17) -0.0119(17) C16B 0.068(2) 0.051(2) 0.0365(16) -0.0034(17) 0.0153(15) 0.0117(17) N17B 0.0351(12) 0.0269(13) 0.0325(12) -0.0070(11) 0.0128(10) -0.0017(10) 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' 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(10) 3_567 . ? O1A Ni1 N17A 87.74(7) 3_567 3_567 ? O1A Ni1 N17A 92.26(7) . 3_567 ? O1A Ni1 N17A 92.26(7) 3_567 . ? O1A Ni1 N17A 87.74(7) . . ? N17A Ni1 N17A 180.00(13) 3_567 . ? O1A Ni1 O1S 89.48(9) 3_567 3_567 ? O1A Ni1 O1S 90.52(9) . 3_567 ? N17A Ni1 O1S 89.42(9) 3_567 3_567 ? N17A Ni1 O1S 90.58(9) . 3_567 ? O1A Ni1 O1S 90.52(9) 3_567 . ? O1A Ni1 O1S 89.48(9) . . ? N17A Ni1 O1S 90.58(9) 3_567 . ? N17A Ni1 O1S 89.42(9) . . ? O1S Ni1 O1S 180.0 3_567 . ? C1S O1S Ni1 125.40(19) . . ? C2A O1A Ni1 128.84(17) . . ? O1A C2A C7A 128.2(2) . . ? O1A C2A C3A 112.9(2) . . ? C7A C2A C3A 118.9(2) . . ? F5A C3A F4A 105.4(3) . . ? F5A C3A F6A 105.9(3) . . ? F4A C3A F6A 105.8(3) . . ? F5A C3A C2A 115.4(3) . . ? F4A C3A C2A 111.5(3) . . ? F6A C3A C2A 112.1(3) . . ? C2A C7A C8A 124.0(2) . . ? N17A C8A C7A 125.9(2) . . ? N17A C8A C9A 115.3(2) . . ? C7A C8A C9A 118.8(2) . . ? N12A C9A C8A 98.5(2) . . ? N12A C9A C11A 110.5(2) . . ? C8A C9A C11A 113.3(2) . . ? N12A C9A C10A 110.3(2) . . ? C8A C9A C10A 112.4(2) . . ? C11A C9A C10A 111.2(3) . . ? O13A N12A C9A 124.6(2) . . ? O13A N12A C14A 121.7(2) . . ? C9A N12A C14A 113.7(2) . . ? N17A C14A N12A 101.9(2) . . ? N17A C14A C16A 111.3(2) . . ? N12A C14A C16A 108.6(2) . . ? N17A C14A C15A 111.5(2) . . ? N12A C14A C15A 109.5(2) . . ? C16A C14A C15A 113.3(3) . . ? C8A N17A C14A 110.1(2) . . ? C8A N17A Ni1 125.25(16) . . ? C14A N17A Ni1 124.63(16) . . ? O1B Ni2 O1B 180.0 3_669 . ? O1B Ni2 O1T 90.45(8) 3_669 . ? O1B Ni2 O1T 89.55(8) . . ? O1B Ni2 O1T 89.55(8) 3_669 3_669 ? O1B Ni2 O1T 90.45(8) . 3_669 ? O1T Ni2 O1T 180.0 . 3_669 ? O1B Ni2 N17B 91.44(7) 3_669 . ? O1B Ni2 N17B 88.56(7) . . ? O1T Ni2 N17B 88.87(9) . . ? O1T Ni2 N17B 91.13(9) 3_669 . ? O1B Ni2 N17B 88.56(7) 3_669 3_669 ? O1B Ni2 N17B 91.44(7) . 3_669 ? O1T Ni2 N17B 91.13(9) . 3_669 ? O1T Ni2 N17B 88.87(9) 3_669 3_669 ? N17B Ni2 N17B 180.00(7) . 3_669 ? C1T O1T Ni2 129.5(2) . . ? O1T C1T C2T 114.3(3) . . ? C2B O1B Ni2 128.33(17) . . ? O1B C2B C7B 128.4(2) . . ? O1B C2B C3B 112.9(2) . . ? C7B C2B C3B 118.7(2) . . ? F5B C3B F4B 106.3(3) . . ? F5B C3B F6B 105.7(2) . . ? F4B C3B F6B 105.8(3) . . ? F5B C3B C2B 111.3(2) . . ? F4B C3B C2B 111.8(2) . . ? F6B C3B C2B 115.3(2) . . ? C2B C7B C8B 124.5(2) . . ? N17B C8B C7B 125.9(2) . . ? N17B C8B C9B 114.9(2) . . ? C7B C8B C9B 119.2(2) . . ? N12B C9B C8B 99.1(2) . . ? N12B C9B C10B 109.7(2) . . ? C8B C9B C10B 114.0(2) . . ? N12B C9B C11B 109.6(2) . . ? C8B C9B C11B 111.7(2) . . ? C10B C9B C11B 111.8(3) . . ? O13B N12B C9B 124.2(2) . . ? O13B N12B C14B 122.5(2) . . ? C9B N12B C14B 113.4(2) . . ? N12B C14B N17B 101.8(2) . . ? N12B C14B C16B 109.1(2) . . ? N17B C14B C16B 111.9(2) . . ? N12B C14B C15B 108.0(2) . . ? N17B C14B C15B 112.0(2) . . ? C16B C14B C15B 113.3(2) . . ? C8B N17B C14B 110.6(2) . . ? C8B N17B Ni2 123.99(17) . . ? C14B N17B Ni2 125.39(16) . . ? 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 2.0076(19) 3_567 ? Ni1 O1A 2.0076(19) . ? Ni1 N17A 2.117(2) 3_567 ? Ni1 N17A 2.117(2) . ? Ni1 O1S 2.127(2) 3_567 ? Ni1 O1S 2.127(2) . ? O1S C1S 1.447(4) . ? O1A C2A 1.275(3) . ? C2A C7A 1.357(3) . ? C2A C3A 1.503(4) . ? C3A F5A 1.316(3) . ? C3A F4A 1.320(3) . ? C3A F6A 1.320(3) . ? C7A C8A 1.423(3) . ? C8A N17A 1.304(3) . ? C8A C9A 1.509(3) . ? C9A N12A 1.453(3) . ? C9A C11A 1.522(4) . ? C9A C10A 1.525(4) . ? N12A O13A 1.271(3) . ? N12A C14A 1.482(3) . ? C14A N17A 1.478(3) . ? C14A C16A 1.524(4) . ? C14A C15A 1.522(4) . ? Ni2 O1B 1.9943(19) 3_669 ? Ni2 O1B 1.9944(19) . ? Ni2 O1T 2.111(2) . ? Ni2 O1T 2.111(2) 3_669 ? Ni2 N17B 2.133(2) . ? Ni2 N17B 2.133(2) 3_669 ? O1T C1T 1.429(3) . ? C1T C2T 1.485(4) . ? O1B C2B 1.270(3) . ? C2B C7B 1.361(4) . ? C2B C3B 1.509(4) . ? C3B F5B 1.327(3) . ? C3B F4B 1.323(3) . ? C3B F6B 1.329(3) . ? C7B C8B 1.422(3) . ? C8B N17B 1.305(3) . ? C8B C9B 1.505(4) . ? C9B N12B 1.463(3) . ? C9B C10B 1.520(4) . ? C9B C11B 1.547(4) . ? N12B O13B 1.277(3) . ? N12B C14B 1.481(3) . ? C14B N17B 1.485(3) . ? C14B C16B 1.506(4) . ? C14B C15B 1.521(4) . ? 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 O1S H1S O13A 0.69(3) 2.13(3) 2.764(3) 153(3) 2_547 O1T H1T O13B 0.79(3) 1.97(3) 2.763(3) 177(3) 4_566