#------------------------------------------------------------------------------ #$Date: 2017-03-20 06:47:03 +0200 (Mon, 20 Mar 2017) $ #$Revision: 194354 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/60/7056070.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_7056070 loop_ _publ_author_name 'Liu, Yu-Ling' 'Wu, De-Hong' 'Wang, Zhongxia' 'Zhang, Yi' _publ_section_title ; Switchings of dielectric constant, second harmonic generation and polarization in a polar hybrid cyanometallate crystal ; _journal_name_full 'New J. Chem.' _journal_paper_doi 10.1039/C6NJ03973A _journal_year 2017 _chemical_formula_moiety 'C6 Co N6, 2(C3 H4 N S), H3 O' _chemical_formula_sum 'C12 H11 Co N8 O S2' _chemical_formula_weight 406.34 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-03-17 deposited with the CCDC. 2017-03-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.033(14) _cell_length_b 8.920(10) _cell_length_c 13.208(12) _cell_measurement_reflns_used 480 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.4855 _cell_measurement_theta_min 1.5415 _cell_volume 1771(3) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 28.6533 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Saturn724+ (4x4 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0505 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12203 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_min 2.655 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T.(1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour light-yellow _exptl_crystal_density_diffrn 1.524 _exptl_crystal_description block _exptl_crystal_F_000 692 _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.2300 _exptl_crystal_size_min 0.2000 _refine_diff_density_max 1.249 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.141 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.09(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 249 _refine_ls_number_reflns 4032 _refine_ls_number_restraints 163 _refine_ls_restrained_S_all 1.238 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_gt 0.0955 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2817 _refine_ls_wR_factor_ref 0.2975 _reflns_Friedel_coverage 0.917 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 3233 _reflns_number_total 4032 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6nj03973a2.cif _cod_data_source_block 293K _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7056070 _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 ; new.res created by SHELXL-2014/7 TITL aa in Pna2(1) CELL 0.71073 15.0334 8.9196 13.2080 90.000 90.000 90.000 ZERR 17 0.0138 0.0098 0.0123 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H Cl Co K Mg N O S UNIT 64 0 0 4 0 0 24 4 0 L.S. 5 ACTA BOND $H FMAP 2 PLAN 2 htab eqiv $1 -x+1, -y, z-1/2 eqiv $2 x, y+1, z eqiv $3 x+1/2, -y+1/2, z htab n7 n3_$1 htab n7' n3_$1 htab n8 n5_$2 htab n8' n3_$3 htab o1 n4_$2 htab o1 n6 htab o1 n2_$3 conf eadp c12 c12' eadp c11 c11' eadp s2 s2' eadp c10 c10' eadp n8 n8' twin dfix 1.67 s2 c10 s2 c11 s1 c7 s1 c8 s2' c11' s2' c10' s1' c7' s1' c8' dfix 1.4 0.02 c12' n8' n8' c10' c12' c11' c10 n8 n8 c12 c12 c11 c8' c9' c9' n7' flat 0.01 n7 > c9 flat 0.01 n7' > c9' flat 0.01 n8 > c12 flat 0.01 n8' > c12' simu 0.01 s2 s2' s1 s1' simu 0.01 n8 > c12 simu 0.01 n8' > c12' simu 0.01 n7 > c9 simu 0.01 n7' > c9' isor 0.005 s1 eadp n7 n7' eadp c7 c7' eadp s1 s1' eadp c8 c8' eadp c9 c9' FREE C12 S2 WGHT 0.200000 BASF 0.08632 FVAR 0.70131 0.37002 C1 1 0.609953 0.172503 0.278004 11.00000 0.05586 0.04152 = 0.06220 0.00722 -0.00538 0.00404 C3 1 0.620250 -0.122378 0.275160 11.00000 0.06625 0.04502 = 0.06049 -0.01095 0.00049 -0.01475 C4 1 0.726708 -0.121150 0.113356 11.00000 0.05055 0.04329 = 0.06326 -0.00718 -0.00182 -0.00889 C5 1 0.771343 0.036047 0.277997 11.00000 0.04119 0.05007 = 0.05664 0.00315 0.00391 -0.00325 C6 1 0.716780 0.189754 0.114206 11.00000 0.04850 0.04365 = 0.04838 0.00239 -0.00710 0.00029 PART 1 N7 7 0.496040 0.402146 0.008612 10.37002 0.12452 0.07515 = 0.07809 -0.00664 -0.00921 -0.05597 AFIX 43 H7A 2 0.488880 0.333589 -0.036440 10.37002 -1.20000 AFIX 0 C7 1 0.442114 0.414714 0.099030 10.37002 0.11309 0.06447 = 0.06530 -0.00085 0.00576 -0.06504 AFIX 43 H7 2 0.395519 0.351374 0.116790 10.37002 -1.20000 AFIX 0 S1 9 0.477482 0.561970 0.166241 10.37002 0.14599 0.11013 = 0.10714 -0.00387 -0.01367 -0.02055 C8 1 0.555015 0.592888 0.076526 10.37002 0.14060 0.07492 = 0.09839 -0.00871 -0.00293 -0.05341 AFIX 43 H8 2 0.594121 0.672884 0.084151 10.37002 -1.20000 AFIX 0 C9 1 0.561142 0.514038 0.002690 10.37002 0.13654 0.07212 = 0.07709 0.00231 -0.00734 -0.05701 AFIX 43 H9 2 0.602193 0.525604 -0.049403 10.37002 -1.20000 PART 2 AFIX 0 N7' 7 0.456661 0.413347 0.018906 10.62998 0.12452 0.07515 = 0.07809 -0.00664 -0.00921 -0.05597 AFIX 43 H7A' 2 0.429765 0.355808 -0.023433 10.62998 -1.20000 AFIX 0 C7' 1 0.463836 0.383037 0.119970 10.62998 0.11309 0.06447 = 0.06530 -0.00085 0.00576 -0.06504 AFIX 43 H7' 2 0.441087 0.299561 0.153280 10.62998 -1.20000 AFIX 0 S1' 9 0.519965 0.520950 0.171832 10.62998 0.14599 0.11013 = 0.10714 -0.00387 -0.01367 -0.02055 C8' 1 0.537306 0.622374 0.069823 10.62998 0.14060 0.07492 = 0.09839 -0.00871 -0.00293 -0.05341 AFIX 43 H8' 2 0.568133 0.712652 0.066693 10.62998 -1.20000 AFIX 0 C9' 1 0.498514 0.550420 -0.008678 10.62998 0.13654 0.07212 = 0.07709 0.00231 -0.00734 -0.05701 AFIX 43 H9' 2 0.499129 0.587111 -0.074582 10.62998 -1.20000 PART 1 AFIX 0 N8 7 0.865721 0.667557 0.335585 10.37002 0.05162 0.03971 = 0.08386 -0.00874 0.00731 0.00092 AFIX 43 H8A 2 0.882297 0.759795 0.333688 10.37002 -1.20000 AFIX 0 C10 1 0.775643 0.607895 0.334839 10.37002 0.08835 0.06124 = 0.10922 -0.00730 -0.00008 -0.00722 AFIX 43 H10 2 0.723799 0.664651 0.332261 10.37002 -1.20000 AFIX 0 S2 9 0.780651 0.413534 0.339543 10.37002 0.10968 0.09469 = 0.12917 -0.00275 -0.00666 -0.00436 C11 1 0.886241 0.398917 0.342299 10.37002 0.08184 0.04243 = 0.08913 0.00299 -0.00198 0.01841 AFIX 43 H11 2 0.920416 0.312094 0.344931 10.37002 -1.20000 AFIX 0 C12 1 0.915272 0.547881 0.339812 10.37002 0.07326 0.04289 = 0.07969 0.00659 -0.00001 0.01068 AFIX 43 H12 2 0.976456 0.563108 0.341338 10.37002 -1.20000 PART 2 AFIX 0 N8' 7 0.887228 0.640541 0.336309 10.62998 0.05162 0.03971 = 0.08386 -0.00874 0.00731 0.00092 AFIX 43 H8A' 2 0.928175 0.707867 0.335858 10.62998 -1.20000 AFIX 0 C10' 1 0.802238 0.671362 0.336197 10.62998 0.08835 0.06124 = 0.10922 -0.00730 -0.00008 -0.00722 AFIX 43 H10' 2 0.779714 0.768468 0.335711 10.62998 -1.20000 AFIX 0 S2' 9 0.739868 0.522092 0.336997 10.62998 0.10968 0.09469 = 0.12917 -0.00275 -0.00666 -0.00436 C11' 1 0.838293 0.389232 0.337648 10.62998 0.08184 0.04243 = 0.08913 0.00299 -0.00198 0.01841 AFIX 43 H11' 2 0.837294 0.284983 0.338109 10.62998 -1.20000 AFIX 0 C12' 1 0.905883 0.474581 0.337313 10.62998 0.07326 0.04289 = 0.07969 0.00659 -0.00001 0.01068 AFIX 43 H12' 2 0.963553 0.436853 0.337667 10.62998 -1.20000 PART 0 AFIX 0 CO1 4 0.668544 0.028976 0.193372 11.00000 0.04380 0.03618 = 0.05044 -0.00712 0.00372 -0.00135 N1 7 0.574978 0.259968 0.325089 11.00000 0.09687 0.06875 = 0.06343 -0.01384 0.00652 0.03372 N2 7 0.497215 0.004891 0.068721 11.00000 0.06377 0.06252 = 0.08363 -0.00748 -0.02240 -0.00425 N3 7 0.590621 -0.217188 0.323631 11.00000 0.08942 0.06963 = 0.07665 0.00321 0.01182 -0.01713 N4 7 0.760848 -0.216515 0.071396 11.00000 0.07102 0.04383 = 0.07353 -0.00601 0.00317 0.01102 N5 7 0.833519 0.038668 0.327881 11.00000 0.05659 0.09449 = 0.06918 0.00797 -0.01716 -0.01001 N6 7 0.746810 0.288318 0.073746 11.00000 0.07070 0.04519 = 0.07540 0.00382 0.00086 -0.00958 O1 8 0.832476 0.529025 0.015116 11.00000 0.05611 0.04578 = 0.05877 -0.00503 -0.00759 -0.00640 AFIX 3 H1A 2 0.809206 0.610635 0.035946 11.00000 -1.20000 H1B 2 0.802946 0.454755 0.037926 11.00000 -1.20000 H1C 2 0.885276 0.523035 0.037286 11.00000 -1.20000 AFIX 0 C2 1 0.563492 0.019051 0.111955 11.00000 0.06628 0.04634 = 0.06592 -0.01350 -0.00533 0.00241 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 REM aa in Pna2(1) REM R1 = 0.0955 for 3233 Fo > 4sig(Fo) and 0.1095 for all 4032 data REM 249 parameters refined using 163 restraints END WGHT 0.2000 0.0000 REM Instructions for potential hydrogen bonds HTAB N7 N3_$1 EQIV $4 x-1/2, -y+1/2, z HTAB C7 N6_$4 HTAB C8 N4_$2 EQIV $5 -x+3/2, y+1/2, z-1/2 HTAB C9 N5_$5 HTAB N7' N3_$1 EQIV $6 -x+1, -y+1, z-1/2 HTAB C9' N1_$6 HTAB N8 N5_$2 HTAB C10 N3_$2 HTAB C11 N1_$3 HTAB C12 N3_$3 HTAB N8' N3_$3 HTAB C10' N5_$2 HTAB C11' N5 HTAB C12' N1_$3 HTAB O1 N4_$2 HTAB O1 N6 HTAB O1 N2_$3 REM Highest difference peak 1.249, deepest hole -1.126, 1-sigma level 0.141 Q1 1 0.5752 0.5233 0.1354 11.00000 0.05 0.95 Q2 1 0.4744 0.6033 0.0088 11.00000 0.05 0.58 ; _shelx_res_checksum 55696 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' 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 C1 C 0.6100(7) 0.1725(13) 0.2780(10) 0.053(2) Uani 1 1 d . . . . . C3 C 0.6202(8) -0.1224(13) 0.2752(11) 0.057(3) Uani 1 1 d . . . . . C4 C 0.7267(7) -0.1211(12) 0.1134(11) 0.052(2) Uani 1 1 d . . . . . C5 C 0.7713(7) 0.0360(12) 0.2780(10) 0.049(2) Uani 1 1 d . . . . . C6 C 0.7168(6) 0.1898(12) 0.1142(9) 0.047(2) Uani 1 1 d . . . . . N7 N 0.496(2) 0.402(5) 0.009(4) 0.093(4) Uani 0.37 1 d . U P A 1 H7A H 0.4889 0.3336 -0.0364 0.111 Uiso 0.37 1 calc R U P A 1 C7 C 0.442(3) 0.415(4) 0.099(3) 0.081(4) Uani 0.37 1 d D U P A 1 H7 H 0.3955 0.3514 0.1168 0.097 Uiso 0.37 1 calc R U P A 1 S1 S 0.4775(14) 0.562(2) 0.1662(16) 0.121(3) Uani 0.37 1 d D U P A 1 C8 C 0.555(3) 0.593(7) 0.077(4) 0.105(4) Uani 0.37 1 d D U P A 1 H8 H 0.5941 0.6729 0.0842 0.126 Uiso 0.37 1 calc R U P A 1 C9 C 0.561(3) 0.514(5) 0.003(4) 0.095(5) Uani 0.37 1 d . U P A 1 H9 H 0.6022 0.5256 -0.0494 0.114 Uiso 0.37 1 calc R U P A 1 N7' N 0.4567(13) 0.413(3) 0.019(2) 0.093(4) Uani 0.63 1 d D U P B 2 H7A' H 0.4298 0.3558 -0.0234 0.111 Uiso 0.63 1 calc R U P B 2 C7' C 0.4638(15) 0.383(2) 0.120(2) 0.081(4) Uani 0.63 1 d D U P B 2 H7' H 0.4411 0.2996 0.1533 0.097 Uiso 0.63 1 calc R U P B 2 S1' S 0.5200(8) 0.5209(13) 0.1718(11) 0.121(3) Uani 0.63 1 d D U P B 2 C8' C 0.5373(17) 0.622(3) 0.070(2) 0.105(4) Uani 0.63 1 d D U P B 2 H8' H 0.5681 0.7127 0.0667 0.126 Uiso 0.63 1 calc R U P B 2 C9' C 0.4985(15) 0.550(3) -0.009(2) 0.095(5) Uani 0.63 1 d D U P B 2 H9' H 0.4991 0.5871 -0.0746 0.114 Uiso 0.63 1 calc R U P B 2 N8 N 0.866(2) 0.668(4) 0.336(2) 0.058(3) Uani 0.37 1 d D U P C 1 H8A H 0.8823 0.7598 0.3337 0.070 Uiso 0.37 1 calc R U P C 1 C10 C 0.776(3) 0.608(3) 0.335(2) 0.086(4) Uani 0.37 1 d D U P C 1 H10 H 0.7238 0.6647 0.3323 0.104 Uiso 0.37 1 calc R U P C 1 S2 S 0.7807(11) 0.414(2) 0.3395(12) 0.111(2) Uani 0.37 1 d D U P C 1 C11 C 0.8862(18) 0.399(4) 0.342(2) 0.071(4) Uani 0.37 1 d D U P C 1 H11 H 0.9204 0.3121 0.3449 0.085 Uiso 0.37 1 calc R U P C 1 C12 C 0.915(3) 0.548(3) 0.340(2) 0.065(4) Uani 0.37 1 d D U P C 1 H12 H 0.9765 0.5631 0.3413 0.078 Uiso 0.37 1 calc R U P C 1 N8' N 0.8872(12) 0.641(2) 0.3363(15) 0.058(3) Uani 0.63 1 d D U P D 2 H8A' H 0.9282 0.7079 0.3359 0.070 Uiso 0.63 1 calc R U P D 2 C10' C 0.8022(14) 0.671(3) 0.3362(13) 0.086(4) Uani 0.63 1 d D U P D 2 H10' H 0.7797 0.7685 0.3357 0.104 Uiso 0.63 1 calc R U P D 2 S2' S 0.7399(7) 0.5221(11) 0.3370(9) 0.111(2) Uani 0.63 1 d D U P D 2 C11' C 0.8383(14) 0.389(2) 0.3376(16) 0.071(4) Uani 0.63 1 d D U P D 2 H11' H 0.8373 0.2850 0.3381 0.085 Uiso 0.63 1 calc R U P D 2 C12' C 0.9059(15) 0.475(2) 0.3373(15) 0.065(4) Uani 0.63 1 d D U P D 2 H12' H 0.9636 0.4369 0.3377 0.078 Uiso 0.63 1 calc R U P D 2 Co1 Co 0.66854(7) 0.02898(12) 0.1934(5) 0.0435(5) Uani 1 1 d . . . . . N1 N 0.5750(8) 0.2600(13) 0.3251(10) 0.076(4) Uani 1 1 d . . . . . N2 N 0.4972(8) 0.0049(14) 0.0687(14) 0.070(3) Uani 1 1 d . . . . . N3 N 0.5906(8) -0.2172(16) 0.3236(11) 0.079(3) Uani 1 1 d . . . . . N4 N 0.7608(7) -0.2165(12) 0.0714(10) 0.063(2) Uani 1 1 d . . . . . N5 N 0.8335(6) 0.0387(16) 0.3279(12) 0.073(4) Uani 1 1 d . . . . . N6 N 0.7468(7) 0.2883(12) 0.0737(11) 0.064(2) Uani 1 1 d . . . . . O1 O 0.8325(5) 0.5290(9) 0.0151(9) 0.054(2) Uani 1 1 d . . . . . H1A H 0.8092 0.6106 0.0359 0.064 Uiso 1 1 d R U . . . H1B H 0.8029 0.4548 0.0379 0.064 Uiso 1 1 d R U . . . H1C H 0.8853 0.5230 0.0373 0.064 Uiso 1 1 d R U . . . C2 C 0.5635(9) 0.0191(13) 0.1120(12) 0.060(3) 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 C1 0.056(5) 0.042(6) 0.062(6) 0.007(5) -0.005(5) 0.004(4) C3 0.066(6) 0.045(6) 0.060(7) -0.011(5) 0.000(5) -0.015(5) C4 0.051(5) 0.043(5) 0.063(6) -0.007(5) -0.002(5) -0.009(4) C5 0.041(5) 0.050(6) 0.057(6) 0.003(4) 0.004(5) -0.003(4) C6 0.049(5) 0.044(5) 0.048(5) 0.002(4) -0.007(4) 0.000(4) N7 0.125(10) 0.075(7) 0.078(7) -0.007(6) -0.009(9) -0.056(8) C7 0.113(8) 0.064(7) 0.065(7) -0.001(6) 0.006(7) -0.065(6) S1 0.146(6) 0.110(5) 0.107(4) -0.004(4) -0.014(4) -0.021(4) C8 0.141(9) 0.075(8) 0.098(7) -0.009(7) -0.003(8) -0.053(7) C9 0.137(10) 0.072(8) 0.077(8) 0.002(7) -0.007(9) -0.057(8) N7' 0.125(10) 0.075(7) 0.078(7) -0.007(6) -0.009(9) -0.056(8) C7' 0.113(8) 0.064(7) 0.065(7) -0.001(6) 0.006(7) -0.065(6) S1' 0.146(6) 0.110(5) 0.107(4) -0.004(4) -0.014(4) -0.021(4) C8' 0.141(9) 0.075(8) 0.098(7) -0.009(7) -0.003(8) -0.053(7) C9' 0.137(10) 0.072(8) 0.077(8) 0.002(7) -0.007(9) -0.057(8) N8 0.052(8) 0.040(7) 0.084(6) -0.009(5) 0.007(6) 0.001(6) C10 0.088(8) 0.061(8) 0.109(8) -0.007(7) 0.000(7) -0.007(7) S2 0.110(5) 0.095(4) 0.129(5) -0.003(4) -0.007(4) -0.004(3) C11 0.082(8) 0.042(6) 0.089(7) 0.003(6) -0.002(7) 0.018(7) C12 0.073(7) 0.043(8) 0.080(7) 0.007(7) 0.000(6) 0.011(7) N8' 0.052(8) 0.040(7) 0.084(6) -0.009(5) 0.007(6) 0.001(6) C10' 0.088(8) 0.061(8) 0.109(8) -0.007(7) 0.000(7) -0.007(7) S2' 0.110(5) 0.095(4) 0.129(5) -0.003(4) -0.007(4) -0.004(3) C11' 0.082(8) 0.042(6) 0.089(7) 0.003(6) -0.002(7) 0.018(7) C12' 0.073(7) 0.043(8) 0.080(7) 0.007(7) 0.000(6) 0.011(7) Co1 0.0438(7) 0.0362(7) 0.0504(7) -0.0071(8) 0.0037(7) -0.0013(4) N1 0.097(8) 0.069(8) 0.063(6) -0.014(6) 0.007(5) 0.034(7) N2 0.064(6) 0.063(6) 0.084(8) -0.007(6) -0.022(6) -0.004(5) N3 0.089(8) 0.070(7) 0.077(7) 0.003(6) 0.012(6) -0.017(7) N4 0.071(6) 0.044(5) 0.074(6) -0.006(5) 0.003(5) 0.011(4) N5 0.057(7) 0.094(11) 0.069(8) 0.008(6) -0.017(5) -0.010(5) N6 0.071(6) 0.045(5) 0.075(6) 0.004(5) 0.001(5) -0.010(5) O1 0.056(5) 0.046(5) 0.059(5) -0.005(3) -0.008(3) -0.006(3) C2 0.066(7) 0.046(6) 0.066(7) -0.013(5) -0.005(6) 0.002(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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' S S 0.1246 0.1234 '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 N1 C1 Co1 177.7(11) N3 C3 Co1 178.6(11) N4 C4 Co1 175.4(12) N5 C5 Co1 179.0(12) N6 C6 Co1 175.3(11) C9 N7 C7 112(4) C9 N7 H7A 123.8 C7 N7 H7A 123.8 N7 C7 S1 109(3) N7 C7 H7 125.6 S1 C7 H7 125.6 C7 S1 C8 89(3) C9 C8 S1 122(5) C9 C8 H8 119.1 S1 C8 H8 119.1 C8 C9 N7 108(5) C8 C9 H9 125.8 N7 C9 H9 125.8 C7' N7' C9' 113(2) C7' N7' H7A' 123.7 C9' N7' H7A' 123.7 N7' C7' S1' 107.5(18) N7' C7' H7' 126.3 S1' C7' H7' 126.3 C7' S1' C8' 98.7(16) C9' C8' S1' 107(2) C9' C8' H8' 126.3 S1' C8' H8' 126.3 C8' C9' N7' 114(3) C8' C9' H9' 123.1 N7' C9' H9' 123.1 C12 N8 C10 103(4) C12 N8 H8A 128.3 C10 N8 H8A 128.3 N8 C10 S2 109(3) N8 C10 H10 125.5 S2 C10 H10 125.5 C11 S2 C10 97.2(18) C12 C11 S2 103(3) C12 C11 H11 128.3 S2 C11 H11 128.3 N8 C12 C11 127(4) N8 C12 H12 116.5 C11 C12 H12 116.5 C10' N8' C12' 113(2) C10' N8' H8A' 123.6 C12' N8' H8A' 123.6 N8' C10' S2' 113(2) N8' C10' H10' 123.5 S2' C10' H10' 123.5 C10' S2' C11' 93.5(12) C12' C11' S2' 104.5(16) C12' C11' H11' 127.8 S2' C11' H11' 127.8 C11' C12' N8' 116.1(19) C11' C12' H12' 121.9 N8' C12' H12' 121.9 C3 Co1 C5 90.0(5) C3 Co1 C2 88.3(6) C5 Co1 C2 178.2(6) C3 Co1 C1 88.1(5) C5 Co1 C1 90.5(5) C2 Co1 C1 88.8(5) C3 Co1 C4 89.5(5) C5 Co1 C4 88.7(5) C2 Co1 C4 92.0(5) C1 Co1 C4 177.5(5) C3 Co1 C6 177.6(5) C5 Co1 C6 89.3(4) C2 Co1 C6 92.3(5) C1 Co1 C6 89.6(4) C4 Co1 C6 92.8(5) H1A O1 H1B 109.6 H1A O1 H1C 109.0 H1B O1 H1C 108.5 N2 C2 Co1 174.3(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.128(15) C1 Co1 1.914(12) C3 N3 1.150(18) C3 Co1 1.875(12) C4 N4 1.138(15) C4 Co1 1.917(12) C5 N5 1.144(15) C5 Co1 1.908(11) C6 N6 1.124(15) C6 Co1 1.917(11) N7 C9 1.40(5) N7 C7 1.45(7) N7 H7A 0.8600 C7 S1 1.67(2) C7 H7 0.9300 S1 C8 1.68(3) C8 C9 1.21(8) C8 H8 0.9300 C9 H9 0.9300 N7' C7' 1.37(4) N7' C9' 1.42(2) N7' H7A' 0.8600 C7' S1' 1.641(18) C7' H7' 0.9300 S1' C8' 1.64(2) C8' C9' 1.35(3) C8' H8' 0.9300 C9' H9' 0.9300 N8 C12 1.30(2) N8 C10 1.46(3) N8 H8A 0.8600 C10 S2 1.74(3) C10 H10 0.9300 S2 C11 1.59(2) C11 C12 1.40(3) C11 H11 0.9300 C12 H12 0.9300 N8' C10' 1.31(2) N8' C12' 1.51(2) N8' H8A' 0.8600 C10' S2' 1.63(2) C10' H10' 0.9300 S2' C11' 1.896(19) C11' C12' 1.27(2) C11' H11' 0.9300 C12' H12' 0.9300 Co1 C2 1.913(13) N2 C2 1.155(17) O1 H1A 0.8532 O1 H1B 0.8525 O1 H1C 0.8477 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 N7 H7A N3 0.86 2.43 3.22(5) 152.9 2_654 N7' H7A' N3 0.86 2.39 3.20(3) 156.8 2_654 N8 H8A N5 0.86 2.59 3.35(4) 146.7 1_565 N8' H8A' N3 0.86 2.45 3.14(2) 137.6 3 O1 H1A N4 0.85 1.77 2.620(14) 176.5 1_565 O1 H1B N6 0.85 1.77 2.621(13) 173.4 . O1 H1C N2 0.85 1.75 2.594(14) 172.2 3 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 C9 N7 C7 S1 0.0(3) N7 C7 S1 C8 -0.1(2) C7 S1 C8 C9 0.3(6) S1 C8 C9 N7 -0.3(8) C7 N7 C9 C8 0.2(6) C9' N7' C7' S1' -0.1(3) N7' C7' S1' C8' -0.2(2) C7' S1' C8' C9' 0.4(5) S1' C8' C9' N7' -0.5(7) C7' N7' C9' C8' 0.4(6) C12 N8 C10 S2 -0.1(3) N8 C10 S2 C11 -0.1(2) C10 S2 C11 C12 0.2(4) C10 N8 C12 C11 0.4(7) S2 C11 C12 N8 -0.4(8) C12' N8' C10' S2' -0.1(3) N8' C10' S2' C11' 0.0(2) C10' S2' C11' C12' 0.1(5) S2' C11' C12' N8' -0.1(7) C10' N8' C12' C11' 0.2(7)