#------------------------------------------------------------------------------ #$Date: 2017-02-21 09:16:28 +0200 (Tue, 21 Feb 2017) $ #$Revision: 192407 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/53/1545300.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_1545300 loop_ _publ_author_name 'Chen, Huafeng' 'Pan, Weijing' 'Huang, Kuo-Wei' 'Zhang, Xuequan' 'Gong, Dirong' _publ_section_title ; Controlled polymerization of isoprene promoted by a type of hemilabile X=PN3 (X=O, S) ligand supported cobalt (II) complexes: the role of hemilabile donor on the level of control ; _journal_name_full 'Polym. Chem.' _journal_paper_doi 10.1039/C7PY00252A _journal_year 2017 _chemical_formula_moiety 'C44 H42 Cl4 Co2 N8 P2 S2' _chemical_formula_sum 'C44 H42 Cl4 Co2 N8 P2 S2' _chemical_formula_weight 1068.58 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2016-08-31 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221) ; _audit_update_record ; 2016-11-23 deposited with the CCDC. 2017-02-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.147(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.4650(10) _cell_length_b 15.7090(16) _cell_length_c 16.2919(16) _cell_measurement_reflns_used 2694 _cell_measurement_temperature 173 _cell_measurement_theta_max 27.148 _cell_measurement_theta_min 2.593 _cell_volume 2326.8(4) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 173 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_unetI/netI 0.0674 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 13806 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.572 _diffrn_reflns_theta_min 2.588 _exptl_absorpt_coefficient_mu 1.144 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.525 _exptl_crystal_description block _exptl_crystal_F_000 1092 _refine_diff_density_max 0.416 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 282 _refine_ls_number_reflns 5257 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.995 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0412 _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^)+(0.0414P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.0931 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3738 _reflns_number_total 5257 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7py00252a2.cif _cod_data_source_block gdr47_0m _cod_database_code 1545300 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Riding coordinates: N4(H4) 2.b Aromatic/amide H refined with riding coordinates: C4(H4A), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19) 2.c Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C) ; _shelx_res_file ; gdr47_0m.res created by SHELXL-2014/7 TITL gdr47_0m P 1 21/n 1 R = 0.04 CELL 0.71073 9.465 15.709 16.2919 90 106.147 90 ZERR 2 0.001 0.0016 0.0016 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C 2.310 20.844 1.02 10.208 1.589 0.569 0.865 51.651 0.216 0.003 0.002 = 11.5 0.68 12.01 SFAC H 0.493 10.511 0.323 26.126 0.14 3.142 0.041 57.8 0.003 0 0 0.624 0.35 = 1.008 SFAC Cl SFAC Co 12.284 4.279 7.341 0.278 4.003 13.536 2.349 71.169 1.012 0.349 = 0.972 4010 1.23 58.93 SFAC N 12.213 0.006 3.132 9.893 2.013 28.998 1.166 0.583 -11.529 0.006 = 0.003 19.6 0.68 14.01 SFAC P 6.435 1.907 4.179 27.157 1.78 0.526 1.491 68.165 1.115 0.102 0.094 = 410 1.05 30.97 SFAC S 6.905 1.468 5.203 22.215 1.438 0.254 1.586 56.172 0.867 0.125 0.123 = 532 1.04 32.06 UNIT 88 84 8 4 16 4 4 L.S. 5 PLAN -20 TEMP -100 BOND $H CONF MORE -1 fmap 2 acta OMIT 0 1 1 REM REM REM WGHT 0.041400 FVAR 0.40559 CO1 4 0.147828 0.475718 0.591440 11.00000 0.01373 0.01727 = 0.01540 -0.00074 0.00459 -0.00202 CL2 3 0.081002 0.440150 0.446054 11.00000 0.01451 0.03125 = 0.01937 -0.00595 0.00293 0.00302 CL1 3 0.080880 0.379331 0.677087 11.00000 0.04500 0.02489 = 0.04511 0.00905 0.03317 0.00431 S3 7 0.461029 0.112111 0.640028 11.00000 0.02745 0.03084 = 0.02669 0.00408 0.00024 0.00924 P1 6 0.293098 0.168425 0.563943 11.00000 0.01682 0.01472 = 0.02019 0.00021 0.00478 0.00082 N1 5 0.298113 0.570095 0.635368 11.00000 0.01463 0.02001 = 0.01650 0.00073 0.00318 0.00234 N2 5 0.442469 0.548497 0.643321 11.00000 0.01304 0.01622 = 0.01761 -0.00117 0.00360 -0.00011 N3 5 0.364588 0.411836 0.603558 11.00000 0.01306 0.01514 = 0.01354 0.00039 0.00192 -0.00147 N4 5 0.279133 0.274086 0.577979 11.00000 0.01268 0.01545 = 0.02954 -0.00196 0.00791 -0.00134 AFIX 3 H4 2 0.196933 0.293176 0.586649 11.00000 -1.20000 AFIX 0 C1 1 0.472180 0.469148 0.610691 11.00000 0.01589 0.01636 = 0.01400 0.00251 0.00248 -0.00012 C2 1 0.387682 0.333111 0.577134 11.00000 0.01621 0.01554 = 0.01561 0.00049 0.00454 0.00018 C3 1 0.292375 0.158608 0.453074 11.00000 0.01682 0.01360 = 0.02224 -0.00077 0.00526 -0.00248 C4 1 0.398723 0.110354 0.430077 11.00000 0.02378 0.01539 = 0.03108 0.00071 0.01059 0.00273 AFIX 43 H4A 2 0.471274 0.080833 0.472633 11.00000 -1.20000 AFIX 0 C5 1 0.398885 0.105322 0.345058 11.00000 0.03225 0.02258 = 0.03759 -0.00515 0.02036 -0.00160 AFIX 43 H5 2 0.473296 0.073672 0.329794 11.00000 -1.20000 AFIX 0 C6 1 0.292223 0.145792 0.283044 11.00000 0.03862 0.02672 = 0.02166 -0.00684 0.01114 -0.01024 AFIX 43 H6 2 0.292473 0.141425 0.224925 11.00000 -1.20000 AFIX 0 C7 1 0.183975 0.193044 0.304405 11.00000 0.02673 0.03492 = 0.02456 0.00554 0.00202 -0.00360 AFIX 43 H7 2 0.109420 0.220306 0.261083 11.00000 -1.20000 AFIX 0 C8 1 0.185178 0.200295 0.389605 11.00000 0.01751 0.02670 = 0.02801 0.00209 0.00630 0.00098 AFIX 43 H8 2 0.112640 0.233806 0.404673 11.00000 -1.20000 AFIX 0 C9 1 0.117141 0.132539 0.573676 11.00000 0.02633 0.01848 = 0.02235 -0.00860 0.01164 -0.00784 C10 1 -0.009759 0.180567 0.544011 11.00000 0.02166 0.03362 = 0.03613 -0.00495 0.01003 -0.00435 AFIX 43 H10 2 -0.004707 0.235419 0.520437 11.00000 -1.20000 AFIX 0 C11 1 -0.144790 0.148617 0.548667 11.00000 0.02689 0.04797 = 0.05740 -0.01613 0.02074 -0.00978 AFIX 43 H11 2 -0.231715 0.181323 0.527371 11.00000 -1.20000 AFIX 0 C12 1 -0.152282 0.070191 0.583880 11.00000 0.03870 0.05074 = 0.06010 -0.02795 0.03158 -0.02521 AFIX 43 H12 2 -0.244367 0.048773 0.587252 11.00000 -1.20000 AFIX 0 C13 1 -0.026813 0.022240 0.614430 11.00000 0.07106 0.02639 = 0.04840 -0.01211 0.03692 -0.02724 AFIX 43 H13 2 -0.032804 -0.032148 0.638739 11.00000 -1.20000 AFIX 0 C14 1 0.108515 0.052957 0.609902 11.00000 0.04325 0.02049 = 0.03222 -0.00448 0.01860 -0.00678 AFIX 43 H14 2 0.194887 0.019837 0.631420 11.00000 -1.20000 AFIX 0 C15 1 0.513660 0.312527 0.552560 11.00000 0.01785 0.01857 = 0.02771 -0.00513 0.00862 0.00163 AFIX 43 H15 2 0.526764 0.256814 0.533208 11.00000 -1.20000 AFIX 0 C16 1 0.618282 0.374310 0.556880 11.00000 0.01514 0.02467 = 0.02252 0.00117 0.00956 0.00292 AFIX 43 H16 2 0.703281 0.361846 0.538898 11.00000 -1.20000 AFIX 0 C17 1 0.600127 0.454785 0.587411 11.00000 0.01381 0.01988 = 0.02157 0.00256 0.00454 -0.00284 AFIX 43 H17 2 0.672103 0.498036 0.592132 11.00000 -1.20000 AFIX 0 C18 1 0.536105 0.610322 0.686008 11.00000 0.01808 0.01794 = 0.02021 0.00099 0.00213 -0.00309 C19 1 0.448672 0.673336 0.703252 11.00000 0.02237 0.01470 = 0.02409 -0.00475 0.00324 -0.00241 AFIX 43 H19 2 0.481258 0.725565 0.731611 11.00000 -1.20000 AFIX 0 C20 1 0.303822 0.647004 0.671760 11.00000 0.01905 0.01707 = 0.01609 0.00005 0.00195 0.00027 C21 1 0.170163 0.694312 0.675806 11.00000 0.02061 0.02671 = 0.03049 -0.00760 0.00645 0.00162 AFIX 137 H21A 2 0.107883 0.704906 0.617722 11.00000 -1.50000 H21B 2 0.198954 0.748725 0.705106 11.00000 -1.50000 H21C 2 0.115410 0.660538 0.707262 11.00000 -1.50000 AFIX 0 C22 1 0.699872 0.603454 0.712480 11.00000 0.01519 0.02964 = 0.03306 -0.00928 0.00253 -0.00388 AFIX 137 H22A 2 0.728643 0.545548 0.732719 11.00000 -1.50000 H22B 2 0.740978 0.644118 0.758552 11.00000 -1.50000 H22C 2 0.737504 0.616189 0.663546 11.00000 -1.50000 AFIX 0 HKLF 4 REM gdr47_0m P 1 21/n 1 R = 0.04 REM R1 = 0.0412 for 3738 Fo > 4sig(Fo) and 0.0720 for all 5257 data REM 282 parameters refined using 0 restraints END WGHT 0.0414 0.0000 REM Highest difference peak 0.416, deepest hole -0.507, 1-sigma level 0.090 Q1 1 0.3706 0.1979 0.2119 11.00000 0.05 0.42 Q2 1 0.3011 0.1639 0.5092 11.00000 0.05 0.41 Q3 1 0.0761 0.3752 0.4891 11.00000 0.05 0.36 Q4 1 0.0669 0.4845 0.6418 11.00000 0.05 0.35 Q5 1 0.5010 0.5815 0.6545 11.00000 0.05 0.35 Q6 1 0.5210 0.4643 0.5741 11.00000 0.05 0.34 Q7 1 0.4312 0.4311 0.6061 11.00000 0.05 0.34 Q8 1 0.2824 0.2233 0.5716 11.00000 0.05 0.34 Q9 1 0.3684 0.6792 0.6709 11.00000 0.05 0.34 Q10 1 0.0988 0.6682 0.6479 11.00000 0.05 0.33 Q11 1 0.2814 0.1977 0.4046 11.00000 0.05 0.33 Q12 1 0.1895 0.4338 0.6563 11.00000 0.05 0.32 Q13 1 0.2209 0.5187 0.6681 11.00000 0.05 0.32 Q14 1 0.4737 0.1779 0.3033 11.00000 0.05 0.32 Q15 1 0.6817 0.6567 0.7495 11.00000 0.05 0.32 Q16 1 0.7549 0.5628 0.7990 11.00000 0.05 0.32 Q17 1 0.2876 0.4295 0.6413 11.00000 0.05 0.31 Q18 1 0.5380 0.6410 0.6721 11.00000 0.05 0.31 Q19 1 0.3500 0.1456 0.4390 11.00000 0.05 0.31 Q20 1 0.2203 0.2862 0.6264 11.00000 0.05 0.31 ; _shelx_res_checksum 59924 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Co1 Co 0.14783(4) 0.47572(2) 0.59144(2) 0.01536(11) Uani 1 1 d . Cl2 Cl 0.08100(7) 0.44015(5) 0.44605(5) 0.02207(17) Uani 1 1 d . Cl1 Cl 0.08088(9) 0.37933(5) 0.67709(6) 0.0342(2) Uani 1 1 d . S3 S 0.46103(9) 0.11211(5) 0.64003(5) 0.0298(2) Uani 1 1 d . P1 P 0.29310(8) 0.16842(5) 0.56394(5) 0.01732(17) Uani 1 1 d . N1 N 0.2981(2) 0.57009(15) 0.63537(14) 0.0173(5) Uani 1 1 d . N2 N 0.4425(2) 0.54850(14) 0.64332(14) 0.0158(5) Uani 1 1 d . N3 N 0.3646(2) 0.41184(14) 0.60356(14) 0.0143(5) Uani 1 1 d . N4 N 0.2791(2) 0.27409(14) 0.57798(15) 0.0188(5) Uani 1 1 d . H4 H 0.1969 0.2932 0.5866 0.023 Uiso 1 1 d R C1 C 0.4722(3) 0.46915(17) 0.61069(17) 0.0158(6) Uani 1 1 d . C2 C 0.3877(3) 0.33311(17) 0.57713(17) 0.0158(6) Uani 1 1 d . C3 C 0.2924(3) 0.15861(17) 0.45307(18) 0.0176(6) Uani 1 1 d . C4 C 0.3987(3) 0.11035(18) 0.4301(2) 0.0228(7) Uani 1 1 d . H4A H 0.4713 0.0808 0.4726 0.027 Uiso 1 1 calc R C5 C 0.3989(3) 0.10532(19) 0.3451(2) 0.0287(7) Uani 1 1 d . H5 H 0.4733 0.0737 0.3298 0.034 Uiso 1 1 calc R C6 C 0.2922(4) 0.14579(19) 0.2830(2) 0.0284(7) Uani 1 1 d . H6 H 0.2925 0.1414 0.2249 0.034 Uiso 1 1 calc R C7 C 0.1840(3) 0.1930(2) 0.3044(2) 0.0298(8) Uani 1 1 d . H7 H 0.1094 0.2203 0.2611 0.036 Uiso 1 1 calc R C8 C 0.1852(3) 0.20030(19) 0.38961(19) 0.0241(7) Uani 1 1 d . H8 H 0.1126 0.2338 0.4047 0.029 Uiso 1 1 calc R C9 C 0.1171(3) 0.13254(18) 0.57368(19) 0.0214(7) Uani 1 1 d . C10 C -0.0098(3) 0.1806(2) 0.5440(2) 0.0301(8) Uani 1 1 d . H10 H -0.0047 0.2354 0.5204 0.036 Uiso 1 1 calc R C11 C -0.1448(4) 0.1486(2) 0.5487(2) 0.0423(10) Uani 1 1 d . H11 H -0.2317 0.1813 0.5274 0.051 Uiso 1 1 calc R C12 C -0.1523(4) 0.0702(3) 0.5839(3) 0.0463(10) Uani 1 1 d . H12 H -0.2444 0.0488 0.5873 0.056 Uiso 1 1 calc R C13 C -0.0268(5) 0.0222(2) 0.6144(2) 0.0445(10) Uani 1 1 d . H13 H -0.0328 -0.0321 0.6387 0.053 Uiso 1 1 calc R C14 C 0.1085(4) 0.05296(19) 0.6099(2) 0.0304(8) Uani 1 1 d . H14 H 0.1949 0.0198 0.6314 0.036 Uiso 1 1 calc R C15 C 0.5137(3) 0.31253(18) 0.55256(19) 0.0209(7) Uani 1 1 d . H15 H 0.5268 0.2568 0.5332 0.025 Uiso 1 1 calc R C16 C 0.6183(3) 0.37431(18) 0.55688(19) 0.0199(6) Uani 1 1 d . H16 H 0.7033 0.3618 0.5389 0.024 Uiso 1 1 calc R C17 C 0.6001(3) 0.45479(18) 0.58741(18) 0.0185(6) Uani 1 1 d . H17 H 0.6721 0.4980 0.5921 0.022 Uiso 1 1 calc R C18 C 0.5361(3) 0.61032(18) 0.68601(18) 0.0194(6) Uani 1 1 d . C19 C 0.4487(3) 0.67334(18) 0.70325(19) 0.0210(6) Uani 1 1 d . H19 H 0.4813 0.7256 0.7316 0.025 Uiso 1 1 calc R C20 C 0.3038(3) 0.64700(17) 0.67176(18) 0.0180(6) Uani 1 1 d . C21 C 0.1702(3) 0.69431(19) 0.6758(2) 0.0261(7) Uani 1 1 d . H21A H 0.1079 0.7049 0.6177 0.039 Uiso 1 1 calc GR H21B H 0.1990 0.7487 0.7051 0.039 Uiso 1 1 calc GR H21C H 0.1154 0.6605 0.7073 0.039 Uiso 1 1 calc GR C22 C 0.6999(3) 0.6035(2) 0.7125(2) 0.0268(7) Uani 1 1 d . H22A H 0.7286 0.5455 0.7327 0.040 Uiso 1 1 calc GR H22B H 0.7410 0.6441 0.7586 0.040 Uiso 1 1 calc GR H22C H 0.7375 0.6162 0.6635 0.040 Uiso 1 1 calc GR loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01373(19) 0.0173(2) 0.0154(2) -0.00074(16) 0.00459(15) -0.00202(15) Cl2 0.0145(3) 0.0313(4) 0.0194(4) -0.0059(3) 0.0029(3) 0.0030(3) Cl1 0.0450(5) 0.0249(4) 0.0451(5) 0.0091(4) 0.0332(4) 0.0043(4) S3 0.0275(4) 0.0308(5) 0.0267(4) 0.0041(4) 0.0002(4) 0.0092(3) P1 0.0168(4) 0.0147(4) 0.0202(4) 0.0002(3) 0.0048(3) 0.0008(3) N1 0.0146(12) 0.0200(13) 0.0165(13) 0.0007(10) 0.0032(10) 0.0023(10) N2 0.0130(11) 0.0162(12) 0.0176(13) -0.0012(10) 0.0036(10) -0.0001(9) N3 0.0131(11) 0.0151(12) 0.0135(12) 0.0004(9) 0.0019(10) -0.0015(9) N4 0.0127(11) 0.0155(12) 0.0295(14) -0.0020(10) 0.0079(11) -0.0013(9) C1 0.0159(14) 0.0164(14) 0.0140(14) 0.0025(12) 0.0025(12) -0.0001(11) C2 0.0162(14) 0.0155(14) 0.0156(14) 0.0005(12) 0.0045(12) 0.0002(11) C3 0.0168(14) 0.0136(14) 0.0222(16) -0.0008(12) 0.0053(12) -0.0025(11) C4 0.0238(16) 0.0154(15) 0.0311(18) 0.0007(13) 0.0106(14) 0.0027(12) C5 0.0323(18) 0.0226(17) 0.038(2) -0.0052(15) 0.0204(16) -0.0016(13) C6 0.0386(19) 0.0267(18) 0.0217(17) -0.0068(14) 0.0111(15) -0.0102(14) C7 0.0267(17) 0.0349(19) 0.0246(18) 0.0055(15) 0.0020(14) -0.0036(14) C8 0.0175(15) 0.0267(17) 0.0280(18) 0.0021(14) 0.0063(13) 0.0010(12) C9 0.0263(16) 0.0185(16) 0.0224(17) -0.0086(12) 0.0116(14) -0.0078(12) C10 0.0217(16) 0.0336(19) 0.036(2) -0.0049(15) 0.0100(15) -0.0043(14) C11 0.0269(19) 0.048(2) 0.057(3) -0.016(2) 0.0207(18) -0.0098(16) C12 0.039(2) 0.051(3) 0.060(3) -0.028(2) 0.032(2) -0.0252(19) C13 0.071(3) 0.0264(19) 0.048(2) -0.0121(17) 0.037(2) -0.0272(19) C14 0.043(2) 0.0205(17) 0.032(2) -0.0045(14) 0.0186(17) -0.0068(14) C15 0.0179(14) 0.0186(16) 0.0277(17) -0.0051(13) 0.0086(13) 0.0016(12) C16 0.0151(14) 0.0247(17) 0.0225(16) 0.0012(13) 0.0096(13) 0.0029(12) C17 0.0138(14) 0.0199(16) 0.0216(16) 0.0026(12) 0.0045(12) -0.0028(11) C18 0.0181(14) 0.0179(15) 0.0202(16) 0.0010(12) 0.0021(13) -0.0031(12) C19 0.0224(15) 0.0147(15) 0.0241(16) -0.0047(13) 0.0032(13) -0.0024(12) C20 0.0190(14) 0.0171(15) 0.0161(15) 0.0000(12) 0.0019(12) 0.0003(11) C21 0.0206(15) 0.0267(17) 0.0305(18) -0.0076(14) 0.0065(14) 0.0016(13) C22 0.0152(15) 0.0296(18) 0.0331(19) -0.0093(14) 0.0025(14) -0.0039(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 '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_3 Cl2 Co1 Cl2 84.59(3) 3_566 Cl1 Co1 Cl2 97.70(3) 3_566 Cl1 Co1 Cl2 114.84(3) . N1 Co1 Cl2 119.57(7) . N1 Co1 Cl2 100.14(7) 3_566 N1 Co1 Cl1 123.81(7) . N1 Co1 N3 76.29(8) . N3 Co1 Cl2 88.02(6) . N3 Co1 Cl2 168.82(6) 3_566 N3 Co1 Cl1 93.01(6) . Co1 Cl2 Co1 95.41(3) 3_566 N4 P1 S3 116.38(9) . N4 P1 C3 103.91(12) . N4 P1 C9 100.74(12) . C3 P1 S3 111.98(10) . C9 P1 S3 114.45(11) . C9 P1 C3 108.25(13) . N2 N1 Co1 115.47(16) . C20 N1 Co1 138.43(19) . C20 N1 N2 105.3(2) . N1 N2 C1 118.5(2) . C18 N2 N1 111.0(2) . C18 N2 C1 130.5(2) . C1 N3 Co1 111.20(17) . C1 N3 C2 117.2(2) . C2 N3 Co1 127.47(17) . P1 N4 H4 117.6 . C2 N4 P1 124.80(19) . C2 N4 H4 117.6 . N3 C1 N2 113.5(2) . N3 C1 C17 124.6(3) . C17 C1 N2 121.8(2) . N3 C2 N4 115.1(2) . N3 C2 C15 122.1(2) . N4 C2 C15 122.8(2) . C4 C3 P1 120.8(2) . C4 C3 C8 119.2(3) . C8 C3 P1 120.0(2) . C3 C4 H4A 120.0 . C5 C4 C3 120.1(3) . C5 C4 H4A 120.0 . C4 C5 H5 119.9 . C6 C5 C4 120.3(3) . C6 C5 H5 119.9 . C5 C6 H6 119.7 . C5 C6 C7 120.5(3) . C7 C6 H6 119.7 . C6 C7 H7 120.2 . C6 C7 C8 119.6(3) . C8 C7 H7 120.2 . C3 C8 H8 119.9 . C7 C8 C3 120.3(3) . C7 C8 H8 119.9 . C10 C9 P1 122.0(2) . C10 C9 C14 119.2(3) . C14 C9 P1 118.7(2) . C9 C10 H10 119.9 . C9 C10 C11 120.2(3) . C11 C10 H10 119.9 . C10 C11 H11 119.9 . C12 C11 C10 120.1(4) . C12 C11 H11 119.9 . C11 C12 H12 119.9 . C11 C12 C13 120.2(3) . C13 C12 H12 119.9 . C12 C13 H13 119.8 . C12 C13 C14 120.4(3) . C14 C13 H13 119.8 . C9 C14 H14 120.1 . C13 C14 C9 119.8(3) . C13 C14 H14 120.1 . C2 C15 H15 120.6 . C16 C15 C2 118.8(3) . C16 C15 H15 120.6 . C15 C16 H16 119.9 . C15 C16 C17 120.2(3) . C17 C16 H16 119.9 . C1 C17 C16 116.9(3) . C1 C17 H17 121.6 . C16 C17 H17 121.6 . N2 C18 C19 105.9(2) . N2 C18 C22 124.7(3) . C19 C18 C22 129.2(3) . C18 C19 H19 126.3 . C18 C19 C20 107.5(3) . C20 C19 H19 126.3 . N1 C20 C19 110.3(2) . N1 C20 C21 122.7(2) . C19 C20 C21 127.0(3) . C20 C21 H21A 109.5 . C20 C21 H21B 109.5 . C20 C21 H21C 109.5 . H21A C21 H21B 109.5 . H21A C21 H21C 109.5 . H21B C21 H21C 109.5 . C18 C22 H22A 109.5 . C18 C22 H22B 109.5 . C18 C22 H22C 109.5 . H22A C22 H22B 109.5 . H22A C22 H22C 109.5 . H22B C22 H22C 109.5 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 Cl2 2.3429(8) . Co1 Cl2 2.4648(8) 3_566 Co1 Cl1 2.2656(9) . Co1 N1 2.041(2) . Co1 N3 2.243(2) . Cl2 Co1 2.4647(8) 3_566 S3 P1 1.9364(11) . P1 N4 1.686(2) . P1 C3 1.811(3) . P1 C9 1.807(3) . N1 N2 1.379(3) . N1 C20 1.340(3) . N2 C1 1.414(3) . N2 C18 1.367(3) . N3 C1 1.340(3) . N3 C2 1.347(3) . N4 H4 0.8811 . N4 C2 1.387(3) . C1 C17 1.384(4) . C2 C15 1.397(4) . C3 C4 1.392(4) . C3 C8 1.394(4) . C4 H4A 0.9500 . C4 C5 1.388(4) . C5 H5 0.9500 . C5 C6 1.370(4) . C6 H6 0.9500 . C6 C7 1.386(4) . C7 H7 0.9500 . C7 C8 1.390(4) . C8 H8 0.9500 . C9 C10 1.387(4) . C9 C14 1.395(4) . C10 H10 0.9500 . C10 C11 1.395(4) . C11 H11 0.9500 . C11 C12 1.369(5) . C12 H12 0.9500 . C12 C13 1.377(5) . C13 H13 0.9500 . C13 C14 1.390(5) . C14 H14 0.9500 . C15 H15 0.9500 . C15 C16 1.374(4) . C16 H16 0.9500 . C16 C17 1.387(4) . C17 H17 0.9500 . C18 C19 1.369(4) . C18 C22 1.493(4) . C19 H19 0.9500 . C19 C20 1.387(4) . C20 C21 1.484(4) . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 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 Co1 N1 N2 C1 8.2(3) Co1 N1 N2 C18 -169.97(18) Co1 N1 C20 C19 167.6(2) Co1 N1 C20 C21 -12.4(5) Co1 N3 C1 N2 24.4(3) Co1 N3 C1 C17 -154.4(2) Co1 N3 C2 N4 -30.4(3) Co1 N3 C2 C15 151.0(2) S3 P1 N4 C2 55.2(3) S3 P1 C3 C4 3.9(3) S3 P1 C3 C8 -175.5(2) S3 P1 C9 C10 160.9(2) S3 P1 C9 C14 -21.0(3) P1 N4 C2 N3 -169.43(19) P1 N4 C2 C15 9.2(4) P1 C3 C4 C5 -178.3(2) P1 C3 C8 C7 180.0(2) P1 C9 C10 C11 176.6(3) P1 C9 C14 C13 -177.0(2) N1 N2 C1 N3 -22.8(3) N1 N2 C1 C17 156.0(2) N1 N2 C18 C19 -1.7(3) N1 N2 C18 C22 174.1(3) N2 N1 C20 C19 -0.8(3) N2 N1 C20 C21 179.2(3) N2 C1 C17 C16 179.5(3) N2 C18 C19 C20 1.1(3) N3 C1 C17 C16 -1.9(4) N3 C2 C15 C16 1.1(4) N4 P1 C3 C4 130.3(2) N4 P1 C3 C8 -49.1(3) N4 P1 C9 C10 35.3(3) N4 P1 C9 C14 -146.7(2) N4 C2 C15 C16 -177.5(3) C1 N2 C18 C19 -179.5(3) C1 N2 C18 C22 -3.7(5) C1 N3 C2 N4 174.5(2) C1 N3 C2 C15 -4.1(4) C2 N3 C1 N2 -176.6(2) C2 N3 C1 C17 4.6(4) C2 C15 C16 C17 1.8(4) C3 P1 N4 C2 -68.4(2) C3 P1 C9 C10 -73.4(3) C3 P1 C9 C14 104.7(3) C3 C4 C5 C6 -1.8(4) C4 C3 C8 C7 0.6(4) C4 C5 C6 C7 0.8(5) C5 C6 C7 C8 0.9(5) C6 C7 C8 C3 -1.6(4) C8 C3 C4 C5 1.1(4) C9 P1 N4 C2 179.5(2) C9 P1 C3 C4 -123.2(2) C9 P1 C3 C8 57.4(3) C9 C10 C11 C12 1.1(5) C10 C9 C14 C13 1.1(5) C10 C11 C12 C13 -0.4(6) C11 C12 C13 C14 0.1(6) C12 C13 C14 C9 -0.4(5) C14 C9 C10 C11 -1.5(5) C15 C16 C17 C1 -1.4(4) C18 N2 C1 N3 154.9(3) C18 N2 C1 C17 -26.3(4) C18 C19 C20 N1 -0.2(3) C18 C19 C20 C21 179.9(3) C20 N1 N2 C1 179.7(2) C20 N1 N2 C18 1.5(3) C22 C18 C19 C20 -174.4(3)