#------------------------------------------------------------------------------ #$Date: 2020-02-08 07:10:01 +0200 (Sat, 08 Feb 2020) $ #$Revision: 247975 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557270.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_1557270 loop_ _publ_author_name 'Xu, Yuechao' 'zhao, Junyi' 'Gan, Qiao' 'Ying, Weilun' 'Hu, Zhonghan' 'Tang, Fuming' 'Luo, Wanwei' 'Luo, Yunjie' 'Jian, Zhongbao' 'Gong, Dirong' _publ_section_title ; Synthesis and properties investigation of hydroxyl functionalized polyisoprene prepared by cobalt catalyzed co-polymerization of isoprene and hydroxylmyrcene ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/C9PY01808E _journal_year 2020 _chemical_formula_moiety 'C17 H30 Cl2 Co N3 O3 P' _chemical_formula_sum 'C17 H30 Cl2 Co N3 O3 P' _chemical_formula_weight 485.24 _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_creation_date 2017-11-08 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _audit_update_record ; 2017-12-10 deposited with the CCDC. 2020-02-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.858(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.5582(3) _cell_length_b 8.70090(10) _cell_length_c 16.7290(3) _cell_measurement_reflns_used 5722 _cell_measurement_temperature 296 _cell_measurement_theta_max 73.7900 _cell_measurement_theta_min 5.7070 _cell_volume 2236.90(7) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _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 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.0 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 42.00 88.00 0.50 0.50 -- 0.00 38.00-180.00 92 2 \w -60.00 -35.00 0.50 0.50 -- 0.00 -38.00 -90.00 50 3 \w -15.00 29.00 0.50 0.50 -- 0.00 38.00 60.00 88 4 \w -86.00 22.00 0.50 0.50 -- 0.00 -57.00-180.00 216 5 \w 59.00 84.00 0.50 0.50 -- 0.00 38.00 60.00 50 6 \w 44.00 119.00 0.50 1.98 -- 95.20 -61.00-150.00 150 7 \w 64.00 109.00 0.50 1.98 -- 95.20 -30.00-120.00 90 8 \w 79.00 154.00 0.50 1.98 -- 95.20 30.00-150.00 150 9 \w 52.00 118.00 0.50 1.98 -- 95.20 -82.00-150.00 132 10 \w 72.00 161.00 0.50 1.98 -- 95.20 15.00 -30.00 178 11 \w 9.00 111.00 0.50 1.98 -- 95.20 -61.00 60.00 204 12 \w 147.00 175.00 0.50 1.98 -- 95.20 15.00 30.00 56 13 \w 80.00 106.00 0.50 1.98 -- 95.20 15.00 30.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0552609000 _diffrn_orient_matrix_UB_12 -0.0705689000 _diffrn_orient_matrix_UB_13 -0.0879342000 _diffrn_orient_matrix_UB_21 0.0681814000 _diffrn_orient_matrix_UB_22 0.0523403000 _diffrn_orient_matrix_UB_23 -0.0366520000 _diffrn_orient_matrix_UB_31 0.0485280000 _diffrn_orient_matrix_UB_32 -0.1536160000 _diffrn_orient_matrix_UB_33 0.0278930000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 11707 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.093 _diffrn_reflns_theta_min 2.875 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.073 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.12401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.441 _exptl_crystal_description block _exptl_crystal_F_000 1012 _refine_diff_density_max 0.302 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 4399 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0354 _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^)+(0.0446P)^2^+0.3559P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.0881 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3744 _reflns_number_total 4399 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9py01808e2.cif _cod_data_source_block lwx-1-1 _cod_database_code 1557270 _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. ; _reflns_odcompleteness_completeness 99.88 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O1-H1 0.85 with sigma of 0.01 C17-H1 1.901768 with sigma of 0.02 Co1-H1 2.759685 with sigma of 0.02 3.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B) 3.b Aromatic/amide H refined with riding coordinates: N3(H3), C5(H5), C6(H6), C7(H7) 3.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C) ; _shelx_res_file ; TITL lwx-1-1_a.res in P2(1)/c lwx-1-1.res created by SHELXL-2016/6 at 11:06:08 on 08-Nov-2017 REM Old TITL lwx-1-1_a.res in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.117, Rweak 0.015, Alpha 0.040, Orientation as input REM Formula found by SHELXT: C17 Cl2 Co N4 O2 P CELL 1.54184 16.5582 8.7009 16.729 90 111.858 90 ZERR 4 0.0003 0.0001 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Co N O P UNIT 68 120 8 4 12 12 4 DFIX 0.85 0.01 O1 H1 DANG 1.901768 0.02 C17 H1 DANG 2.759685 0.02 Co1 H1 L.S. 10 PLAN 20 TEMP 22.85 BOND $H list 4 MORE -1 CONF fmap 2 acta REM REM REM WGHT 0.044600 0.355900 FVAR 0.50609 CO1 4 0.307626 0.540271 0.276011 11.00000 0.03502 0.02777 = 0.03125 -0.00219 0.01128 -0.00212 CL1 3 0.365023 0.305642 0.261950 11.00000 0.05340 0.03743 = 0.03870 -0.00387 0.01350 0.00876 P1 7 0.195923 0.176996 0.445982 11.00000 0.03568 0.02775 = 0.03092 0.00078 0.01266 -0.00430 CL2 3 0.161857 0.552864 0.248325 11.00000 0.03575 0.05833 = 0.05302 0.00968 0.01095 0.00298 O1 6 0.296781 0.605809 0.150392 11.00000 0.06590 0.03493 = 0.03192 -0.00132 0.01580 0.00174 H1 2 0.288213 0.536429 0.110342 11.00000 -1.50000 O2 6 0.479229 0.841341 0.447032 11.00000 0.05226 0.03558 = 0.04968 -0.00942 0.01668 -0.01776 O3 6 0.254185 0.098648 0.524954 11.00000 0.05384 0.04239 = 0.04007 0.01076 0.01009 -0.00387 N2 5 0.341325 0.514017 0.419259 11.00000 0.03043 0.02675 = 0.02877 -0.00335 0.01301 -0.00276 N1 5 0.390846 0.720375 0.328224 11.00000 0.04144 0.02926 = 0.03662 -0.00101 0.01712 -0.00580 N3 5 0.249771 0.312697 0.414235 11.00000 0.03826 0.04051 = 0.02502 0.00043 0.00924 -0.01141 AFIX 43 H3 2 0.232507 0.325986 0.359463 11.00000 -1.20000 AFIX 0 C8 1 0.317750 0.406159 0.463184 11.00000 0.02873 0.03207 = 0.02733 -0.00197 0.01035 -0.00029 C4 1 0.403101 0.616393 0.465135 11.00000 0.03116 0.02777 = 0.03263 -0.00627 0.01267 -0.00162 C3 1 0.423527 0.728125 0.410268 11.00000 0.03225 0.02771 = 0.04176 -0.00744 0.01568 -0.00446 C5 1 0.445030 0.612374 0.553194 11.00000 0.03578 0.03607 = 0.03308 -0.00987 0.00898 -0.00386 AFIX 43 H5 2 0.486136 0.686075 0.582313 11.00000 -1.20000 AFIX 0 C6 1 0.423234 0.493444 0.596596 11.00000 0.03611 0.04658 = 0.02625 -0.00535 0.00957 0.00333 AFIX 43 H6 2 0.451932 0.484124 0.655874 11.00000 -1.20000 AFIX 0 C7 1 0.360094 0.389798 0.553295 11.00000 0.03843 0.03804 = 0.02718 0.00131 0.01360 0.00039 AFIX 43 H7 2 0.345323 0.310312 0.582453 11.00000 -1.20000 AFIX 0 C16 1 0.160290 0.046297 0.353184 11.00000 0.05025 0.03347 = 0.04672 -0.01073 0.02047 -0.01083 C11 1 0.108300 0.277415 0.467591 11.00000 0.04540 0.04540 = 0.05359 -0.00315 0.02909 -0.00367 C1 1 0.428446 0.847672 0.295576 11.00000 0.05861 0.03981 = 0.05325 0.00326 0.02827 -0.01200 AFIX 23 H1A 2 0.383181 0.915183 0.258894 11.00000 -1.20000 H1B 2 0.461991 0.809048 0.263117 11.00000 -1.20000 AFIX 0 C13 1 0.099377 -0.076751 0.365036 11.00000 0.06938 0.04879 = 0.06300 -0.01104 0.02027 -0.02383 AFIX 137 H13A 2 0.122552 -0.114085 0.423203 11.00000 -1.50000 H13B 2 0.094536 -0.160302 0.326038 11.00000 -1.50000 H13C 2 0.042910 -0.032895 0.353287 11.00000 -1.50000 AFIX 0 C17 1 0.242960 0.732186 0.107535 11.00000 0.08568 0.03819 = 0.04634 0.00743 0.01633 0.00447 AFIX 137 H17A 2 0.254548 0.758534 0.057107 11.00000 -1.50000 H17B 2 0.255287 0.818968 0.145658 11.00000 -1.50000 H17C 2 0.182884 0.703967 0.091047 11.00000 -1.50000 AFIX 0 C2 1 0.486366 0.930955 0.375784 11.00000 0.06882 0.03949 = 0.06548 0.00076 0.02477 -0.02118 AFIX 23 H2A 2 0.546058 0.933409 0.378977 11.00000 -1.20000 H2B 2 0.466435 1.035547 0.376659 11.00000 -1.20000 AFIX 0 C14 1 0.116979 0.124036 0.265563 11.00000 0.12615 0.06841 = 0.03650 -0.00846 0.01472 -0.03073 AFIX 137 H14A 2 0.063466 0.171046 0.262536 11.00000 -1.50000 H14B 2 0.105104 0.048657 0.220727 11.00000 -1.50000 H14C 2 0.155174 0.201217 0.258411 11.00000 -1.50000 AFIX 0 C15 1 0.244834 -0.032800 0.356378 11.00000 0.07094 0.06872 = 0.12286 -0.05077 0.04932 -0.00960 AFIX 137 H15A 2 0.283593 0.042708 0.348682 11.00000 -1.50000 H15B 2 0.231290 -0.108004 0.311282 11.00000 -1.50000 H15C 2 0.272224 -0.082318 0.411155 11.00000 -1.50000 AFIX 0 C9 1 0.151368 0.402372 0.533615 11.00000 0.07819 0.09368 = 0.12486 -0.06522 0.05929 -0.01692 AFIX 137 H9A 2 0.195136 0.357152 0.583260 11.00000 -1.50000 H9B 2 0.108307 0.451708 0.550456 11.00000 -1.50000 H9C 2 0.177781 0.476942 0.508706 11.00000 -1.50000 AFIX 0 C10 1 0.062728 0.166525 0.507988 11.00000 0.10093 0.08069 = 0.12402 -0.00185 0.08734 -0.01766 AFIX 137 H10A 2 0.029223 0.093683 0.465467 11.00000 -1.50000 H10B 2 0.024863 0.223218 0.528872 11.00000 -1.50000 H10C 2 0.105479 0.113032 0.554994 11.00000 -1.50000 AFIX 0 C12 1 0.040498 0.347432 0.386749 11.00000 0.06711 0.12002 = 0.09767 0.02670 0.04040 0.04445 AFIX 137 H12A 2 0.068822 0.413713 0.359401 11.00000 -1.50000 H12B 2 -0.000662 0.405778 0.402281 11.00000 -1.50000 H12C 2 0.010693 0.266842 0.347721 11.00000 -1.50000 AFIX 0 HKLF 4 REM lwx-1-1_a.res in P2(1)/c REM R1 = 0.0354 for 3744 Fo > 4sig(Fo) and 0.0438 for all 4399 data REM 254 parameters refined using 3 restraints END WGHT 0.0446 0.3559 REM Highest difference peak 0.302, deepest hole -0.328, 1-sigma level 0.053 Q1 1 0.2358 0.5482 0.2654 11.00000 0.05 0.30 Q2 1 0.1701 0.4567 0.2350 11.00000 0.05 0.27 Q3 1 0.1979 0.0212 0.3556 11.00000 0.05 0.21 Q4 1 0.3033 0.3113 0.2514 11.00000 0.05 0.20 Q5 1 0.1840 0.6842 0.0336 11.00000 0.05 0.19 Q6 1 0.0881 0.4331 0.4104 11.00000 0.05 0.19 Q7 1 0.2071 0.1392 0.2645 11.00000 0.05 0.18 Q8 1 0.3580 0.6513 0.3064 11.00000 0.05 0.18 Q9 1 0.3042 -0.0044 0.3808 11.00000 0.05 0.18 Q10 1 0.1413 0.1923 0.4513 11.00000 0.05 0.18 Q11 1 0.3414 0.4024 0.5108 11.00000 0.05 0.17 Q12 1 0.1730 0.1147 0.3878 11.00000 0.05 0.17 Q13 1 0.3360 0.4231 0.2762 11.00000 0.05 0.17 Q14 1 0.5428 0.6663 0.5945 11.00000 0.05 0.17 Q15 1 0.3333 0.9421 0.2452 11.00000 0.05 0.16 Q16 1 0.3008 0.2277 0.2773 11.00000 0.05 0.16 Q17 1 0.2068 0.3648 0.3747 11.00000 0.05 0.16 Q18 1 0.3784 0.4741 0.5811 11.00000 0.05 0.16 Q19 1 0.0383 0.4752 0.4626 11.00000 0.05 0.16 Q20 1 0.0931 0.2461 0.2577 11.00000 0.05 0.15 ; _shelx_res_checksum 99896 _shelx_shelxl_version_number 2016/6 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 5.549 _oxdiff_exptl_absorpt_empirical_full_min 0.581 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 Co1 Co 0.30763(2) 0.54027(4) 0.27601(2) 0.03165(11) Uani 1 1 d D Cl1 Cl 0.36502(4) 0.30564(7) 0.26195(4) 0.04423(15) Uani 1 1 d . P1 P 0.19592(3) 0.17700(7) 0.44598(3) 0.03137(13) Uani 1 1 d . Cl2 Cl 0.16186(4) 0.55286(8) 0.24833(4) 0.05064(17) Uani 1 1 d . O1 O 0.29678(12) 0.6058(2) 0.15039(10) 0.0449(4) Uani 1 1 d D H1 H 0.2882(18) 0.5364(18) 0.1103(9) 0.067 Uiso 1 1 d DR O2 O 0.47923(11) 0.8413(2) 0.44703(11) 0.0465(4) Uani 1 1 d . O3 O 0.25418(11) 0.0986(2) 0.52495(10) 0.0476(4) Uani 1 1 d . N2 N 0.34133(11) 0.5140(2) 0.41926(10) 0.0281(4) Uani 1 1 d . N1 N 0.39085(12) 0.7204(2) 0.32822(11) 0.0350(4) Uani 1 1 d . N3 N 0.24977(12) 0.3127(2) 0.41423(11) 0.0353(4) Uani 1 1 d . H3 H 0.232507 0.325986 0.359463 0.042 Uiso 1 1 calc R C8 C 0.31775(13) 0.4062(3) 0.46318(12) 0.0294(4) Uani 1 1 d . C4 C 0.40310(13) 0.6164(3) 0.46513(13) 0.0303(4) Uani 1 1 d . C3 C 0.42353(13) 0.7281(3) 0.41027(14) 0.0334(5) Uani 1 1 d . C5 C 0.44503(14) 0.6124(3) 0.55319(13) 0.0361(5) Uani 1 1 d . H5 H 0.486136 0.686075 0.582313 0.043 Uiso 1 1 calc R C6 C 0.42323(14) 0.4934(3) 0.59660(13) 0.0369(5) Uani 1 1 d . H6 H 0.451932 0.484124 0.655874 0.044 Uiso 1 1 calc R C7 C 0.36009(14) 0.3898(3) 0.55330(13) 0.0341(5) Uani 1 1 d . H7 H 0.345323 0.310312 0.582453 0.041 Uiso 1 1 calc R C16 C 0.16029(16) 0.0463(3) 0.35318(16) 0.0428(6) Uani 1 1 d . C11 C 0.10830(16) 0.2774(3) 0.46759(17) 0.0451(6) Uani 1 1 d . C1 C 0.42845(18) 0.8477(3) 0.29558(16) 0.0484(6) Uani 1 1 d . H1A H 0.383181 0.915183 0.258894 0.058 Uiso 1 1 calc R H1B H 0.461991 0.809048 0.263117 0.058 Uiso 1 1 calc R C13 C 0.0994(2) -0.0768(3) 0.3650(2) 0.0616(8) Uani 1 1 d . H13A H 0.122552 -0.114085 0.423203 0.092 Uiso 1 1 calc GR H13B H 0.094536 -0.160302 0.326038 0.092 Uiso 1 1 calc GR H13C H 0.042910 -0.032895 0.353287 0.092 Uiso 1 1 calc GR C17 C 0.2430(2) 0.7322(3) 0.10754(17) 0.0591(7) Uani 1 1 d D H17A H 0.254548 0.758534 0.057107 0.089 Uiso 1 1 calc GR H17B H 0.255287 0.818968 0.145658 0.089 Uiso 1 1 calc GR H17C H 0.182884 0.703967 0.091047 0.089 Uiso 1 1 calc GR C2 C 0.4864(2) 0.9310(3) 0.37578(19) 0.0580(7) Uani 1 1 d . H2A H 0.546058 0.933409 0.378977 0.070 Uiso 1 1 calc R H2B H 0.466435 1.035547 0.376659 0.070 Uiso 1 1 calc R C14 C 0.1170(3) 0.1240(4) 0.26556(17) 0.0815(11) Uani 1 1 d . H14A H 0.063466 0.171046 0.262536 0.122 Uiso 1 1 calc GR H14B H 0.105104 0.048657 0.220727 0.122 Uiso 1 1 calc GR H14C H 0.155174 0.201217 0.258411 0.122 Uiso 1 1 calc GR C15 C 0.2448(2) -0.0328(4) 0.3564(3) 0.0837(12) Uani 1 1 d . H15A H 0.283593 0.042708 0.348682 0.126 Uiso 1 1 calc GR H15B H 0.231290 -0.108004 0.311282 0.126 Uiso 1 1 calc GR H15C H 0.272224 -0.082318 0.411155 0.126 Uiso 1 1 calc GR C9 C 0.1514(2) 0.4024(5) 0.5336(3) 0.0927(13) Uani 1 1 d . H9A H 0.195136 0.357152 0.583260 0.139 Uiso 1 1 calc GR H9B H 0.108307 0.451708 0.550456 0.139 Uiso 1 1 calc GR H9C H 0.177781 0.476942 0.508706 0.139 Uiso 1 1 calc GR C10 C 0.0627(3) 0.1665(5) 0.5080(3) 0.0888(12) Uani 1 1 d . H10A H 0.029223 0.093683 0.465467 0.133 Uiso 1 1 calc GR H10B H 0.024863 0.223218 0.528872 0.133 Uiso 1 1 calc GR H10C H 0.105479 0.113032 0.554994 0.133 Uiso 1 1 calc GR C12 C 0.0405(2) 0.3474(5) 0.3867(2) 0.0921(13) Uani 1 1 d . H12A H 0.068822 0.413713 0.359401 0.138 Uiso 1 1 calc GR H12B H -0.000662 0.405778 0.402281 0.138 Uiso 1 1 calc GR H12C H 0.010693 0.266842 0.347721 0.138 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 0.03502(19) 0.0278(2) 0.03125(19) -0.00219(14) 0.01128(14) -0.00212(14) Cl1 0.0534(3) 0.0374(3) 0.0387(3) -0.0039(2) 0.0135(2) 0.0088(2) P1 0.0357(3) 0.0277(3) 0.0309(3) 0.0008(2) 0.0127(2) -0.0043(2) Cl2 0.0357(3) 0.0583(4) 0.0530(4) 0.0097(3) 0.0110(2) 0.0030(3) O1 0.0659(11) 0.0349(10) 0.0319(8) -0.0013(7) 0.0158(8) 0.0017(8) O2 0.0523(10) 0.0356(10) 0.0497(10) -0.0094(8) 0.0167(8) -0.0178(8) O3 0.0538(10) 0.0424(10) 0.0401(9) 0.0108(8) 0.0101(7) -0.0039(8) N2 0.0304(8) 0.0268(10) 0.0288(8) -0.0033(7) 0.0130(7) -0.0028(7) N1 0.0414(10) 0.0293(11) 0.0366(9) -0.0010(8) 0.0171(8) -0.0058(8) N3 0.0383(9) 0.0405(12) 0.0250(8) 0.0004(8) 0.0092(7) -0.0114(8) C8 0.0287(10) 0.0321(12) 0.0273(10) -0.0020(8) 0.0103(8) -0.0003(8) C4 0.0312(10) 0.0278(12) 0.0326(10) -0.0063(9) 0.0127(8) -0.0016(8) C3 0.0323(10) 0.0277(12) 0.0418(12) -0.0074(9) 0.0157(9) -0.0045(8) C5 0.0358(11) 0.0361(13) 0.0331(11) -0.0099(9) 0.0090(9) -0.0039(9) C6 0.0361(11) 0.0466(14) 0.0263(10) -0.0054(10) 0.0096(8) 0.0033(10) C7 0.0384(11) 0.0380(13) 0.0272(10) 0.0013(9) 0.0136(8) 0.0004(10) C16 0.0503(14) 0.0335(14) 0.0467(14) -0.0107(10) 0.0205(11) -0.0108(10) C11 0.0454(13) 0.0454(16) 0.0536(14) -0.0032(12) 0.0291(11) -0.0037(11) C1 0.0586(15) 0.0398(15) 0.0532(15) 0.0033(11) 0.0283(12) -0.0120(12) C13 0.0694(19) 0.0488(18) 0.0630(18) -0.0110(14) 0.0203(14) -0.0238(15) C17 0.086(2) 0.0382(16) 0.0463(15) 0.0074(12) 0.0163(14) 0.0045(14) C2 0.0688(18) 0.0395(16) 0.0655(18) 0.0008(13) 0.0248(14) -0.0212(13) C14 0.126(3) 0.068(2) 0.0365(15) -0.0085(15) 0.0147(17) -0.031(2) C15 0.071(2) 0.069(2) 0.123(3) -0.051(2) 0.049(2) -0.0096(17) C9 0.078(2) 0.094(3) 0.125(3) -0.065(3) 0.059(2) -0.017(2) C10 0.101(3) 0.081(3) 0.124(3) -0.002(2) 0.087(3) -0.018(2) C12 0.067(2) 0.120(3) 0.098(3) 0.027(2) 0.040(2) 0.044(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 Cl2 Co1 Cl1 117.86(3) O1 Co1 Cl1 91.32(5) O1 Co1 Cl2 95.33(5) O1 Co1 N2 167.04(7) N2 Co1 Cl1 94.04(5) N2 Co1 Cl2 92.58(5) N1 Co1 Cl1 118.89(6) N1 Co1 Cl2 122.71(6) N1 Co1 O1 90.70(7) N1 Co1 N2 76.39(7) O3 P1 N3 111.07(10) O3 P1 C16 111.53(12) O3 P1 C11 110.04(11) N3 P1 C16 102.08(10) N3 P1 C11 106.16(11) C16 P1 C11 115.56(12) Co1 O1 H1 120.3(13) C17 O1 Co1 120.75(16) C17 O1 H1 104.7(13) C3 O2 C2 105.63(18) C8 N2 Co1 130.27(13) C8 N2 C4 117.55(17) C4 N2 Co1 111.68(13) C3 N1 Co1 116.51(15) C3 N1 C1 106.91(19) C1 N1 Co1 136.53(15) P1 N3 H3 115.2 C8 N3 P1 129.55(14) C8 N3 H3 115.2 N2 C8 N3 115.29(17) N2 C8 C7 121.78(19) N3 C8 C7 122.9(2) N2 C4 C3 112.54(17) N2 C4 C5 124.2(2) C5 C4 C3 123.19(19) O2 C3 C4 118.97(19) N1 C3 O2 118.6(2) N1 C3 C4 122.42(19) C4 C5 H5 121.5 C4 C5 C6 117.0(2) C6 C5 H5 121.5 C5 C6 H6 119.6 C7 C6 C5 120.8(2) C7 C6 H6 119.6 C8 C7 H7 120.8 C6 C7 C8 118.5(2) C6 C7 H7 120.8 C13 C16 P1 110.06(18) C13 C16 C15 108.4(2) C14 C16 P1 115.16(19) C14 C16 C13 109.7(2) C14 C16 C15 109.0(3) C15 C16 P1 104.20(19) C9 C11 P1 106.88(19) C9 C11 C10 107.7(3) C9 C11 C12 110.4(3) C10 C11 P1 110.0(2) C12 C11 P1 112.9(2) C12 C11 C10 108.8(3) N1 C1 H1A 110.9 N1 C1 H1B 110.9 N1 C1 C2 104.3(2) H1A C1 H1B 108.9 C2 C1 H1A 110.9 C2 C1 H1B 110.9 C16 C13 H13A 109.5 C16 C13 H13B 109.5 C16 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 O1 C17 H17A 109.5 O1 C17 H17B 109.5 O1 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 O2 C2 C1 104.49(19) O2 C2 H2A 110.9 O2 C2 H2B 110.9 C1 C2 H2A 110.9 C1 C2 H2B 110.9 H2A C2 H2B 108.9 C16 C14 H14A 109.5 C16 C14 H14B 109.5 C16 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C16 C15 H15A 109.5 C16 C15 H15B 109.5 C16 C15 H15C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C11 C9 H9A 109.5 C11 C9 H9B 109.5 C11 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C11 C10 H10A 109.5 C11 C10 H10B 109.5 C11 C10 H10C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C11 C12 H12A 109.5 C11 C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Co1 Cl1 2.3006(7) Co1 Cl2 2.2847(7) Co1 O1 2.1196(16) Co1 N2 2.2607(16) Co1 N1 2.0546(18) P1 O3 1.4804(16) P1 N3 1.6804(19) P1 C16 1.836(2) P1 C11 1.841(3) O1 H1 0.873(9) O1 C17 1.429(3) O2 C3 1.333(2) O2 C2 1.465(3) N2 C8 1.337(3) N2 C4 1.358(3) N1 C3 1.276(3) N1 C1 1.472(3) N3 H3 0.8600 N3 C8 1.383(3) C8 C7 1.413(3) C4 C3 1.461(3) C4 C5 1.375(3) C5 H5 0.9300 C5 C6 1.387(3) C6 H6 0.9300 C6 C7 1.366(3) C7 H7 0.9300 C16 C13 1.534(4) C16 C14 1.529(4) C16 C15 1.543(4) C11 C9 1.524(4) C11 C10 1.529(4) C11 C12 1.526(4) C1 H1A 0.9700 C1 H1B 0.9700 C1 C2 1.512(4) C13 H13A 0.9600 C13 H13B 0.9600 C13 H13C 0.9600 C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C2 H2A 0.9700 C2 H2B 0.9700 C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 C9 H9A 0.9600 C9 H9B 0.9600 C9 H9C 0.9600 C10 H10A 0.9600 C10 H10B 0.9600 C10 H10C 0.9600 C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 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 N2 C8 N3 -13.9(3) Co1 N2 C8 C7 165.91(15) Co1 N2 C4 C3 7.1(2) Co1 N2 C4 C5 -170.15(17) Co1 N1 C3 O2 178.69(15) Co1 N1 C3 C4 -0.4(3) Co1 N1 C1 C2 -178.77(19) P1 N3 C8 N2 -173.69(16) P1 N3 C8 C7 6.5(3) O3 P1 N3 C8 -33.1(2) O3 P1 C16 C13 68.4(2) O3 P1 C16 C14 -167.0(2) O3 P1 C16 C15 -47.6(2) O3 P1 C11 C9 64.2(3) O3 P1 C11 C10 -52.5(2) O3 P1 C11 C12 -174.2(2) N2 C8 C7 C6 3.9(3) N2 C4 C3 O2 175.90(18) N2 C4 C3 N1 -5.0(3) N2 C4 C5 C6 1.4(3) N1 C1 C2 O2 1.9(3) N3 P1 C16 C13 -172.91(19) N3 P1 C16 C14 -48.4(2) N3 P1 C16 C15 71.0(2) N3 P1 C11 C9 -56.1(3) N3 P1 C11 C10 -172.8(2) N3 P1 C11 C12 65.5(3) N3 C8 C7 C6 -176.3(2) C8 N2 C4 C3 179.88(18) C8 N2 C4 C5 2.6(3) C4 N2 C8 N3 174.94(18) C4 N2 C8 C7 -5.3(3) C4 C5 C6 C7 -2.8(3) C3 O2 C2 C1 -1.4(3) C3 N1 C1 C2 -1.8(3) C3 C4 C5 C6 -175.6(2) C5 C4 C3 O2 -6.8(3) C5 C4 C3 N1 172.3(2) C5 C6 C7 C8 0.3(3) C16 P1 N3 C8 -152.1(2) C16 P1 C11 C9 -168.4(2) C16 P1 C11 C10 74.9(2) C16 P1 C11 C12 -46.8(3) C11 P1 N3 C8 86.5(2) C11 P1 C16 C13 -58.2(2) C11 P1 C16 C14 66.3(3) C11 P1 C16 C15 -174.3(2) C1 N1 C3 O2 1.0(3) C1 N1 C3 C4 -178.1(2) C2 O2 C3 N1 0.3(3) C2 O2 C3 C4 179.4(2)