#------------------------------------------------------------------------------ #$Date: 2021-09-30 03:46:04 +0300 (Thu, 30 Sep 2021) $ #$Revision: 269389 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/09/7060979.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_7060979 loop_ _publ_author_name 'Li, Yonghui' 'Fan, Qingqing' 'Yang, Haiquan' 'Xie, Shangqing' 'Huang, Wei' 'Li, Xiaoyan' 'Sun, Hongjian' 'Fuhr, Olaf' 'Fenske, Dieter' _publ_section_title ; Synthesis and property of [PCP] pincer silylene cobalt(I) complexes ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ02982G _journal_year 2021 _chemical_formula_moiety 'C30 H34 Co I O2 P3' _chemical_formula_sum 'C30 H34 Co I O2 P3' _chemical_formula_weight 705.31 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-08-02 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-09-14 deposited with the CCDC. 2021-09-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 21.4260(11) _cell_length_b 15.1726(7) _cell_length_c 18.2179(8) _cell_measurement_reflns_used 19802 _cell_measurement_temperature 180 _cell_measurement_theta_max 64.11 _cell_measurement_theta_min 3.75 _cell_volume 5922.4(5) _computing_cell_refinement 'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)' _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 180 _diffrn_detector 'Eiger R 4M' _diffrn_detector_area_resol_mean 13.33 _diffrn_detector_type DECTRIS _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'Eulerian 4-circle diffractometer' _diffrn_measurement_device_type 'Stoe StadiVari' _diffrn_measurement_method 'rotation method, \w scans' _diffrn_radiation_collimation '1.2 0.6 mm diameter' _diffrn_radiation_monochromator 'Graded multilayer mirror' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34143 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_unetI/netI 0.0502 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 30142 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 53.597 _diffrn_reflns_theta_max 57.586 _diffrn_reflns_theta_min 3.755 _diffrn_source 'Metaljet D2' _diffrn_source_current 2.860 _diffrn_source_power 0.200 _diffrn_source_target Ga _diffrn_source_type 'Metaljet D2' _diffrn_source_voltage 70 _exptl_absorpt_coefficient_mu 9.750 _exptl_absorpt_correction_T_max 0.0434 _exptl_absorpt_correction_T_min 0.0008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; STOE LANA, absorption correction by scaling of reflection intensities. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different absorption corrections on the model structure of tetrakis(\m~2~-acetato)- diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Afterwards a spherical absorption correction was performed within STOE LANA. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.582 _exptl_crystal_description plate _exptl_crystal_F_000 2840 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.760 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 6138 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.916 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0344 _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^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.0793 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4154 _reflns_number_total 6138 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj02982g2.cif _cod_data_source_block sun55 _cod_database_code 7060979 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.759 _shelx_estimated_absorpt_t_min 0.223 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C14(H14) 2.b Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C15(H15A,H15B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27) 2.d Idealised Me refined as rotating group: C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C) ; _shelx_res_file ; TITL sun55_a.res in Pbca sun55.res created by SHELXL-2018/3 at 12:55:01 on 02-Aug-2019 REM Old TITL SUN55, 180K, GA-JET REM SHELXT solution in Pbca: R1 0.177, Rweak 0.008, Alpha 0.055 REM 0.232 for 456 systematic absences, Orientation as input REM Formula found by SHELXT: C28 N2 O2 P Cl2 Co I CELL 1.34143 21.426 15.1726 18.2179 90 90 90 ZERR 8 0.0011 0.0007 0.0008 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Co I O P DISP C 0.0148 0.007 57.7477 DISP Co -0.6673 2.8829 21740.9299 DISP H -0 0 0.6481 DISP I 0.0968 5.4979 40725.1667 DISP O 0.0412 0.025 193.9543 DISP P 0.2596 0.3354 2524.1876 UNIT 240 272 8 8 16 24 L.S. 4 0 0 PLAN 20 SIZE 0.03 0.18 0.22 TEMP -93.15 BOND list 4 fmap 2 53 ACTA REM REM REM WGHT 0.045500 FVAR 0.16591 I1 4 0.493070 0.342799 0.586213 11.00000 0.03424 0.05302 = 0.05806 0.01192 0.00179 0.00231 CO1 3 0.612163 0.355225 0.562993 11.00000 0.03298 0.03540 = 0.02425 0.00079 -0.00012 0.00170 P1 6 0.645744 0.295562 0.461892 11.00000 0.03689 0.03824 = 0.02624 -0.00060 -0.00022 0.00395 P2 6 0.671431 0.458468 0.604973 11.00000 0.03642 0.03846 = 0.02871 -0.00024 0.00106 -0.00023 P3 6 0.629205 0.246323 0.642268 11.00000 0.03871 0.04243 = 0.02930 0.00638 0.00209 0.00257 O1 5 0.608416 0.344361 0.395499 11.00000 0.05025 0.04363 = 0.02684 -0.00097 -0.00547 0.01092 O2 5 0.699193 0.513931 0.536464 11.00000 0.04186 0.04330 = 0.03634 0.00721 0.00204 -0.00483 C1 1 0.625268 0.181644 0.442800 11.00000 0.04184 0.04194 = 0.02964 -0.00249 -0.00133 0.00349 C2 1 0.562625 0.161504 0.432685 11.00000 0.04295 0.04589 = 0.05880 -0.00724 -0.01036 0.00490 AFIX 43 H2 2 0.532685 0.207675 0.431808 11.00000 -1.20000 AFIX 0 C3 1 0.543180 0.075220 0.423870 11.00000 0.04995 0.05650 = 0.07984 -0.00501 -0.01709 -0.00692 AFIX 43 H3 2 0.500221 0.062039 0.417084 11.00000 -1.20000 AFIX 0 C4 1 0.587227 0.008109 0.425063 11.00000 0.07145 0.04045 = 0.06074 -0.00704 -0.01185 -0.00378 AFIX 43 H4 2 0.574269 -0.051318 0.418940 11.00000 -1.20000 AFIX 0 C5 1 0.649317 0.026860 0.435007 11.00000 0.05849 0.04291 = 0.04948 -0.00592 -0.00231 0.00706 AFIX 43 H5 2 0.679115 -0.019497 0.435774 11.00000 -1.20000 AFIX 0 C6 1 0.668489 0.113108 0.443900 11.00000 0.04610 0.04266 = 0.03848 -0.00287 0.00040 0.00246 AFIX 43 H6 2 0.711509 0.125783 0.450823 11.00000 -1.20000 AFIX 0 C7 1 0.725819 0.300842 0.430767 11.00000 0.04248 0.03304 = 0.03147 -0.00234 0.00269 0.00308 C8 1 0.740103 0.319661 0.357771 11.00000 0.04249 0.06916 = 0.03255 -0.00373 0.00114 0.00119 AFIX 43 H8 2 0.707489 0.333944 0.324507 11.00000 -1.20000 AFIX 0 C9 1 0.801111 0.317799 0.333192 11.00000 0.05262 0.06822 = 0.03541 -0.00310 0.00752 -0.00515 AFIX 43 H9 2 0.810082 0.331429 0.283402 11.00000 -1.20000 AFIX 0 C10 1 0.848895 0.296376 0.380246 11.00000 0.04315 0.04701 = 0.04955 -0.00032 0.01200 -0.00021 AFIX 43 H10 2 0.890613 0.292993 0.362809 11.00000 -1.20000 AFIX 0 C11 1 0.835718 0.279910 0.452723 11.00000 0.04045 0.04837 = 0.05399 0.01146 0.00251 0.00416 AFIX 43 H11 2 0.868615 0.265870 0.485672 11.00000 -1.20000 AFIX 0 C12 1 0.774946 0.283594 0.478157 11.00000 0.04498 0.04826 = 0.03707 0.00628 0.00401 0.00470 AFIX 43 H12 2 0.766760 0.274175 0.528803 11.00000 -1.20000 AFIX 0 C13 1 0.572403 0.420060 0.418927 11.00000 0.05084 0.04002 = 0.03178 0.00458 -0.00505 0.00794 AFIX 23 H13A 2 0.528381 0.402488 0.426568 11.00000 -1.20000 H13B 2 0.573469 0.465914 0.380286 11.00000 -1.20000 AFIX 0 C14 1 0.598737 0.457051 0.489576 11.00000 0.04185 0.03368 = 0.02770 0.00231 -0.00111 0.00453 AFIX 13 H14 2 0.567377 0.498605 0.510906 11.00000 -1.20000 AFIX 0 C15 1 0.658041 0.508635 0.472975 11.00000 0.05011 0.04050 = 0.02990 0.00575 -0.00037 0.00042 AFIX 23 H15A 2 0.680512 0.479840 0.431994 11.00000 -1.20000 H15B 2 0.646723 0.568968 0.457130 11.00000 -1.20000 AFIX 0 C16 1 0.625448 0.540995 0.653325 11.00000 0.03792 0.03742 = 0.03327 -0.00493 -0.00413 0.00018 C17 1 0.628370 0.627819 0.632366 11.00000 0.05191 0.04458 = 0.05280 -0.00516 -0.00810 0.00219 AFIX 43 H17 2 0.656445 0.644844 0.594577 11.00000 -1.20000 AFIX 0 C18 1 0.590981 0.691216 0.665459 11.00000 0.07236 0.04375 = 0.07760 -0.01086 -0.02007 0.01142 AFIX 43 H18 2 0.593898 0.751194 0.650888 11.00000 -1.20000 AFIX 0 C19 1 0.549696 0.666436 0.719506 11.00000 0.05979 0.07263 = 0.06134 -0.02800 -0.01311 0.02714 AFIX 43 H19 2 0.523738 0.709292 0.742162 11.00000 -1.20000 AFIX 0 C20 1 0.546074 0.580713 0.740439 11.00000 0.05840 0.07474 = 0.04864 -0.01199 0.00453 0.01321 AFIX 43 H20 2 0.517823 0.563954 0.778128 11.00000 -1.20000 AFIX 0 C21 1 0.582867 0.518100 0.707619 11.00000 0.04962 0.04985 = 0.04505 -0.00523 0.00351 0.00776 AFIX 43 H21 2 0.579188 0.458215 0.722215 11.00000 -1.20000 AFIX 0 C22 1 0.741437 0.448899 0.660682 11.00000 0.04017 0.03363 = 0.03607 -0.00200 -0.00322 -0.00408 C23 1 0.737961 0.444359 0.737041 11.00000 0.04957 0.05592 = 0.04137 -0.00735 -0.00332 -0.00258 AFIX 43 H23 2 0.699035 0.452862 0.760983 11.00000 -1.20000 AFIX 0 C24 1 0.790867 0.427557 0.777957 11.00000 0.06563 0.07366 = 0.04609 -0.00494 -0.02028 -0.00205 AFIX 43 H24 2 0.787725 0.422284 0.829787 11.00000 -1.20000 AFIX 0 C25 1 0.847641 0.418429 0.744828 11.00000 0.05507 0.05427 = 0.07302 -0.00356 -0.02970 -0.00166 AFIX 43 H25 2 0.883907 0.408064 0.773560 11.00000 -1.20000 AFIX 0 C26 1 0.852115 0.424288 0.669832 11.00000 0.04105 0.04887 = 0.07690 0.00533 -0.00277 -0.00091 AFIX 43 H26 2 0.891645 0.418417 0.646725 11.00000 -1.20000 AFIX 0 C27 1 0.799240 0.438735 0.627600 11.00000 0.04283 0.04324 = 0.04909 0.00209 0.00093 -0.00271 AFIX 43 H27 2 0.802664 0.441682 0.575667 11.00000 -1.20000 AFIX 0 C28 1 0.609326 0.272699 0.736962 11.00000 0.05083 0.05481 = 0.03252 0.00718 0.00049 0.00169 AFIX 137 H28A 2 0.640173 0.313959 0.756880 11.00000 -1.50000 H28B 2 0.609298 0.218591 0.766340 11.00000 -1.50000 H28C 2 0.567812 0.299738 0.738616 11.00000 -1.50000 AFIX 0 C29 1 0.707500 0.201680 0.652645 11.00000 0.04916 0.05350 = 0.04176 0.00958 -0.00015 0.00829 AFIX 137 H29A 2 0.721190 0.176095 0.605950 11.00000 -1.50000 H29B 2 0.707311 0.155925 0.690614 11.00000 -1.50000 H29C 2 0.736180 0.248966 0.666962 11.00000 -1.50000 AFIX 0 C30 1 0.586127 0.145113 0.627904 11.00000 0.05733 0.04451 = 0.04692 0.00660 0.00518 -0.00093 AFIX 137 H30A 2 0.541307 0.157952 0.627009 11.00000 -1.50000 H30B 2 0.595181 0.103857 0.667901 11.00000 -1.50000 H30C 2 0.598576 0.118751 0.581029 11.00000 -1.50000 AFIX 0 HKLF 4 REM sun55_a.res in Pbca REM wR2 = 0.0793, GooF = S = 0.916, Restrained GooF = 0.916 for all data REM R1 = 0.0344 for 4154 Fo > 4sig(Fo) and 0.0618 for all 6138 data REM 337 parameters refined using 0 restraints END WGHT 0.0455 0.0000 REM Highest difference peak 0.760, deepest hole -0.353, 1-sigma level 0.090 Q1 1 0.5536 0.3349 0.5780 11.00000 0.05 0.76 Q2 1 0.4365 0.3048 0.5851 11.00000 0.05 0.45 Q3 1 0.4327 0.3636 0.5801 11.00000 0.05 0.44 Q4 1 0.5969 0.3057 0.5953 11.00000 0.05 0.40 Q5 1 0.5362 0.2830 0.6159 11.00000 0.05 0.39 Q6 1 0.6862 0.3023 0.4449 11.00000 0.05 0.38 Q7 1 0.6401 0.4130 0.5852 11.00000 0.05 0.36 Q8 1 0.4921 0.3254 0.6613 11.00000 0.05 0.36 Q9 1 0.6790 0.3610 0.5959 11.00000 0.05 0.35 Q10 1 0.4954 0.3389 0.5047 11.00000 0.05 0.35 Q11 1 0.6510 0.2991 0.5960 11.00000 0.05 0.35 Q12 1 0.4949 0.3549 0.6643 11.00000 0.05 0.34 Q13 1 0.6576 0.4107 0.5451 11.00000 0.05 0.32 Q14 1 0.7165 0.3269 0.4137 11.00000 0.05 0.32 Q15 1 0.7200 0.3361 0.5734 11.00000 0.05 0.31 Q16 1 0.6764 0.3336 0.5678 11.00000 0.05 0.30 Q17 1 0.6447 0.3000 0.5296 11.00000 0.05 0.30 Q18 1 0.7196 0.3963 0.5806 11.00000 0.05 0.29 Q19 1 0.8164 0.2796 0.3659 11.00000 0.05 0.28 Q20 1 0.7178 0.2628 0.4236 11.00000 0.05 0.28 ; _shelx_res_checksum 35304 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 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 I1 I 0.49307(2) 0.34280(2) 0.58621(2) 0.04844(9) Uani 1 1 d . . . . . Co1 Co 0.61216(2) 0.35522(3) 0.56299(2) 0.03088(12) Uani 1 1 d . . . . . P1 P 0.64574(4) 0.29556(6) 0.46189(4) 0.0338(2) Uani 1 1 d . . . . . P2 P 0.67143(4) 0.45847(6) 0.60497(4) 0.0345(2) Uani 1 1 d . . . . . P3 P 0.62920(4) 0.24632(6) 0.64227(4) 0.0368(2) Uani 1 1 d . . . . . O1 O 0.60842(10) 0.34436(15) 0.39550(11) 0.0402(5) Uani 1 1 d . . . . . O2 O 0.69919(10) 0.51393(15) 0.53646(11) 0.0405(5) Uani 1 1 d . . . . . C1 C 0.62527(15) 0.1816(2) 0.44280(16) 0.0378(8) Uani 1 1 d . . . . . C2 C 0.56262(16) 0.1615(3) 0.43269(19) 0.0492(10) Uani 1 1 d . . . . . H2 H 0.532685 0.207675 0.431808 0.059 Uiso 1 1 calc R . . . . C3 C 0.54318(19) 0.0752(3) 0.4239(2) 0.0621(11) Uani 1 1 d . . . . . H3 H 0.500221 0.062039 0.417084 0.075 Uiso 1 1 calc R . . . . C4 C 0.58723(19) 0.0081(3) 0.4251(2) 0.0575(10) Uani 1 1 d . . . . . H4 H 0.574269 -0.051318 0.418940 0.069 Uiso 1 1 calc R . . . . C5 C 0.64932(18) 0.0269(3) 0.43501(19) 0.0503(9) Uani 1 1 d . . . . . H5 H 0.679115 -0.019497 0.435774 0.060 Uiso 1 1 calc R . . . . C6 C 0.66849(16) 0.1131(3) 0.44390(17) 0.0424(8) Uani 1 1 d . . . . . H6 H 0.711509 0.125783 0.450823 0.051 Uiso 1 1 calc R . . . . C7 C 0.72582(14) 0.3008(2) 0.43077(16) 0.0357(7) Uani 1 1 d . . . . . C8 C 0.74010(16) 0.3197(3) 0.35777(17) 0.0481(9) Uani 1 1 d . . . . . H8 H 0.707489 0.333944 0.324507 0.058 Uiso 1 1 calc R . . . . C9 C 0.80111(17) 0.3178(3) 0.33319(19) 0.0521(10) Uani 1 1 d . . . . . H9 H 0.810082 0.331429 0.283402 0.062 Uiso 1 1 calc R . . . . C10 C 0.84890(16) 0.2964(2) 0.38025(19) 0.0466(9) Uani 1 1 d . . . . . H10 H 0.890613 0.292993 0.362809 0.056 Uiso 1 1 calc R . . . . C11 C 0.83572(16) 0.2799(2) 0.45272(19) 0.0476(9) Uani 1 1 d . . . . . H11 H 0.868615 0.265870 0.485672 0.057 Uiso 1 1 calc R . . . . C12 C 0.77495(15) 0.2836(2) 0.47816(17) 0.0434(9) Uani 1 1 d . . . . . H12 H 0.766760 0.274175 0.528803 0.052 Uiso 1 1 calc R . . . . C13 C 0.57240(16) 0.4201(2) 0.41893(16) 0.0409(8) Uani 1 1 d . . . . . H13A H 0.528381 0.402488 0.426568 0.049 Uiso 1 1 calc R . . . . H13B H 0.573469 0.465914 0.380286 0.049 Uiso 1 1 calc R . . . . C14 C 0.59874(14) 0.4571(2) 0.48958(15) 0.0344(7) Uani 1 1 d . . . . . H14 H 0.567377 0.498605 0.510906 0.041 Uiso 1 1 calc R . . . . C15 C 0.65804(15) 0.5086(2) 0.47298(16) 0.0402(8) Uani 1 1 d . . . . . H15A H 0.680512 0.479840 0.431994 0.048 Uiso 1 1 calc R . . . . H15B H 0.646723 0.568968 0.457130 0.048 Uiso 1 1 calc R . . . . C16 C 0.62545(14) 0.5410(2) 0.65333(16) 0.0362(8) Uani 1 1 d . . . . . C17 C 0.62837(17) 0.6278(3) 0.6324(2) 0.0498(9) Uani 1 1 d . . . . . H17 H 0.656445 0.644844 0.594577 0.060 Uiso 1 1 calc R . . . . C18 C 0.5910(2) 0.6912(3) 0.6655(2) 0.0646(12) Uani 1 1 d . . . . . H18 H 0.593898 0.751194 0.650888 0.077 Uiso 1 1 calc R . . . . C19 C 0.54970(19) 0.6664(3) 0.7195(2) 0.0646(13) Uani 1 1 d . . . . . H19 H 0.523738 0.709292 0.742162 0.078 Uiso 1 1 calc R . . . . C20 C 0.54607(18) 0.5807(3) 0.7404(2) 0.0606(11) Uani 1 1 d . . . . . H20 H 0.517823 0.563954 0.778128 0.073 Uiso 1 1 calc R . . . . C21 C 0.58287(16) 0.5181(3) 0.70762(18) 0.0482(9) Uani 1 1 d . . . . . H21 H 0.579188 0.458215 0.722215 0.058 Uiso 1 1 calc R . . . . C22 C 0.74144(14) 0.4489(2) 0.66068(16) 0.0366(7) Uani 1 1 d . . . . . C23 C 0.73796(16) 0.4444(3) 0.73704(18) 0.0490(9) Uani 1 1 d . . . . . H23 H 0.699035 0.452862 0.760983 0.059 Uiso 1 1 calc R . . . . C24 C 0.79087(19) 0.4276(3) 0.7780(2) 0.0618(11) Uani 1 1 d . . . . . H24 H 0.787725 0.422284 0.829787 0.074 Uiso 1 1 calc R . . . . C25 C 0.84764(19) 0.4184(3) 0.7448(2) 0.0608(11) Uani 1 1 d . . . . . H25 H 0.883907 0.408064 0.773560 0.073 Uiso 1 1 calc R . . . . C26 C 0.85211(17) 0.4243(3) 0.6698(2) 0.0556(10) Uani 1 1 d . . . . . H26 H 0.891645 0.418417 0.646725 0.067 Uiso 1 1 calc R . . . . C27 C 0.79924(15) 0.4387(2) 0.62760(19) 0.0451(9) Uani 1 1 d . . . . . H27 H 0.802664 0.441682 0.575667 0.054 Uiso 1 1 calc R . . . . C28 C 0.60933(16) 0.2727(2) 0.73696(16) 0.0461(9) Uani 1 1 d . . . . . H28A H 0.640173 0.313959 0.756880 0.069 Uiso 1 1 calc GR . . . . H28B H 0.609298 0.218591 0.766340 0.069 Uiso 1 1 calc GR . . . . H28C H 0.567812 0.299738 0.738616 0.069 Uiso 1 1 calc GR . . . . C29 C 0.70750(16) 0.2017(3) 0.65265(18) 0.0481(9) Uani 1 1 d . . . . . H29A H 0.721190 0.176095 0.605950 0.072 Uiso 1 1 calc GR . . . . H29B H 0.707311 0.155925 0.690614 0.072 Uiso 1 1 calc GR . . . . H29C H 0.736180 0.248966 0.666962 0.072 Uiso 1 1 calc GR . . . . C30 C 0.58613(17) 0.1451(2) 0.62790(19) 0.0496(9) Uani 1 1 d . . . . . H30A H 0.541307 0.157952 0.627009 0.074 Uiso 1 1 calc GR . . . . H30B H 0.595181 0.103857 0.667901 0.074 Uiso 1 1 calc GR . . . . H30C H 0.598576 0.118751 0.581029 0.074 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 I1 0.03424(12) 0.05302(18) 0.05806(14) 0.01192(11) 0.00179(9) 0.00231(10) Co1 0.0330(2) 0.0354(3) 0.02425(19) 0.00079(18) -0.00012(16) 0.00170(19) P1 0.0369(4) 0.0382(6) 0.0262(4) -0.0006(3) -0.0002(3) 0.0040(4) P2 0.0364(4) 0.0385(6) 0.0287(4) -0.0002(3) 0.0011(3) -0.0002(4) P3 0.0387(4) 0.0424(6) 0.0293(4) 0.0064(4) 0.0021(3) 0.0026(4) O1 0.0502(13) 0.0436(16) 0.0268(10) -0.0010(10) -0.0055(9) 0.0109(11) O2 0.0419(12) 0.0433(15) 0.0363(11) 0.0072(10) 0.0020(9) -0.0048(11) C1 0.0418(19) 0.042(2) 0.0296(15) -0.0025(14) -0.0013(13) 0.0035(15) C2 0.043(2) 0.046(3) 0.059(2) -0.0072(18) -0.0104(16) 0.0049(17) C3 0.050(2) 0.057(3) 0.080(3) -0.005(2) -0.017(2) -0.007(2) C4 0.071(3) 0.040(3) 0.061(2) -0.0070(19) -0.0119(19) -0.004(2) C5 0.058(2) 0.043(3) 0.049(2) -0.0059(18) -0.0023(16) 0.0071(19) C6 0.046(2) 0.043(3) 0.0385(17) -0.0029(16) 0.0004(14) 0.0025(17) C7 0.0425(18) 0.033(2) 0.0315(16) -0.0023(14) 0.0027(13) 0.0031(15) C8 0.042(2) 0.069(3) 0.0326(17) -0.0037(16) 0.0011(14) 0.0012(18) C9 0.053(2) 0.068(3) 0.0354(18) -0.0031(17) 0.0075(15) -0.0051(19) C10 0.043(2) 0.047(3) 0.050(2) -0.0003(18) 0.0120(16) -0.0002(17) C11 0.0404(19) 0.048(3) 0.054(2) 0.0115(17) 0.0025(16) 0.0042(16) C12 0.045(2) 0.048(3) 0.0371(17) 0.0063(15) 0.0040(14) 0.0047(16) C13 0.0508(19) 0.040(2) 0.0318(16) 0.0046(14) -0.0050(14) 0.0079(16) C14 0.0419(18) 0.034(2) 0.0277(14) 0.0023(13) -0.0011(12) 0.0045(15) C15 0.050(2) 0.040(2) 0.0299(15) 0.0057(14) -0.0004(14) 0.0004(16) C16 0.0379(17) 0.037(2) 0.0333(16) -0.0049(14) -0.0041(13) 0.0002(15) C17 0.052(2) 0.045(3) 0.053(2) -0.0052(18) -0.0081(17) 0.0022(18) C18 0.072(3) 0.044(3) 0.078(3) -0.011(2) -0.020(2) 0.011(2) C19 0.060(3) 0.073(4) 0.061(3) -0.028(2) -0.013(2) 0.027(2) C20 0.058(2) 0.075(4) 0.049(2) -0.012(2) 0.0045(17) 0.013(2) C21 0.050(2) 0.050(3) 0.0450(18) -0.0052(17) 0.0035(15) 0.0078(18) C22 0.0402(18) 0.034(2) 0.0361(16) -0.0020(14) -0.0032(13) -0.0041(15) C23 0.050(2) 0.056(3) 0.0414(19) -0.0074(17) -0.0033(15) -0.0026(18) C24 0.066(3) 0.074(3) 0.046(2) -0.005(2) -0.0203(19) -0.002(2) C25 0.055(2) 0.054(3) 0.073(3) -0.004(2) -0.030(2) -0.0017(19) C26 0.041(2) 0.049(3) 0.077(3) 0.005(2) -0.0028(18) -0.0009(18) C27 0.0428(19) 0.043(2) 0.049(2) 0.0021(17) 0.0009(15) -0.0027(16) C28 0.051(2) 0.055(3) 0.0325(16) 0.0072(16) 0.0005(14) 0.0017(17) C29 0.049(2) 0.054(3) 0.0418(18) 0.0096(17) -0.0001(15) 0.0083(18) C30 0.057(2) 0.045(3) 0.0469(19) 0.0066(17) 0.0052(16) -0.0009(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0148 0.0070 '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' Co Co -0.6673 2.8829 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I 0.0968 5.4979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2596 0.3354 '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 P1 Co1 I1 115.68(3) . . ? P1 Co1 P3 100.74(4) . . ? P2 Co1 I1 125.05(3) . . ? P2 Co1 P1 114.07(4) . . ? P2 Co1 P3 102.28(3) . . ? P3 Co1 I1 90.09(3) . . ? C14 Co1 I1 91.32(9) . . ? C14 Co1 P1 78.98(9) . . ? C14 Co1 P2 76.59(9) . . ? C14 Co1 P3 178.54(9) . . ? O1 P1 Co1 106.10(9) . . ? O1 P1 C1 99.89(13) . . ? O1 P1 C7 102.29(13) . . ? C1 P1 Co1 118.57(10) . . ? C7 P1 Co1 124.12(11) . . ? C7 P1 C1 102.19(15) . . ? O2 P2 Co1 108.70(9) . . ? O2 P2 C16 102.38(14) . . ? O2 P2 C22 99.72(13) . . ? C16 P2 Co1 110.64(11) . . ? C22 P2 Co1 128.77(12) . . ? C22 P2 C16 103.38(14) . . ? C28 P3 Co1 114.41(12) . . ? C29 P3 Co1 119.70(12) . . ? C29 P3 C28 101.48(15) . . ? C30 P3 Co1 116.90(12) . . ? C30 P3 C28 101.77(17) . . ? C30 P3 C29 99.75(18) . . ? C13 O1 P1 113.80(17) . . ? C15 O2 P2 111.17(18) . . ? C2 C1 P1 117.9(3) . . ? C2 C1 C6 118.7(3) . . ? C6 C1 P1 123.2(3) . . ? C3 C2 C1 121.0(3) . . ? C2 C3 C4 119.2(4) . . ? C5 C4 C3 120.6(4) . . ? C4 C5 C6 120.0(4) . . ? C5 C6 C1 120.5(3) . . ? C8 C7 P1 121.1(2) . . ? C12 C7 P1 121.1(2) . . ? C12 C7 C8 117.8(3) . . ? C9 C8 C7 120.8(3) . . ? C10 C9 C8 120.5(3) . . ? C11 C10 C9 119.3(3) . . ? C10 C11 C12 120.6(3) . . ? C11 C12 C7 120.9(3) . . ? O1 C13 C14 110.3(2) . . ? C13 C14 Co1 109.0(2) . . ? C13 C14 C15 109.4(2) . . ? C15 C14 Co1 113.4(2) . . ? O2 C15 C14 112.1(2) . . ? C17 C16 P2 120.0(3) . . ? C17 C16 C21 117.9(3) . . ? C21 C16 P2 121.9(3) . . ? C16 C17 C18 121.2(4) . . ? C19 C18 C17 119.5(4) . . ? C20 C19 C18 120.0(4) . . ? C19 C20 C21 120.5(4) . . ? C20 C21 C16 121.0(4) . . ? C23 C22 P2 121.1(2) . . ? C27 C22 P2 120.2(2) . . ? C27 C22 C23 118.4(3) . . ? C24 C23 C22 120.3(3) . . ? C25 C24 C23 120.8(4) . . ? C24 C25 C26 119.7(4) . . ? C25 C26 C27 120.4(4) . . ? C22 C27 C26 120.4(3) . . ? 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 I1 Co1 2.5934(5) . ? Co1 P1 2.1748(9) . ? Co1 P2 2.1567(9) . ? Co1 P3 2.2247(9) . ? Co1 C14 2.064(3) . ? P1 O1 1.628(2) . ? P1 C1 1.817(4) . ? P1 C7 1.809(3) . ? P2 O2 1.619(2) . ? P2 C16 1.821(3) . ? P2 C22 1.817(3) . ? P3 C28 1.821(3) . ? P3 C29 1.819(3) . ? P3 C30 1.811(4) . ? O1 C13 1.448(4) . ? O2 C15 1.457(4) . ? C1 C2 1.389(5) . ? C1 C6 1.393(5) . ? C2 C3 1.383(5) . ? C3 C4 1.389(5) . ? C4 C5 1.372(5) . ? C5 C6 1.381(5) . ? C7 C8 1.394(4) . ? C7 C12 1.386(4) . ? C8 C9 1.382(5) . ? C9 C10 1.374(5) . ? C10 C11 1.373(5) . ? C11 C12 1.383(4) . ? C13 C14 1.513(4) . ? C14 C15 1.523(4) . ? C16 C17 1.373(5) . ? C16 C21 1.390(5) . ? C17 C18 1.389(5) . ? C18 C19 1.376(6) . ? C19 C20 1.358(6) . ? C20 C21 1.372(5) . ? C22 C23 1.395(4) . ? C22 C27 1.386(4) . ? C23 C24 1.380(5) . ? C24 C25 1.365(6) . ? C25 C26 1.373(5) . ? C26 C27 1.387(5) . ?