#------------------------------------------------------------------------------ #$Date: 2021-01-07 08:32:53 +0200 (Thu, 07 Jan 2021) $ #$Revision: 260793 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705267.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_7705267 loop_ _publ_author_name 'Kephart, Jonathan A.' 'Boggiano, Andrew C.' 'Kaminsky, Werner' 'Velian, Alexandra' _publ_section_title ; Inorganic clusters as metalloligands: ligand effects on the synthesis and properties of ternary nanopropeller clusters. ; _journal_issue 45 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 16464 _journal_page_last 16473 _journal_paper_doi 10.1039/d0dt02416c _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C12 H22 Co N O3 P' _chemical_formula_sum 'C12 H22 Co N O3 P' _chemical_formula_weight 318.2 _chemical_name_systematic '[Co(CO)3(iPr2PNHiPr)]2' _space_group_IT_number 205 _space_group_name_Hall '-P 2ac 2ab 3' _space_group_name_H-M_alt 'P a -3' _symmetry_cell_setting cubic _symmetry_Int_Tables_number 205 _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2017-08-24T13:49:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2020-07-06 deposited with the CCDC. 2020-08-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.6369(9) _cell_length_b 14.6369(9) _cell_length_c 14.6369(9) _cell_measurement_reflns_used 103929 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.33 _cell_measurement_theta_min 1.39 _cell_measurement_wavelength 0.71073 _cell_volume 3135.8(3) _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker APEXII CCD area-detector' _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device 'Bruker Apex II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_unetI/netI 0.0618 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 2470 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 28.328 _diffrn_reflns_theta_min 2.41 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_description shard _exptl_crystal_F_000 1335.9 _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max 0.946 _exptl_transmission_factor_min 0.878 _refine_diff_density_max 0.341 _refine_diff_density_min -0.26 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 139 _refine_ls_number_reflns 1306 _refine_ls_number_restraints 95 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.1349 _refine_ls_R_factor_gt 0.0414 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0983 _refine_ls_wR_factor_ref 0.1479 _reflns_Friedel_coverage 0 _reflns_number_gt 589 _reflns_number_total 1306 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02416c2.cif _cod_data_source_block shelx _cod_depositor_comments 'Adding full bibliography for 7705267--7705273.cif.' _cod_original_cell_volume 3135.8(6) _cod_database_code 7705267 _shelx_estimated_absorpt_t_min 0.921 _shelx_estimated_absorpt_t_max 0.954 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL JAK_1_0m in Pa-3 CELL 0.71073 14.6369 14.6369 14.6369 90.000 90.000 90.000 ZERR 8.00 0.0009 0.0009 0.0009 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM Z, X, Y SYMM 1/2 + Z, 1/2 - X, - Y SYMM 1/2 - Z, - X, 1/2 + Y SYMM - Z, 1/2 + X, 1/2 - Y SYMM Y, Z, X SYMM - Y, 1/2 + Z, 1/2 - X SYMM 1/2 + Y, 1/2 - Z, - X SYMM 1/2 - Y, - Z, 1/2 + X SFAC C H P O CO N UNIT 96 176 8 24 8 8 MERG 3 OMIT 2 1 8 OMIT 2 1 4 OMIT 2 5 5 OMIT 1 4 5 OMIT 1 0 6 OMIT 3 4 5 OMIT 0 0 2 OMIT 2 1 6 OMIT 5 1 11 OMIT 3 7 15 ISOR 0.015 $C SADI 0.005 C1 C2 C1 C3 EADP C1 N1 C4 EADP C2 C5 C9 DFIX -2.000 0.020 H5B H1 DFIX 1.400 0.020 C9 N1 FMAP 2 PLAN 20 SIZE 0.040 0.050 0.070 ACTA 50.00 BOND $H WPDB -2 L.S. 16 TEMP -173.00 WGHT 0.073800 FVAR 0.12043 PART -1 C1 1 0.894421 0.249230 0.169808 10.33333 0.07317 0.09408 = 0.10268 0.02393 0.02312 -0.02456 AFIX 13 H1 2 0.944586 0.258793 0.215192 10.33333 -1.20000 AFIX 0 C2 1 0.944792 0.197400 0.099329 10.33333 0.09522 0.10787 = 0.10414 0.00870 -0.00781 -0.01283 AFIX 137 H2A 2 1.000335 0.230788 0.082504 10.33333 -1.50000 H2B 2 0.906057 0.189829 0.045245 10.33333 -1.50000 H2C 2 0.961394 0.137206 0.123494 10.33333 -1.50000 AFIX 0 C3 1 0.829986 0.196520 0.226476 10.33333 0.13028 0.10851 = 0.13218 0.06662 -0.04004 -0.05514 AFIX 137 H3A 2 0.861426 0.143460 0.252532 10.33333 -1.50000 H3B 2 0.778799 0.175768 0.188633 10.33333 -1.50000 H3C 2 0.806893 0.235288 0.275939 10.33333 -1.50000 AFIX 0 PART 0 SAME 0.005 P1 C1 C2 C3 P1 3 0.859538 0.373182 0.149011 10.33333 0.06687 0.03695 = 0.03795 0.00410 0.00978 0.00089 PART -1 C4 1 0.744510 0.352451 0.090013 10.33333 0.07317 0.09408 = 0.10268 0.02393 0.02312 -0.02456 AFIX 13 H4 2 0.713739 0.309079 0.132906 10.33333 -1.20000 AFIX 0 C5 1 0.743496 0.300931 0.002762 10.33333 0.09522 0.10787 = 0.10414 0.00870 -0.00781 -0.01283 AFIX 137 H5A 2 0.680929 0.281391 -0.010893 10.33333 -1.50000 H5B 2 0.783003 0.247144 0.008143 10.33333 -1.50000 H5C 2 0.765885 0.340218 -0.046616 10.33333 -1.50000 AFIX 0 C6 1 0.683336 0.433092 0.093262 10.33333 0.11037 0.22358 = 0.11887 -0.01588 0.02549 -0.00185 AFIX 137 H6A 2 0.619618 0.412951 0.089111 10.33333 -1.50000 H6B 2 0.697275 0.473762 0.041934 10.33333 -1.50000 H6C 2 0.692670 0.465879 0.150888 10.33333 -1.50000 AFIX 0 N1 6 0.823174 0.415779 0.232694 10.33333 0.07317 0.09408 = 0.10268 0.02393 0.02312 -0.02456 AFIX 43 H1A 2 0.769745 0.395600 0.251476 10.33333 -1.20000 AFIX 0 SAME C1 C2 C3 C9 1 0.862858 0.483833 0.285534 10.33333 0.09522 0.10787 = 0.10414 0.00870 -0.00781 -0.01283 AFIX 13 H9 2 0.913052 0.511225 0.248145 10.33333 -1.20000 AFIX 0 C10 1 0.906907 0.445379 0.371715 10.33333 0.25070 0.21437 = 0.08643 -0.00705 -0.02723 -0.01553 AFIX 137 H10A 2 0.859147 0.426628 0.414729 10.33333 -1.50000 H10B 2 0.945262 0.492377 0.400051 10.33333 -1.50000 H10C 2 0.944630 0.392412 0.355769 10.33333 -1.50000 AFIX 0 C11 1 0.795159 0.554456 0.298727 10.33333 0.14984 0.14989 = 0.19428 0.01407 0.08483 0.01102 AFIX 137 H11A 2 0.754791 0.556923 0.245369 10.33333 -1.50000 H11B 2 0.825730 0.613536 0.306335 10.33333 -1.50000 H11C 2 0.759040 0.540809 0.353427 10.33333 -1.50000 AFIX 0 PART 1 C7 1 0.916905 0.390519 -0.049448 10.33333 0.04492 0.05658 = 0.05828 0.01679 -0.00637 -0.01286 O1 4 0.899464 0.353681 -0.117784 10.33333 0.05934 0.08707 = 0.07845 -0.01189 -0.01015 0.00008 SAME C7 O1 CO1 C8 1 1.041518 0.444349 0.127534 10.33333 0.06660 0.06516 = 0.06396 0.00317 0.01170 -0.00062 O2 4 1.099724 0.442174 0.180443 10.33333 0.09171 0.08594 = 0.11446 0.03564 -0.03520 -0.01225 PART 0 SAME CO1 C7 O1 CO1 5 0.947284 0.447284 0.052716 10.33333 0.05165 0.05165 = 0.05165 0.00815 0.00815 -0.00815 PART 1 C12 1 0.861507 0.529255 0.030854 10.33333 0.06404 0.04287 = 0.04903 -0.00113 0.00933 -0.01205 O3 4 0.810326 0.587503 0.015883 10.33333 0.08011 0.06969 = 0.05850 0.00722 0.01670 0.01380 HKLF 4 REM JAK_1_0m in Pa-3 REM R1 = 0.0414 for 589 Fo > 4sig(Fo) and 0.1349 for all 1306 data REM 139 parameters refined using 95 restraints END WGHT 0.0741 0.0000 REM Highest difference peak 0.341, deepest hole -0.260, 1-sigma level 0.056 Q1 1 0.7681 0.2562 -0.0145 11.00000 0.05 0.34 Q2 1 1.0000 0.5000 0.0000 10.16667 0.05 0.28 Q3 1 0.9803 0.5165 0.0027 11.00000 0.05 0.27 Q4 1 0.8343 0.5491 -0.0455 11.00000 0.05 0.24 Q5 1 0.9283 0.1894 0.0378 11.00000 0.05 0.20 Q6 1 0.6680 0.3142 0.1311 11.00000 0.05 0.19 Q7 1 0.7679 0.5985 0.2534 11.00000 0.05 0.18 Q8 1 0.9007 0.4007 0.0993 10.33333 0.05 0.18 Q9 1 0.8513 0.5616 0.3365 11.00000 0.05 0.17 Q10 1 0.8665 0.3785 -0.1223 11.00000 0.05 0.16 Q11 1 0.6368 0.3189 0.0054 11.00000 0.05 0.16 Q12 1 0.7397 0.3456 -0.0227 11.00000 0.05 0.16 Q13 1 0.7214 0.4002 0.1713 11.00000 0.05 0.16 Q14 1 0.5920 0.3712 0.1851 11.00000 0.05 0.16 Q15 1 0.7295 0.3605 -0.0395 11.00000 0.05 0.15 Q16 1 0.8554 0.5548 0.3574 11.00000 0.05 0.15 Q17 1 0.9085 0.5832 0.3584 11.00000 0.05 0.15 Q18 1 0.6347 0.4997 0.1877 11.00000 0.05 0.15 Q19 1 0.7757 0.1203 0.2110 11.00000 0.05 0.14 Q20 1 0.8595 0.5734 0.3181 11.00000 0.05 0.14 ; _shelx_res_checksum 34011 loop_ _symmetry_equiv_pos_as_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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-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 0.8944(14) 0.2492(14) 0.1698(17) 0.090(3) Uani 0.3333 1 d D U P A -1 H1 H 0.9446 0.2588 0.2152 0.108 Uiso 0.3333 1 calc DR U P A -1 C2 C 0.9448(15) 0.1974(17) 0.0993(14) 0.102(4) Uani 0.3333 1 d D U P A -1 H2A H 1.0003 0.2308 0.0825 0.154 Uiso 0.3333 1 calc R U P A -1 H2B H 0.9061 0.1898 0.0452 0.154 Uiso 0.3333 1 calc R U P A -1 H2C H 0.9614 0.1372 0.1235 0.154 Uiso 0.3333 1 calc R U P A -1 C3 C 0.8300(12) 0.1965(11) 0.2265(13) 0.124(7) Uani 0.3333 1 d D U P A -1 H3A H 0.8614 0.1435 0.2525 0.185 Uiso 0.3333 1 calc R U P A -1 H3B H 0.7788 0.1758 0.1886 0.185 Uiso 0.3333 1 calc R U P A -1 H3C H 0.8069 0.2353 0.2759 0.185 Uiso 0.3333 1 calc R U P A -1 P1 P 0.8595(10) 0.3732(7) 0.1490(10) 0.047(3) Uani 0.3333 1 d D . P . . C4 C 0.7445(13) 0.3525(11) 0.0900(17) 0.090(3) Uani 0.3333 1 d D U P A -1 H4 H 0.7137 0.3091 0.1329 0.108 Uiso 0.3333 1 calc R U P A -1 C5 C 0.7435(13) 0.3009(13) 0.0028(12) 0.102(4) Uani 0.3333 1 d D U P A -1 H5A H 0.6809 0.2814 -0.0109 0.154 Uiso 0.3333 1 calc R U P A -1 H5B H 0.783 0.2471 0.0081 0.154 Uiso 0.3333 1 calc DR U P A -1 H5C H 0.7659 0.3402 -0.0466 0.154 Uiso 0.3333 1 calc R U P A -1 C6 C 0.6833(18) 0.4331(18) 0.0933(19) 0.151(11) Uani 0.3333 1 d D U P A -1 H6A H 0.6196 0.413 0.0891 0.226 Uiso 0.3333 1 calc R U P A -1 H6B H 0.6973 0.4738 0.0419 0.226 Uiso 0.3333 1 calc R U P A -1 H6C H 0.6927 0.4659 0.1509 0.226 Uiso 0.3333 1 calc R U P A -1 N1 N 0.8232(14) 0.4158(12) 0.2327(11) 0.090(3) Uani 0.3333 1 d D . P A -1 H1A H 0.7697 0.3956 0.2515 0.108 Uiso 0.3333 1 calc R U P A -1 C9 C 0.8629(16) 0.4838(14) 0.2855(12) 0.102(4) Uani 0.3333 1 d D U P A -1 H9 H 0.9131 0.5112 0.2481 0.123 Uiso 0.3333 1 calc R U P A -1 C10 C 0.907(2) 0.445(2) 0.3717(17) 0.184(14) Uani 0.3333 1 d D U P A -1 H10A H 0.8591 0.4266 0.4147 0.276 Uiso 0.3333 1 calc R U P A -1 H10B H 0.9453 0.4924 0.4001 0.276 Uiso 0.3333 1 calc R U P A -1 H10C H 0.9446 0.3924 0.3558 0.276 Uiso 0.3333 1 calc R U P A -1 C11 C 0.7952(16) 0.5545(17) 0.299(2) 0.165(11) Uani 0.3333 1 d D U P A -1 H11A H 0.7548 0.5569 0.2454 0.247 Uiso 0.3333 1 calc R U P A -1 H11B H 0.8257 0.6135 0.3063 0.247 Uiso 0.3333 1 calc R U P A -1 H11C H 0.759 0.5408 0.3534 0.247 Uiso 0.3333 1 calc R U P A -1 C7 C 0.9169(16) 0.3905(16) -0.0494(13) 0.053(6) Uani 0.3333 1 d D U P . 1 O1 O 0.8995(10) 0.3537(11) -0.1178(10) 0.075(4) Uani 0.3333 1 d D . P . 1 C8 C 1.042(2) 0.444(3) 0.128(3) 0.065(14) Uani 0.3333 1 d D U P . 1 O2 O 1.0997(15) 0.4422(15) 0.1804(18) 0.097(10) Uani 0.3333 1 d D . P . 1 Co1 Co 0.94728(3) 0.44728(3) 0.05272(3) 0.0516(4) Uani 1 3 d DS T P . . C12 C 0.8615(18) 0.5293(16) 0.0309(19) 0.052(6) Uani 0.3333 1 d D U P . 1 O3 O 0.8103(14) 0.5875(14) 0.0159(11) 0.069(5) Uani 0.3333 1 d D . P . 1 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 0.073(6) 0.094(7) 0.103(7) 0.024(5) 0.023(6) -0.025(6) C2 0.095(7) 0.108(8) 0.104(7) 0.009(6) -0.008(6) -0.013(6) C3 0.130(14) 0.109(13) 0.132(14) 0.067(11) -0.040(11) -0.055(11) P1 0.067(7) 0.037(4) 0.038(4) 0.004(4) 0.010(3) 0.001(3) C4 0.073(6) 0.094(7) 0.103(7) 0.024(5) 0.023(6) -0.025(6) C5 0.095(7) 0.108(8) 0.104(7) 0.009(6) -0.008(6) -0.013(6) C6 0.110(16) 0.22(2) 0.119(17) -0.016(16) 0.025(15) -0.002(18) N1 0.073(6) 0.094(7) 0.103(7) 0.024(5) 0.023(6) -0.025(6) C9 0.095(7) 0.108(8) 0.104(7) 0.009(6) -0.008(6) -0.013(6) C10 0.25(3) 0.21(3) 0.086(14) -0.007(16) -0.027(17) -0.02(2) C11 0.150(18) 0.150(19) 0.19(2) 0.014(16) 0.085(16) 0.011(16) C7 0.045(10) 0.057(10) 0.058(10) 0.017(8) -0.006(7) -0.013(8) O1 0.059(9) 0.087(9) 0.078(8) -0.012(7) -0.010(6) 0.000(6) C8 0.067(17) 0.065(19) 0.064(16) 0.003(11) 0.012(11) -0.001(11) O2 0.092(14) 0.09(2) 0.114(18) 0.036(16) -0.035(14) -0.012(15) Co1 0.0516(4) 0.0516(4) 0.0516(4) 0.0082(2) 0.0082(2) -0.0082(2) C12 0.064(11) 0.043(8) 0.049(11) -0.001(8) 0.009(8) -0.012(8) O3 0.080(8) 0.070(8) 0.058(11) 0.007(8) 0.017(8) 0.014(7) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' N N 0.0061 0.0033 '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 C3 C1 C2 116.3(16) . . ? C3 C1 P1 114.6(10) . . ? C2 C1 P1 120.7(13) . . ? C3 C1 H1 99.7 . . ? C2 C1 H1 99.7 . . ? P1 C1 H1 99.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P1 P1 P1 60.004(13) 8_645 11_556 ? P1 P1 N1 140(4) 8_645 . ? P1 P1 N1 141(4) 11_556 . ? P1 P1 C1 75(4) 8_645 . ? N1 P1 C1 111.5(11) . . ? P1 P1 C4 100(4) 11_556 . ? N1 P1 C4 97.1(11) . . ? C1 P1 C4 99.0(9) . . ? P1 P1 Co1 84.8(3) 8_645 . ? P1 P1 Co1 84.8(3) 11_556 . ? N1 P1 Co1 122.4(9) . . ? C1 P1 Co1 114.6(6) . . ? C4 P1 Co1 107.6(11) . . ? C6 C4 C5 115.2(16) . . ? C6 C4 P1 113.0(11) . . ? C5 C4 P1 118.5(12) . . ? C6 C4 H4 102.3 . . ? C5 C4 H4 102.3 . . ? P1 C4 H4 102.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 N1 P1 128.0(16) . . ? C9 N1 H1A 116 . . ? P1 N1 H1A 116 . . ? N1 C9 C11 108(2) . . ? N1 C9 C10 112(2) . . ? C11 C9 C10 116(2) . . ? N1 C9 H9 106.9 . . ? C11 C9 H9 106.9 . . ? C10 C9 H9 106.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C7 O1 98(3) 11_556 . ? C12 C7 O1 104.1(19) 8_645 . ? C8 C7 O2 59(3) 11_556 11_556 ? C12 C7 O2 65.6(19) 8_645 11_556 ? O1 C7 O3 60.3(13) . 8_645 ? C8 C7 Co1 81(2) 11_556 . ? C12 C7 Co1 74.8(13) 8_645 . ? O1 C7 Co1 178(2) . . ? O2 C7 Co1 140(2) 11_556 . ? O3 C7 Co1 118.4(15) 8_645 . ? O2 O1 C7 80.9(18) 11_556 . ? O2 O1 C8 59.4(16) 11_556 11_556 ? C7 O1 O3 75.8(16) . 8_645 ? C8 O1 O3 54.1(16) 11_556 8_645 ? C12 C8 C7 166(4) 11_556 8_645 ? C12 C8 O2 95(4) 11_556 . ? C7 C8 O2 99(4) 8_645 . ? C12 C8 O3 65(3) 11_556 11_556 ? C7 C8 O3 129(3) 8_645 11_556 ? C12 C8 O1 133(3) 11_556 8_645 ? C7 C8 O1 61(3) 8_645 8_645 ? O3 C8 O1 68.4(12) 11_556 8_645 ? C12 C8 Co1 83(3) 11_556 . ? C7 C8 Co1 83(2) 8_645 . ? O2 C8 Co1 176(4) . . ? O3 C8 Co1 148(3) 11_556 . ? O1 C8 Co1 143(3) 8_645 . ? O3 O2 O1 155(6) 11_556 8_645 ? O3 O2 C8 85(3) 11_556 . ? O1 O2 C8 82(3) 8_645 . ? O3 O2 C12 65(2) 11_556 11_556 ? O1 O2 C12 102(2) 8_645 11_556 ? O3 O2 C7 106(2) 11_556 8_645 ? O1 O2 C7 60.2(17) 8_645 8_645 ? C8 Co1 C8 119.4(5) 11_556 . ? C8 Co1 C8 119.4(5) 11_556 8_645 ? C8 Co1 C8 119.4(5) . 8_645 ? C8 Co1 C12 105.3(18) . 8_645 ? C8 Co1 C12 133.3(18) 8_645 8_645 ? C8 Co1 C12 133.3(18) 11_556 11_556 ? C8 Co1 C12 105.3(18) 8_645 11_556 ? C12 Co1 C12 119.3(3) 8_645 11_556 ? C8 Co1 C12 105.3(18) 11_556 . ? C8 Co1 C12 133.3(18) . . ? C12 Co1 C12 119.3(3) 8_645 . ? C12 Co1 C12 119.3(3) 11_556 . ? C8 Co1 C7 103.4(15) 11_556 8_645 ? C8 Co1 C7 135.3(15) 8_645 8_645 ? C12 Co1 C7 89.3(15) 8_645 8_645 ? C12 Co1 C7 149.0(15) . 8_645 ? C8 Co1 C7 135.3(15) 11_556 11_556 ? C8 Co1 C7 103.4(15) . 11_556 ? C12 Co1 C7 149.0(15) 8_645 11_556 ? C12 Co1 C7 89.3(15) 11_556 11_556 ? C7 Co1 C7 119.5(2) 8_645 11_556 ? C8 Co1 C7 135.3(15) . . ? C8 Co1 C7 103.4(15) 8_645 . ? C12 Co1 C7 149.0(16) 11_556 . ? C12 Co1 C7 89.3(15) . . ? C7 Co1 C7 119.5(2) 8_645 . ? C7 Co1 C7 119.5(2) 11_556 . ? C8 Co1 P1 100.5(18) 11_556 . ? C8 Co1 P1 92.7(18) . . ? C8 Co1 P1 90.4(18) 8_645 . ? C12 Co1 P1 101.0(11) 8_645 . ? C12 Co1 P1 91.8(12) 11_556 . ? C12 Co1 P1 92.1(11) . . ? C7 Co1 P1 94.0(10) 8_645 . ? C7 Co1 P1 88.9(9) 11_556 . ? C7 Co1 P1 99.4(9) . . ? C8 Co1 P1 92.7(18) 11_556 11_556 ? C8 Co1 P1 90.4(18) . 11_556 ? C8 Co1 P1 100.5(18) 8_645 11_556 ? C12 Co1 P1 91.8(12) 8_645 11_556 ? C12 Co1 P1 92.1(11) 11_556 11_556 ? C12 Co1 P1 101.0(11) . 11_556 ? C7 Co1 P1 88.9(9) 8_645 11_556 ? C7 Co1 P1 99.4(9) 11_556 11_556 ? C7 Co1 P1 94.0(10) . 11_556 ? C8 Co1 P1 90.4(18) 11_556 8_645 ? C8 Co1 P1 100.5(18) . 8_645 ? C8 Co1 P1 92.7(18) 8_645 8_645 ? C12 Co1 P1 92.1(11) 8_645 8_645 ? C12 Co1 P1 101.0(11) 11_556 8_645 ? C12 Co1 P1 91.8(12) . 8_645 ? C7 Co1 P1 99.4(9) 8_645 8_645 ? C7 Co1 P1 94.0(10) 11_556 8_645 ? C7 Co1 P1 88.9(9) . 8_645 ? C8 C12 O3 95(3) 8_645 . ? C7 C12 O3 103(2) 11_556 . ? C8 C12 O2 65(3) 8_645 8_645 ? C7 C12 O2 73(2) 11_556 8_645 ? C8 C12 Co1 82(3) 8_645 . ? C7 C12 Co1 75.0(13) 11_556 . ? O3 C12 Co1 175(3) . . ? O2 C12 Co1 148(2) 8_645 . ? O1 C12 Co1 118.0(16) 11_556 . ? O2 O3 C12 84(3) 8_645 . ? O2 O3 C8 64(2) 8_645 8_645 ? C12 O3 O1 77.4(19) . 11_556 ? C8 O3 O1 57.5(18) 8_645 11_556 ? O2 O3 C7 52(2) 8_645 11_556 ? 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 C1 C3 1.474(12) . ? C1 C2 1.478(12) . ? C1 P1 1.909(15) . ? C1 H1 1 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? P1 P1 0.40(2) 8_645 ? P1 P1 0.40(2) 11_556 ? P1 N1 1.47(2) . ? P1 C4 1.916(15) . ? P1 Co1 2.194(3) . ? C4 C6 1.482(12) . ? C4 C5 1.483(12) . ? C4 H4 1 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? N1 C9 1.388(17) . ? N1 H1A 0.88 . ? C9 C11 1.445(19) . ? C9 C10 1.524(18) . ? C9 H9 1 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C7 C8 0.49(5) 11_556 ? C7 C12 0.92(5) 8_645 ? C7 O1 1.165(13) . ? C7 O2 1.33(3) 11_556 ? C7 O3 1.63(3) 8_645 ? C7 Co1 1.768(12) . ? O1 O2 0.84(2) 11_556 ? O1 C8 1.32(3) 11_556 ? O1 O3 1.46(3) 8_645 ? O1 C12 1.65(3) 8_645 ? C8 C12 0.44(6) 11_556 ? C8 C7 0.49(5) 8_645 ? C8 O2 1.152(13) . ? C8 O3 1.27(3) 11_556 ? C8 O1 1.32(3) 8_645 ? C8 Co1 1.762(13) . ? O2 O3 0.65(3) 11_556 ? O2 O1 0.84(2) 8_645 ? O2 C12 1.26(2) 11_556 ? O2 C7 1.33(3) 8_645 ? Co1 C8 1.762(13) 11_556 ? Co1 C8 1.762(13) 8_645 ? Co1 C12 1.766(13) 8_645 ? Co1 C12 1.766(13) 11_556 ? Co1 C12 1.766(13) . ? Co1 C7 1.767(12) 8_645 ? Co1 C7 1.767(12) 11_556 ? Co1 P1 2.194(3) 11_556 ? Co1 P1 2.194(3) 8_645 ? C12 C8 0.44(6) 8_645 ? C12 C7 0.92(5) 11_556 ? C12 O3 1.156(13) . ? C12 O2 1.26(2) 8_645 ? C12 O1 1.65(3) 11_556 ? O3 O2 0.65(3) 8_645 ? O3 C8 1.27(3) 8_645 ? O3 O1 1.46(3) 11_556 ? O3 C7 1.63(3) 11_556 ?