# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_CoP3Pz _database_code_depnum_ccdc_archive 'CCDC 887455' #TrackingRef '1 Co(PMe3)3Pz (1).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(trimethylphosphine)-(3,5-bis(trifluoromethyl) pyrazolate)cobalt(i) ; _chemical_name_common ;tris(trimethylphosphine)-(3,5-bis(trifluoromethyl) pyrazolate)cobalt(i) ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H28 Co F6 N2 P3' _chemical_formula_sum 'C14 H28 Co F6 N2 P3' _chemical_formula_weight 490.22 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.2208(18) _cell_length_b 16.675(3) _cell_length_c 15.634(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.27(3) _cell_angle_gamma 90.00 _cell_volume 2319.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 119(2) _cell_measurement_reflns_used 5178 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details '(HKL SCALEPACK; Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 119(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9975 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9975 _reflns_number_gt 7420 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+1.0087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(15) _refine_ls_number_reflns 9975 _refine_ls_number_parameters 516 _refine_ls_number_restraints 139 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.55734(6) 0.67047(3) 1.07291(4) 0.02739(15) Uani 1 1 d . . . Co2 Co 1.17547(7) 0.65087(4) 0.54707(4) 0.03479(17) Uani 1 1 d . . . P1 P 0.46060(14) 0.77184(8) 1.13218(8) 0.0351(3) Uani 1 1 d . . . P2 P 0.36733(12) 0.63727(7) 0.95572(8) 0.0325(3) Uani 1 1 d . . . P3 P 0.71729(13) 0.73165(8) 1.00756(9) 0.0338(3) Uani 1 1 d . . . P4 P 1.03032(18) 0.63047(10) 0.40970(10) 0.0566(4) Uani 1 1 d U . . P5 P 1.34709(18) 0.55294(10) 0.56335(11) 0.0546(4) Uani 1 1 d . . . P6 P 1.3083(2) 0.75962(9) 0.53639(11) 0.0563(4) Uani 1 1 d . . . N1 N 0.6701(4) 0.5699(2) 1.1241(3) 0.0303(9) Uani 1 1 d . . . N2 N 0.7936(4) 0.5499(2) 1.0978(3) 0.0348(9) Uani 1 1 d . . . N3 N 1.0585(4) 0.6216(2) 0.6353(3) 0.0364(10) Uani 1 1 d . . . N4 N 1.0629(5) 0.5452(3) 0.6626(3) 0.0436(11) Uani 1 1 d . . . F1 F 0.5273(4) 0.5694(2) 1.2766(2) 0.0789(12) Uani 1 1 d . . . F2 F 0.3797(3) 0.5345(3) 1.1555(3) 0.0759(11) Uani 1 1 d . . . F3 F 0.4837(5) 0.4457(2) 1.2483(3) 0.0935(15) Uani 1 1 d . . . F4 F 0.9845(4) 0.4509(2) 1.0328(3) 0.0783(12) Uani 1 1 d . . . F5 F 1.0957(4) 0.4599(3) 1.1709(3) 0.1016(17) Uani 1 1 d . . . F6 F 0.9640(4) 0.35759(19) 1.1216(2) 0.0585(9) Uani 1 1 d . . . F7 F 1.0521(5) 0.7941(2) 0.6810(3) 0.0817(12) Uani 1 1 d . . . F8 F 0.8774(5) 0.7669(3) 0.5673(3) 0.0976(14) Uani 1 1 d . . . F9 F 0.8336(5) 0.7763(3) 0.6945(3) 0.1050(16) Uani 1 1 d . . . F10 F 1.0509(9) 0.4165(7) 0.7710(11) 0.136(5) Uani 0.60 1 d PDU A 1 F10B F 0.8167(11) 0.4497(11) 0.7692(14) 0.132(5) Uani 0.40 1 d PDU A 2 F11 F 0.8272(10) 0.4230(4) 0.6967(5) 0.082(2) Uani 0.60 1 d PDU A 1 F11B F 1.0443(15) 0.4478(8) 0.8316(7) 0.087(4) Uani 0.40 1 d PDU A 2 F12 F 0.8826(14) 0.4745(6) 0.8205(6) 0.122(4) Uani 0.60 1 d PDU A 1 F12B F 0.970(2) 0.3958(7) 0.7093(9) 0.121(5) Uani 0.40 1 d PDU A 2 C1 C 0.3321(7) 0.7421(4) 1.1992(4) 0.0603(17) Uani 1 1 d . . . H1A H 0.3885 0.7128 1.2518 0.090 Uiso 1 1 calc R . . H1B H 0.2527 0.7076 1.1638 0.090 Uiso 1 1 calc R . . H1C H 0.2870 0.7901 1.2176 0.090 Uiso 1 1 calc R . . C2 C 0.3438(6) 0.8462(3) 1.0596(4) 0.0477(14) Uani 1 1 d . . . H2A H 0.3101 0.8865 1.0956 0.072 Uiso 1 1 calc R . . H2B H 0.2562 0.8196 1.0207 0.072 Uiso 1 1 calc R . . H2C H 0.4026 0.8722 1.0236 0.072 Uiso 1 1 calc R . . C3 C 0.5911(7) 0.8370(4) 1.2091(4) 0.0686(19) Uani 1 1 d . . . H3A H 0.6645 0.8590 1.1800 0.103 Uiso 1 1 calc R . . H3B H 0.6437 0.8061 1.2614 0.103 Uiso 1 1 calc R . . H3C H 0.5354 0.8811 1.2273 0.103 Uiso 1 1 calc R . . C4 C 0.4008(7) 0.5388(3) 0.9120(4) 0.0563(15) Uani 1 1 d . . . H4A H 0.3171 0.5254 0.8608 0.085 Uiso 1 1 calc R . . H4B H 0.4087 0.4980 0.9582 0.085 Uiso 1 1 calc R . . H4C H 0.4946 0.5403 0.8937 0.085 Uiso 1 1 calc R . . C5 C 0.1788(6) 0.6227(4) 0.9710(4) 0.0593(17) Uani 1 1 d . . . H5A H 0.1394 0.6742 0.9851 0.089 Uiso 1 1 calc R . . H5B H 0.1839 0.5848 1.0196 0.089 Uiso 1 1 calc R . . H5C H 0.1121 0.6012 0.9162 0.089 Uiso 1 1 calc R . . C6 C 0.3234(6) 0.6981(3) 0.8554(3) 0.0495(14) Uani 1 1 d . . . H6A H 0.4155 0.7079 0.8369 0.074 Uiso 1 1 calc R . . H6B H 0.2806 0.7495 0.8673 0.074 Uiso 1 1 calc R . . H6C H 0.2505 0.6698 0.8081 0.074 Uiso 1 1 calc R . . C7 C 0.7659(5) 0.6777(4) 0.9172(3) 0.0471(13) Uani 1 1 d . . . H7A H 0.8448 0.7071 0.8989 0.071 Uiso 1 1 calc R . . H7B H 0.6767 0.6732 0.8669 0.071 Uiso 1 1 calc R . . H7C H 0.8024 0.6240 0.9375 0.071 Uiso 1 1 calc R . . C8 C 0.9043(5) 0.7489(4) 1.0816(4) 0.0492(14) Uani 1 1 d . . . H8A H 0.9493 0.6975 1.1049 0.074 Uiso 1 1 calc R . . H8B H 0.8959 0.7833 1.1309 0.074 Uiso 1 1 calc R . . H8C H 0.9680 0.7752 1.0487 0.074 Uiso 1 1 calc R . . C9 C 0.6730(6) 0.8310(3) 0.9578(4) 0.0543(16) Uani 1 1 d . . . H9A H 0.6614 0.8691 1.0033 0.081 Uiso 1 1 calc R . . H9B H 0.5792 0.8283 0.9105 0.081 Uiso 1 1 calc R . . H9C H 0.7548 0.8488 0.9331 0.081 Uiso 1 1 calc R . . C10 C 0.5071(6) 0.5139(3) 1.2119(4) 0.0451(14) Uani 1 1 d . . . C11 C 0.6369(5) 0.5092(3) 1.1723(3) 0.0341(11) Uani 1 1 d . . . C12 C 0.7381(5) 0.4479(3) 1.1785(3) 0.0378(12) Uani 1 1 d . . . H12 H 0.7422 0.3981 1.2085 0.045 Uiso 1 1 calc R . . C13 C 0.8328(5) 0.4767(3) 1.1301(3) 0.0333(11) Uani 1 1 d . . . C14 C 0.9699(6) 0.4382(3) 1.1152(4) 0.0483(14) Uani 1 1 d . . . C15 C 1.1100(11) 0.6033(6) 0.3197(5) 0.113(3) Uani 1 1 d U . . H15A H 1.1505 0.5487 0.3291 0.169 Uiso 1 1 calc R . . H15B H 1.1910 0.6407 0.3178 0.169 Uiso 1 1 calc R . . H15C H 1.0318 0.6056 0.2635 0.169 Uiso 1 1 calc R . . C16 C 0.8980(11) 0.7075(6) 0.3571(6) 0.136(3) Uani 1 1 d U . . H16A H 0.8418 0.6893 0.2981 0.204 Uiso 1 1 calc R . . H16B H 0.9527 0.7568 0.3516 0.204 Uiso 1 1 calc R . . H16C H 0.8280 0.7181 0.3933 0.204 Uiso 1 1 calc R . . C17 C 0.9031(10) 0.5473(7) 0.4080(6) 0.122(3) Uani 1 1 d U . . H17A H 0.8330 0.5611 0.4432 0.182 Uiso 1 1 calc R . . H17B H 0.9609 0.4997 0.4331 0.182 Uiso 1 1 calc R . . H17C H 0.8466 0.5363 0.3467 0.182 Uiso 1 1 calc R . . C18 C 1.2759(9) 0.4502(4) 0.5430(6) 0.093(3) Uani 1 1 d . . . H18A H 1.2389 0.4411 0.4790 0.139 Uiso 1 1 calc R . . H18B H 1.1937 0.4422 0.5711 0.139 Uiso 1 1 calc R . . H18C H 1.3572 0.4122 0.5681 0.139 Uiso 1 1 calc R . . C19 C 1.4624(8) 0.5446(5) 0.6791(5) 0.080(2) Uani 1 1 d . . . H19A H 1.3973 0.5328 0.7179 0.120 Uiso 1 1 calc R . . H19B H 1.5154 0.5953 0.6973 0.120 Uiso 1 1 calc R . . H19C H 1.5358 0.5012 0.6835 0.120 Uiso 1 1 calc R . . C20 C 1.5011(10) 0.5570(6) 0.5083(7) 0.118(4) Uani 1 1 d . . . H20A H 1.5719 0.5131 0.5301 0.177 Uiso 1 1 calc R . . H20B H 1.5537 0.6084 0.5214 0.177 Uiso 1 1 calc R . . H20C H 1.4596 0.5516 0.4440 0.177 Uiso 1 1 calc R . . C21 C 1.2100(12) 0.8564(4) 0.5245(7) 0.117(3) Uani 1 1 d . . . H21A H 1.2788 0.8991 0.5172 0.175 Uiso 1 1 calc R . . H21B H 1.1754 0.8669 0.5775 0.175 Uiso 1 1 calc R . . H21C H 1.1234 0.8548 0.4723 0.175 Uiso 1 1 calc R . . C22 C 1.3976(11) 0.7679(5) 0.4464(6) 0.118(4) Uani 1 1 d . . . H22A H 1.4388 0.8221 0.4459 0.177 Uiso 1 1 calc R . . H22B H 1.3233 0.7577 0.3899 0.177 Uiso 1 1 calc R . . H22C H 1.4791 0.7286 0.4548 0.177 Uiso 1 1 calc R . . C23 C 1.4650(10) 0.7808(5) 0.6321(6) 0.106(3) Uani 1 1 d . . . H23A H 1.5395 0.7377 0.6393 0.159 Uiso 1 1 calc R . . H23B H 1.4284 0.7843 0.6854 0.159 Uiso 1 1 calc R . . H23C H 1.5116 0.8318 0.6230 0.159 Uiso 1 1 calc R . . C24 C 0.9299(7) 0.7495(4) 0.6515(4) 0.0588(16) Uani 1 1 d . . . C25 C 0.9572(5) 0.6624(4) 0.6686(3) 0.0416(12) Uani 1 1 d . . . C26 C 0.8943(6) 0.6118(4) 0.7177(4) 0.0517(15) Uani 1 1 d . . . H26 H 0.8207 0.6237 0.7484 0.062 Uiso 1 1 calc R . . C27 C 0.9630(6) 0.5392(4) 0.7120(3) 0.0463(13) Uani 1 1 d . A . C28 C 0.9409(7) 0.4615(4) 0.7519(4) 0.0677(17) Uani 1 1 d DU . . 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 0.0241(3) 0.0262(3) 0.0335(3) 0.0019(3) 0.0105(2) 0.0026(3) Co2 0.0385(3) 0.0351(4) 0.0327(3) 0.0029(3) 0.0127(3) 0.0011(3) P1 0.0354(7) 0.0351(7) 0.0354(7) -0.0028(6) 0.0102(6) 0.0072(6) P2 0.0285(6) 0.0311(7) 0.0375(6) -0.0020(6) 0.0080(5) 0.0009(5) P3 0.0291(7) 0.0318(7) 0.0451(7) 0.0026(6) 0.0180(6) -0.0002(5) P4 0.0613(9) 0.0649(11) 0.0381(7) 0.0012(7) 0.0030(7) -0.0128(8) P5 0.0579(9) 0.0564(10) 0.0594(9) 0.0112(8) 0.0330(8) 0.0199(8) P6 0.0760(11) 0.0473(9) 0.0527(9) -0.0093(8) 0.0294(8) -0.0225(8) N1 0.023(2) 0.027(2) 0.040(2) 0.0053(18) 0.0060(17) 0.0034(16) N2 0.027(2) 0.030(2) 0.049(2) 0.002(2) 0.0124(19) 0.0036(17) N3 0.037(2) 0.039(3) 0.034(2) 0.0034(19) 0.0119(18) 0.0021(18) N4 0.048(3) 0.040(3) 0.046(3) 0.001(2) 0.019(2) -0.005(2) F1 0.079(3) 0.094(3) 0.076(3) -0.024(2) 0.044(2) 0.002(2) F2 0.0346(18) 0.117(3) 0.080(2) 0.031(2) 0.0229(18) 0.0075(19) F3 0.108(3) 0.063(2) 0.141(4) 0.050(3) 0.090(3) 0.022(2) F4 0.080(3) 0.074(3) 0.103(3) 0.021(2) 0.065(2) 0.027(2) F5 0.0290(19) 0.097(3) 0.163(4) -0.067(3) -0.003(2) 0.007(2) F6 0.0552(19) 0.0386(19) 0.083(2) 0.0004(17) 0.0199(18) 0.0167(15) F7 0.091(3) 0.046(2) 0.109(3) -0.007(2) 0.027(2) -0.003(2) F8 0.133(4) 0.068(3) 0.073(3) 0.012(2) -0.005(3) 0.038(3) F9 0.093(3) 0.083(3) 0.158(4) -0.018(3) 0.065(3) 0.032(2) F10 0.068(5) 0.110(10) 0.224(13) 0.110(9) 0.025(7) 0.003(5) F10B 0.056(6) 0.144(13) 0.197(15) 0.109(11) 0.034(8) -0.012(7) F11 0.099(6) 0.059(4) 0.080(5) 0.004(4) 0.007(4) -0.038(4) F11B 0.106(8) 0.053(7) 0.081(7) 0.023(6) -0.012(6) -0.032(6) F12 0.186(10) 0.131(7) 0.067(5) -0.006(5) 0.063(6) -0.090(7) F12B 0.223(15) 0.062(7) 0.087(9) -0.009(7) 0.056(10) -0.041(10) C1 0.072(4) 0.066(4) 0.056(4) 0.008(3) 0.040(3) 0.025(3) C2 0.046(3) 0.047(3) 0.049(3) 0.000(3) 0.012(3) 0.017(3) C3 0.068(4) 0.054(4) 0.070(4) -0.018(3) -0.007(4) 0.011(3) C4 0.070(4) 0.033(3) 0.062(4) -0.016(3) 0.009(3) 0.002(3) C5 0.034(3) 0.080(5) 0.065(4) -0.007(3) 0.014(3) -0.011(3) C6 0.050(3) 0.050(3) 0.042(3) 0.004(3) 0.000(3) 0.004(3) C7 0.040(3) 0.063(4) 0.044(3) -0.004(3) 0.021(2) 0.002(3) C8 0.038(3) 0.053(4) 0.060(3) -0.012(3) 0.019(3) -0.007(3) C9 0.043(3) 0.042(3) 0.086(4) 0.026(3) 0.032(3) 0.004(3) C10 0.055(4) 0.041(3) 0.045(3) 0.012(3) 0.024(3) 0.001(3) C11 0.031(3) 0.035(3) 0.035(3) 0.001(2) 0.006(2) -0.002(2) C12 0.040(3) 0.028(3) 0.042(3) 0.004(2) 0.004(2) 0.000(2) C13 0.025(2) 0.029(3) 0.043(3) -0.008(2) 0.004(2) 0.002(2) C14 0.036(3) 0.035(3) 0.072(4) -0.006(3) 0.011(3) 0.004(2) C15 0.136(6) 0.148(7) 0.057(4) -0.037(4) 0.033(4) -0.032(5) C16 0.146(7) 0.122(5) 0.102(6) 0.010(5) -0.035(5) 0.041(5) C17 0.103(5) 0.134(6) 0.111(6) 0.008(5) 0.000(4) -0.065(5) C18 0.109(6) 0.050(4) 0.120(7) -0.019(4) 0.032(5) 0.018(4) C19 0.064(4) 0.087(5) 0.082(5) 0.035(4) 0.009(4) 0.018(4) C20 0.116(6) 0.141(8) 0.134(7) 0.044(7) 0.100(6) 0.061(6) C21 0.178(9) 0.040(4) 0.153(9) 0.022(5) 0.082(8) -0.012(5) C22 0.181(9) 0.098(7) 0.112(6) -0.030(5) 0.104(7) -0.075(6) C23 0.115(6) 0.093(6) 0.098(6) -0.035(5) 0.007(5) -0.048(5) C24 0.048(4) 0.058(4) 0.070(4) -0.008(4) 0.015(3) 0.009(3) C25 0.033(2) 0.055(4) 0.036(3) -0.010(3) 0.007(2) -0.001(3) C26 0.039(3) 0.075(4) 0.046(3) -0.006(3) 0.020(3) -0.007(3) C27 0.039(3) 0.057(4) 0.044(3) 0.001(3) 0.012(3) -0.016(3) C28 0.069(4) 0.078(5) 0.060(4) 0.005(3) 0.025(3) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co1 N1 2.024(4) . ? Co1 P1 2.2241(14) . ? Co1 P2 2.2454(15) . ? Co1 P3 2.2480(13) . ? Co2 N3 2.021(4) . ? Co2 P6 2.2191(16) . ? Co2 P4 2.2373(17) . ? Co2 P5 2.2413(16) . ? P1 C3 1.820(6) . ? P1 C2 1.827(5) . ? P1 C1 1.844(6) . ? P2 C6 1.822(5) . ? P2 C5 1.832(5) . ? P2 C4 1.836(5) . ? P3 C7 1.827(5) . ? P3 C8 1.829(5) . ? P3 C9 1.830(5) . ? P4 C15 1.809(7) . ? P4 C17 1.812(8) . ? P4 C16 1.813(9) . ? P5 C18 1.832(8) . ? P5 C20 1.846(7) . ? P5 C19 1.847(7) . ? P6 C22 1.813(7) . ? P6 C23 1.820(8) . ? P6 C21 1.836(8) . ? N1 C11 1.344(6) . ? N1 N2 1.350(5) . ? N2 C13 1.335(6) . ? N3 N4 1.341(6) . ? N3 C25 1.364(6) . ? N4 C27 1.353(6) . ? F1 C10 1.347(6) . ? F2 C10 1.315(6) . ? F3 C10 1.314(6) . ? F4 C14 1.347(7) . ? F5 C14 1.305(7) . ? F6 C14 1.350(6) . ? F7 C24 1.327(7) . ? F8 C24 1.311(7) . ? F9 C24 1.324(7) . ? F10 C28 1.233(9) . ? F10B C28 1.260(10) . ? F11 C28 1.333(8) . ? F11B C28 1.374(10) . ? F12 C28 1.338(9) . ? F12B C28 1.345(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.486(7) . ? C11 C12 1.371(7) . ? C12 C13 1.383(7) . ? C12 H12 0.9500 . ? C13 C14 1.490(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.486(9) . ? C25 C26 1.368(8) . ? C26 C27 1.380(8) . ? C26 H26 0.9500 . ? C27 C28 1.475(9) . ? 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 N1 Co1 P1 133.28(12) . . ? N1 Co1 P2 109.13(12) . . ? P1 Co1 P2 102.41(5) . . ? N1 Co1 P3 103.04(11) . . ? P1 Co1 P3 103.15(5) . . ? P2 Co1 P3 101.86(5) . . ? N3 Co2 P6 130.76(13) . . ? N3 Co2 P4 109.05(12) . . ? P6 Co2 P4 104.75(6) . . ? N3 Co2 P5 103.55(12) . . ? P6 Co2 P5 102.51(7) . . ? P4 Co2 P5 102.96(7) . . ? C3 P1 C2 100.6(3) . . ? C3 P1 C1 101.4(3) . . ? C2 P1 C1 100.0(3) . . ? C3 P1 Co1 117.5(2) . . ? C2 P1 Co1 119.48(18) . . ? C1 P1 Co1 114.9(2) . . ? C6 P2 C5 100.5(3) . . ? C6 P2 C4 101.5(3) . . ? C5 P2 C4 100.8(3) . . ? C6 P2 Co1 120.91(19) . . ? C5 P2 Co1 119.3(2) . . ? C4 P2 Co1 110.7(2) . . ? C7 P3 C8 100.6(2) . . ? C7 P3 C9 101.0(3) . . ? C8 P3 C9 101.2(3) . . ? C7 P3 Co1 116.87(19) . . ? C8 P3 Co1 113.95(19) . . ? C9 P3 Co1 120.29(17) . . ? C15 P4 C17 101.0(5) . . ? C15 P4 C16 100.8(5) . . ? C17 P4 C16 100.3(5) . . ? C15 P4 Co2 121.5(3) . . ? C17 P4 Co2 110.6(3) . . ? C16 P4 Co2 119.2(3) . . ? C18 P5 C20 103.8(4) . . ? C18 P5 C19 100.8(4) . . ? C20 P5 C19 98.3(4) . . ? C18 P5 Co2 116.9(3) . . ? C20 P5 Co2 121.8(3) . . ? C19 P5 Co2 111.9(3) . . ? C22 P6 C23 101.4(4) . . ? C22 P6 C21 99.6(4) . . ? C23 P6 C21 100.2(5) . . ? C22 P6 Co2 119.6(3) . . ? C23 P6 Co2 115.6(3) . . ? C21 P6 Co2 117.3(3) . . ? C11 N1 N2 108.7(4) . . ? C11 N1 Co1 132.5(3) . . ? N2 N1 Co1 118.1(3) . . ? C13 N2 N1 106.0(4) . . ? N4 N3 C25 108.5(4) . . ? N4 N3 Co2 118.0(3) . . ? C25 N3 Co2 133.0(3) . . ? N3 N4 C27 106.5(4) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F3 C10 F2 107.2(5) . . ? F3 C10 F1 106.0(4) . . ? F2 C10 F1 104.2(5) . . ? F3 C10 C11 112.2(5) . . ? F2 C10 C11 114.2(4) . . ? F1 C10 C11 112.4(5) . . ? N1 C11 C12 110.4(4) . . ? N1 C11 C10 121.4(4) . . ? C12 C11 C10 128.1(5) . . ? C11 C12 C13 102.6(4) . . ? C11 C12 H12 128.7 . . ? C13 C12 H12 128.7 . . ? N2 C13 C12 112.2(4) . . ? N2 C13 C14 119.4(4) . . ? C12 C13 C14 128.3(5) . . ? F5 C14 F4 107.4(5) . . ? F5 C14 F6 105.8(5) . . ? F4 C14 F6 104.1(5) . . ? F5 C14 C13 114.7(5) . . ? F4 C14 C13 112.6(5) . . ? F6 C14 C13 111.4(4) . . ? P4 C15 H15A 109.5 . . ? P4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P4 C16 H16A 109.5 . . ? P4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P4 C17 H17A 109.5 . . ? P4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P5 C18 H18A 109.5 . . ? P5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P5 C19 H19A 109.5 . . ? P5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P5 C20 H20A 109.5 . . ? P5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P6 C21 H21A 109.5 . . ? P6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P6 C22 H22A 109.5 . . ? P6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P6 C23 H23A 109.5 . . ? P6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? F8 C24 F9 108.3(5) . . ? F8 C24 F7 106.2(6) . . ? F9 C24 F7 104.9(5) . . ? F8 C24 C25 113.4(5) . . ? F9 C24 C25 110.1(5) . . ? F7 C24 C25 113.4(5) . . ? N3 C25 C26 109.9(5) . . ? N3 C25 C24 121.3(5) . . ? C26 C25 C24 128.8(5) . . ? C25 C26 C27 103.6(5) . . ? C25 C26 H26 128.2 . . ? C27 C26 H26 128.2 . . ? N4 C27 C26 111.4(5) . . ? N4 C27 C28 119.8(5) . . ? C26 C27 C28 128.8(5) . . ? F10 C28 F11 108.7(9) . . ? F10 C28 F12 112.5(8) . . ? F11 C28 F12 100.5(6) . . ? F10B C28 F12B 106.9(10) . . ? F12 C28 F12B 134.7(9) . . ? F10B C28 F11B 103.4(9) . . ? F12 C28 F11B 68.2(7) . . ? F12B C28 F11B 97.6(9) . . ? F10 C28 C27 116.2(6) . . ? F10B C28 C27 117.5(9) . . ? F11 C28 C27 108.8(6) . . ? F12 C28 C27 109.0(7) . . ? F12B C28 C27 116.0(7) . . ? F11B C28 C27 112.9(7) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 P1 C3 65.9(3) . . . . ? P2 Co1 P1 C3 -162.2(3) . . . . ? P3 Co1 P1 C3 -56.7(3) . . . . ? N1 Co1 P1 C2 -172.0(3) . . . . ? P2 Co1 P1 C2 -40.1(2) . . . . ? P3 Co1 P1 C2 65.5(2) . . . . ? N1 Co1 P1 C1 -53.2(3) . . . . ? P2 Co1 P1 C1 78.7(2) . . . . ? P3 Co1 P1 C1 -175.7(2) . . . . ? N1 Co1 P2 C6 -138.7(2) . . . . ? P1 Co1 P2 C6 76.3(2) . . . . ? P3 Co1 P2 C6 -30.2(2) . . . . ? N1 Co1 P2 C5 95.9(3) . . . . ? P1 Co1 P2 C5 -49.2(3) . . . . ? P3 Co1 P2 C5 -155.7(3) . . . . ? N1 Co1 P2 C4 -20.4(2) . . . . ? P1 Co1 P2 C4 -165.4(2) . . . . ? P3 Co1 P2 C4 88.1(2) . . . . ? N1 Co1 P3 C7 61.9(2) . . . . ? P1 Co1 P3 C7 -157.1(2) . . . . ? P2 Co1 P3 C7 -51.2(2) . . . . ? N1 Co1 P3 C8 -54.9(2) . . . . ? P1 Co1 P3 C8 86.1(2) . . . . ? P2 Co1 P3 C8 -168.0(2) . . . . ? N1 Co1 P3 C9 -175.2(3) . . . . ? P1 Co1 P3 C9 -34.3(3) . . . . ? P2 Co1 P3 C9 71.7(3) . . . . ? N3 Co2 P4 C15 -150.1(4) . . . . ? P6 Co2 P4 C15 66.3(4) . . . . ? P5 Co2 P4 C15 -40.6(4) . . . . ? N3 Co2 P4 C17 -32.1(4) . . . . ? P6 Co2 P4 C17 -175.8(4) . . . . ? P5 Co2 P4 C17 77.4(4) . . . . ? N3 Co2 P4 C16 83.4(5) . . . . ? P6 Co2 P4 C16 -60.3(5) . . . . ? P5 Co2 P4 C16 -167.1(4) . . . . ? N3 Co2 P5 C18 59.2(3) . . . . ? P6 Co2 P5 C18 -163.0(3) . . . . ? P4 Co2 P5 C18 -54.4(3) . . . . ? N3 Co2 P5 C20 -171.9(4) . . . . ? P6 Co2 P5 C20 -34.1(4) . . . . ? P4 Co2 P5 C20 74.5(4) . . . . ? N3 Co2 P5 C19 -56.2(3) . . . . ? P6 Co2 P5 C19 81.6(3) . . . . ? P4 Co2 P5 C19 -169.8(3) . . . . ? N3 Co2 P6 C22 -178.7(4) . . . . ? P4 Co2 P6 C22 -46.4(4) . . . . ? P5 Co2 P6 C22 60.8(4) . . . . ? N3 Co2 P6 C23 59.7(4) . . . . ? P4 Co2 P6 C23 -168.0(4) . . . . ? P5 Co2 P6 C23 -60.8(4) . . . . ? N3 Co2 P6 C21 -58.1(4) . . . . ? P4 Co2 P6 C21 74.1(4) . . . . ? P5 Co2 P6 C21 -178.7(4) . . . . ? P1 Co1 N1 C11 55.9(5) . . . . ? P2 Co1 N1 C11 -73.8(4) . . . . ? P3 Co1 N1 C11 178.5(4) . . . . ? P1 Co1 N1 N2 -135.0(3) . . . . ? P2 Co1 N1 N2 95.2(3) . . . . ? P3 Co1 N1 N2 -12.4(3) . . . . ? C11 N1 N2 C13 0.5(5) . . . . ? Co1 N1 N2 C13 -171.0(3) . . . . ? P6 Co2 N3 N4 -141.4(3) . . . . ? P4 Co2 N3 N4 87.8(3) . . . . ? P5 Co2 N3 N4 -21.3(4) . . . . ? P6 Co2 N3 C25 47.2(5) . . . . ? P4 Co2 N3 C25 -83.6(4) . . . . ? P5 Co2 N3 C25 167.3(4) . . . . ? C25 N3 N4 C27 0.6(5) . . . . ? Co2 N3 N4 C27 -172.8(3) . . . . ? N2 N1 C11 C12 -0.1(5) . . . . ? Co1 N1 C11 C12 169.7(3) . . . . ? N2 N1 C11 C10 179.1(4) . . . . ? Co1 N1 C11 C10 -11.1(7) . . . . ? F3 C10 C11 N1 173.2(5) . . . . ? F2 C10 C11 N1 51.0(7) . . . . ? F1 C10 C11 N1 -67.5(6) . . . . ? F3 C10 C11 C12 -7.7(8) . . . . ? F2 C10 C11 C12 -129.9(6) . . . . ? F1 C10 C11 C12 111.6(6) . . . . ? N1 C11 C12 C13 -0.3(5) . . . . ? C10 C11 C12 C13 -179.5(5) . . . . ? N1 N2 C13 C12 -0.8(5) . . . . ? N1 N2 C13 C14 -177.9(4) . . . . ? C11 C12 C13 N2 0.7(5) . . . . ? C11 C12 C13 C14 177.4(5) . . . . ? N2 C13 C14 F5 82.5(7) . . . . ? C12 C13 C14 F5 -94.0(7) . . . . ? N2 C13 C14 F4 -40.7(7) . . . . ? C12 C13 C14 F4 142.7(5) . . . . ? N2 C13 C14 F6 -157.2(5) . . . . ? C12 C13 C14 F6 26.2(8) . . . . ? N4 N3 C25 C26 -0.4(5) . . . . ? Co2 N3 C25 C26 171.6(4) . . . . ? N4 N3 C25 C24 178.5(5) . . . . ? Co2 N3 C25 C24 -9.5(7) . . . . ? F8 C24 C25 N3 61.8(7) . . . . ? F9 C24 C25 N3 -176.6(5) . . . . ? F7 C24 C25 N3 -59.5(7) . . . . ? F8 C24 C25 C26 -119.5(6) . . . . ? F9 C24 C25 C26 2.1(8) . . . . ? F7 C24 C25 C26 119.2(6) . . . . ? N3 C25 C26 C27 0.1(6) . . . . ? C24 C25 C26 C27 -178.7(5) . . . . ? N3 N4 C27 C26 -0.6(6) . . . . ? N3 N4 C27 C28 179.8(5) . . . . ? C25 C26 C27 N4 0.3(6) . . . . ? C25 C26 C27 C28 179.9(5) . . . . ? N4 C27 C28 F10 29.9(12) . . . . ? C26 C27 C28 F10 -149.7(11) . . . . ? N4 C27 C28 F10B -155.3(13) . . . . ? C26 C27 C28 F10B 25.2(15) . . . . ? N4 C27 C28 F11 -93.1(7) . . . . ? C26 C27 C28 F11 87.3(8) . . . . ? N4 C27 C28 F12 158.1(7) . . . . ? C26 C27 C28 F12 -21.4(10) . . . . ? N4 C27 C28 F12B -27.0(13) . . . . ? C26 C27 C28 F12B 153.5(12) . . . . ? N4 C27 C28 F11B 84.4(10) . . . . ? C26 C27 C28 F11B -95.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.907 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.086 data_CoP3Pz2 _database_code_depnum_ccdc_archive 'CCDC 887456' #TrackingRef '2 Co(PMe3)3Pz2 (2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(trimethylphosphine)-mer-bis(3,5-bis (trifluoromethyl)pyrzolate)cobalt(ii) ; _chemical_name_common ;tris(trimethylphosphine)-mer-bis(3,5-bis (trifluoromethyl)pyrzolate)cobalt(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C19 H29 Co F12 N4 P3' _chemical_formula_sum 'C19 H29 Co F12 N4 P3' _chemical_formula_weight 693.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.3916(8) _cell_length_b 15.6362(12) _cell_length_c 19.3585(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2842.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17672 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20766 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6506 _reflns_number_gt 5775 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.1825P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(12) _refine_ls_number_reflns 6506 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.64031(4) 1.00374(2) 0.649827(18) 0.01190(9) Uani 1 1 d . . . P1 P 0.71069(8) 0.85878(4) 0.61112(4) 0.01679(16) Uani 1 1 d . . . P2 P 0.45111(8) 0.95652(4) 0.71207(4) 0.01450(15) Uani 1 1 d . . . P3 P 0.81601(8) 1.06578(4) 0.58828(4) 0.01596(16) Uani 1 1 d . . . F1 F 0.52625(18) 1.18116(9) 0.66515(8) 0.0220(4) Uani 1 1 d . . . F2 F 0.31254(19) 1.21845(10) 0.63735(9) 0.0306(4) Uani 1 1 d . . . F3 F 0.4884(2) 1.25799(10) 0.57441(9) 0.0291(4) Uani 1 1 d . . . F4 F 0.1732(2) 0.90849(11) 0.48436(9) 0.0320(4) Uani 1 1 d . . . F5 F 0.1749(2) 1.00980(11) 0.41057(9) 0.0392(5) Uani 1 1 d . . . F6 F 0.3390(2) 0.91366(12) 0.40897(10) 0.0380(5) Uani 1 1 d . . . F7 F 0.7763(2) 1.18611(10) 0.73849(9) 0.0300(4) Uani 1 1 d . . . F8 F 0.8101(2) 1.17651(10) 0.84771(10) 0.0422(5) Uani 1 1 d . . . F9 F 0.60699(19) 1.14400(11) 0.80384(11) 0.0352(5) Uani 1 1 d . . . F10 F 0.9411(2) 0.83358(10) 0.89865(9) 0.0313(4) Uani 1 1 d . . . F11 F 1.11756(18) 0.86485(11) 0.83307(11) 0.0360(5) Uani 1 1 d . . . F12 F 0.9542(2) 0.77907(10) 0.79674(10) 0.0331(5) Uani 1 1 d . . . N1 N 0.4993(2) 1.03975(13) 0.57874(12) 0.0140(5) Uani 1 1 d . . . N2 N 0.4524(3) 0.98044(13) 0.53389(12) 0.0159(5) Uani 1 1 d . . . N3 N 0.7631(2) 0.99611(15) 0.73341(10) 0.0132(4) Uani 1 1 d . . . N4 N 0.8251(2) 0.91891(14) 0.74505(12) 0.0165(5) Uani 1 1 d . . . C1 C 0.9014(3) 0.83435(18) 0.59946(17) 0.0250(7) Uani 1 1 d . . . H1A H 0.9507 0.8396 0.6439 0.038 Uiso 1 1 calc R . . H1B H 0.9429 0.8746 0.5663 0.038 Uiso 1 1 calc R . . H1C H 0.9119 0.7758 0.5820 0.038 Uiso 1 1 calc R . . C2 C 0.6658(3) 0.76699(16) 0.66625(16) 0.0230(7) Uani 1 1 d . . . H2A H 0.5625 0.7649 0.6732 0.035 Uiso 1 1 calc R . . H2B H 0.7134 0.7731 0.7110 0.035 Uiso 1 1 calc R . . H2C H 0.6976 0.7141 0.6439 0.035 Uiso 1 1 calc R . . C3 C 0.6398(4) 0.82053(17) 0.52877(15) 0.0279(7) Uani 1 1 d . . . H3A H 0.6818 0.7648 0.5178 0.042 Uiso 1 1 calc R . . H3B H 0.6636 0.8615 0.4922 0.042 Uiso 1 1 calc R . . H3C H 0.5362 0.8149 0.5321 0.042 Uiso 1 1 calc R . . C4 C 0.4926(3) 0.89989(17) 0.79165(15) 0.0207(6) Uani 1 1 d . . . H4A H 0.4040 0.8825 0.8144 0.031 Uiso 1 1 calc R . . H4B H 0.5467 0.9376 0.8224 0.031 Uiso 1 1 calc R . . H4C H 0.5495 0.8490 0.7810 0.031 Uiso 1 1 calc R . . C5 C 0.3289(3) 1.03942(18) 0.74185(15) 0.0227(7) Uani 1 1 d . . . H5A H 0.2866 1.0684 0.7019 0.034 Uiso 1 1 calc R . . H5B H 0.3810 1.0811 0.7699 0.034 Uiso 1 1 calc R . . H5C H 0.2533 1.0133 0.7697 0.034 Uiso 1 1 calc R . . C6 C 0.3260(3) 0.88724(17) 0.66730(15) 0.0227(7) Uani 1 1 d . . . H6A H 0.3773 0.8388 0.6470 0.034 Uiso 1 1 calc R . . H6B H 0.2783 0.9196 0.6306 0.034 Uiso 1 1 calc R . . H6C H 0.2548 0.8660 0.7001 0.034 Uiso 1 1 calc R . . C7 C 0.8322(3) 1.02980(18) 0.49875(15) 0.0252(7) Uani 1 1 d . . . H7A H 0.9038 1.0645 0.4749 0.038 Uiso 1 1 calc R . . H7B H 0.7402 1.0360 0.4754 0.038 Uiso 1 1 calc R . . H7C H 0.8612 0.9696 0.4980 0.038 Uiso 1 1 calc R . . C8 C 0.8014(4) 1.18030(17) 0.57239(16) 0.0245(7) Uani 1 1 d . . . H8A H 0.7864 1.2102 0.6163 0.037 Uiso 1 1 calc R . . H8B H 0.7207 1.1913 0.5416 0.037 Uiso 1 1 calc R . . H8C H 0.8893 1.2010 0.5508 0.037 Uiso 1 1 calc R . . C9 C 0.9930(3) 1.0564(2) 0.62529(16) 0.0270(7) Uani 1 1 d . . . H9A H 1.0635 1.0778 0.5922 0.041 Uiso 1 1 calc R . . H9B H 1.0129 0.9963 0.6357 0.041 Uiso 1 1 calc R . . H9C H 0.9981 1.0901 0.6679 0.041 Uiso 1 1 calc R . . C10 C 0.4384(3) 1.19139(17) 0.61149(15) 0.0198(6) Uani 1 1 d . . . C11 C 0.4209(3) 1.11261(16) 0.56998(14) 0.0146(6) Uani 1 1 d . . . C12 C 0.3205(3) 1.09938(16) 0.51905(14) 0.0157(6) Uani 1 1 d . . . H12 H 0.2509 1.1382 0.5022 0.019 Uiso 1 1 calc R . . C13 C 0.3454(3) 1.01632(15) 0.49851(14) 0.0155(6) Uani 1 1 d . . . C14 C 0.2597(3) 0.96265(17) 0.45051(15) 0.0199(6) Uani 1 1 d . . . C15 C 0.7473(3) 1.13790(18) 0.79439(15) 0.0214(6) Uani 1 1 d . . . C16 C 0.7973(3) 1.04850(16) 0.78739(14) 0.0157(6) Uani 1 1 d . . . C17 C 0.8819(3) 1.00563(17) 0.83445(13) 0.0184(6) Uani 1 1 d . . . H17 H 0.9213 1.0263 0.8765 0.022 Uiso 1 1 calc R . . C18 C 0.8952(3) 0.92471(17) 0.80508(14) 0.0147(6) Uani 1 1 d . . . C19 C 0.9762(3) 0.85065(18) 0.83273(15) 0.0208(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01311(17) 0.01154(16) 0.01104(17) 0.00065(14) -0.00055(14) -0.00059(15) P1 0.0201(4) 0.0130(3) 0.0173(4) -0.0013(3) 0.0012(3) 0.0007(3) P2 0.0146(3) 0.0146(3) 0.0143(4) 0.0015(3) 0.0017(3) 0.0007(3) P3 0.0163(4) 0.0171(3) 0.0145(4) 0.0013(3) 0.0005(3) -0.0031(3) F1 0.0298(10) 0.0183(7) 0.0178(9) -0.0036(7) -0.0081(7) 0.0012(7) F2 0.0261(10) 0.0277(9) 0.0379(11) -0.0104(8) -0.0022(9) 0.0105(8) F3 0.0464(12) 0.0136(7) 0.0272(10) 0.0057(7) -0.0095(9) -0.0025(8) F4 0.0335(11) 0.0352(9) 0.0274(10) 0.0002(8) 0.0012(9) -0.0185(9) F5 0.0466(12) 0.0372(10) 0.0337(11) 0.0055(9) -0.0258(9) -0.0054(10) F6 0.0284(11) 0.0507(11) 0.0347(11) -0.0258(9) 0.0061(9) -0.0112(9) F7 0.0454(12) 0.0173(8) 0.0273(10) 0.0050(7) -0.0040(9) 0.0002(8) F8 0.0663(14) 0.0267(9) 0.0336(11) -0.0147(9) -0.0314(11) 0.0101(10) F9 0.0267(11) 0.0285(9) 0.0504(13) -0.0017(9) 0.0079(9) 0.0121(8) F10 0.0346(11) 0.0358(10) 0.0234(10) 0.0136(8) -0.0015(8) 0.0067(8) F11 0.0141(10) 0.0370(10) 0.0568(14) 0.0178(9) -0.0032(9) 0.0046(8) F12 0.0390(11) 0.0211(9) 0.0394(12) -0.0014(8) -0.0126(10) 0.0111(8) N1 0.0183(13) 0.0112(10) 0.0124(12) 0.0020(9) -0.0036(9) -0.0028(9) N2 0.0186(12) 0.0152(11) 0.0139(12) -0.0013(9) -0.0009(10) -0.0038(10) N3 0.0108(11) 0.0140(10) 0.0149(11) 0.0026(10) -0.0016(8) 0.0007(10) N4 0.0126(12) 0.0176(11) 0.0194(13) 0.0013(9) -0.0015(10) 0.0021(9) C1 0.0266(18) 0.0208(15) 0.0277(18) 0.0029(13) 0.0063(14) 0.0068(12) C2 0.0277(18) 0.0106(12) 0.0307(18) 0.0018(11) 0.0071(14) 0.0004(12) C3 0.039(2) 0.0195(14) 0.0248(17) -0.0065(13) -0.0036(15) 0.0054(15) C4 0.0213(16) 0.0217(14) 0.0191(16) 0.0032(12) 0.0021(13) 0.0024(12) C5 0.0229(17) 0.0217(14) 0.0236(16) 0.0024(12) 0.0065(13) 0.0049(13) C6 0.0194(17) 0.0235(14) 0.0253(17) -0.0001(12) 0.0032(13) -0.0015(12) C7 0.0308(18) 0.0271(15) 0.0177(15) -0.0003(12) 0.0029(13) -0.0014(13) C8 0.0310(18) 0.0192(14) 0.0234(17) 0.0040(12) 0.0036(14) -0.0072(14) C9 0.0192(16) 0.0343(16) 0.0276(18) 0.0029(14) 0.0008(13) -0.0023(14) C10 0.0216(16) 0.0187(14) 0.0191(16) -0.0004(12) -0.0063(13) 0.0059(12) C11 0.0171(15) 0.0129(12) 0.0136(15) 0.0021(11) -0.0011(11) -0.0001(11) C12 0.0143(14) 0.0173(13) 0.0156(14) 0.0055(11) -0.0005(11) 0.0002(11) C13 0.0176(14) 0.0164(13) 0.0125(13) 0.0021(10) 0.0015(11) -0.0027(11) C14 0.0231(16) 0.0232(15) 0.0135(14) -0.0002(12) -0.0005(12) -0.0023(13) C15 0.0257(16) 0.0200(14) 0.0184(16) -0.0020(13) -0.0061(13) 0.0013(13) C16 0.0145(14) 0.0172(13) 0.0153(14) 0.0010(11) -0.0001(11) 0.0012(11) C17 0.0178(14) 0.0242(14) 0.0132(14) -0.0029(12) -0.0039(10) -0.0019(13) C18 0.0108(14) 0.0192(13) 0.0140(14) 0.0031(11) -0.0010(10) 0.0009(11) C19 0.0192(16) 0.0229(14) 0.0201(17) 0.0043(12) -0.0037(12) 0.0033(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co1 N3 1.990(2) . ? Co1 N1 1.991(2) . ? Co1 P3 2.2548(8) . ? Co1 P2 2.2703(8) . ? Co1 P1 2.4772(8) . ? P1 C3 1.828(3) . ? P1 C2 1.837(3) . ? P1 C1 1.845(3) . ? P2 C6 1.818(3) . ? P2 C4 1.819(3) . ? P2 C5 1.825(3) . ? P3 C9 1.816(3) . ? P3 C8 1.822(3) . ? P3 C7 1.828(3) . ? F1 C10 1.336(3) . ? F2 C10 1.352(3) . ? F3 C10 1.349(3) . ? F4 C14 1.344(3) . ? F5 C14 1.332(3) . ? F6 C14 1.337(3) . ? F7 C15 1.347(3) . ? F8 C15 1.333(3) . ? F9 C15 1.334(3) . ? F10 C19 1.345(3) . ? F11 C19 1.346(3) . ? F12 C19 1.334(3) . ? N1 N2 1.345(3) . ? N1 C11 1.367(3) . ? N2 C13 1.339(3) . ? N3 N4 1.359(3) . ? N3 C16 1.366(3) . ? N4 C18 1.339(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.480(4) . ? C11 C12 1.380(4) . ? C12 C13 1.378(4) . ? C12 H12 0.9500 . ? C13 C14 1.489(4) . ? C15 C16 1.481(4) . ? C16 C17 1.382(4) . ? C17 C18 1.393(4) . ? C17 H17 0.9500 . ? C18 C19 1.485(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 N3 Co1 N1 164.60(9) . . ? N3 Co1 P3 91.80(7) . . ? N1 Co1 P3 89.99(7) . . ? N3 Co1 P2 90.14(7) . . ? N1 Co1 P2 86.46(7) . . ? P3 Co1 P2 173.31(3) . . ? N3 Co1 P1 92.09(7) . . ? N1 Co1 P1 103.13(6) . . ? P3 Co1 P1 92.21(3) . . ? P2 Co1 P1 94.12(3) . . ? C3 P1 C2 99.64(14) . . ? C3 P1 C1 100.31(15) . . ? C2 P1 C1 97.58(14) . . ? C3 P1 Co1 117.77(10) . . ? C2 P1 Co1 118.54(9) . . ? C1 P1 Co1 119.04(10) . . ? C6 P2 C4 104.60(14) . . ? C6 P2 C5 99.63(14) . . ? C4 P2 C5 102.30(14) . . ? C6 P2 Co1 116.53(10) . . ? C4 P2 Co1 116.11(10) . . ? C5 P2 Co1 115.41(10) . . ? C9 P3 C8 102.40(15) . . ? C9 P3 C7 105.86(15) . . ? C8 P3 C7 98.55(14) . . ? C9 P3 Co1 115.26(11) . . ? C8 P3 Co1 117.19(11) . . ? C7 P3 Co1 115.42(10) . . ? N2 N1 C11 108.5(2) . . ? N2 N1 Co1 117.99(16) . . ? C11 N1 Co1 132.81(18) . . ? C13 N2 N1 106.7(2) . . ? N4 N3 C16 107.8(2) . . ? N4 N3 Co1 115.86(17) . . ? C16 N3 Co1 136.23(19) . . ? C18 N4 N3 107.1(2) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F1 C10 F3 106.9(2) . . ? F1 C10 F2 106.8(2) . . ? F3 C10 F2 105.1(2) . . ? F1 C10 C11 113.0(2) . . ? F3 C10 C11 113.1(2) . . ? F2 C10 C11 111.4(2) . . ? N1 C11 C12 109.4(2) . . ? N1 C11 C10 124.5(2) . . ? C12 C11 C10 126.0(2) . . ? C13 C12 C11 103.4(2) . . ? C13 C12 H12 128.3 . . ? C11 C12 H12 128.3 . . ? N2 C13 C12 112.0(2) . . ? N2 C13 C14 119.3(2) . . ? C12 C13 C14 128.3(3) . . ? F5 C14 F6 107.5(2) . . ? F5 C14 F4 105.7(2) . . ? F6 C14 F4 105.6(2) . . ? F5 C14 C13 111.9(2) . . ? F6 C14 C13 113.4(2) . . ? F4 C14 C13 112.2(2) . . ? F8 C15 F9 107.4(3) . . ? F8 C15 F7 106.2(2) . . ? F9 C15 F7 105.7(2) . . ? F8 C15 C16 111.0(2) . . ? F9 C15 C16 113.2(2) . . ? F7 C15 C16 113.0(2) . . ? N3 C16 C17 110.4(2) . . ? N3 C16 C15 124.2(2) . . ? C17 C16 C15 125.4(3) . . ? C16 C17 C18 102.9(2) . . ? C16 C17 H17 128.6 . . ? C18 C17 H17 128.6 . . ? N4 C18 C17 111.8(2) . . ? N4 C18 C19 120.8(2) . . ? C17 C18 C19 127.4(2) . . ? F12 C19 F10 106.9(2) . . ? F12 C19 F11 107.1(2) . . ? F10 C19 F11 105.6(2) . . ? F12 C19 C18 112.7(2) . . ? F10 C19 C18 111.8(2) . . ? F11 C19 C18 112.2(2) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Co1 P1 C3 -177.24(14) . . . . ? N1 Co1 P1 C3 5.15(14) . . . . ? P3 Co1 P1 C3 -85.35(13) . . . . ? P2 Co1 P1 C3 92.48(13) . . . . ? N3 Co1 P1 C2 62.63(14) . . . . ? N1 Co1 P1 C2 -114.98(14) . . . . ? P3 Co1 P1 C2 154.52(12) . . . . ? P2 Co1 P1 C2 -27.65(13) . . . . ? N3 Co1 P1 C1 -55.65(14) . . . . ? N1 Co1 P1 C1 126.74(14) . . . . ? P3 Co1 P1 C1 36.23(12) . . . . ? P2 Co1 P1 C1 -145.94(12) . . . . ? N3 Co1 P2 C6 -144.14(12) . . . . ? N1 Co1 P2 C6 50.89(12) . . . . ? P1 Co1 P2 C6 -52.03(11) . . . . ? N3 Co1 P2 C4 -20.19(12) . . . . ? N1 Co1 P2 C4 174.84(12) . . . . ? P1 Co1 P2 C4 71.91(11) . . . . ? N3 Co1 P2 C5 99.51(13) . . . . ? N1 Co1 P2 C5 -65.46(13) . . . . ? P1 Co1 P2 C5 -168.39(12) . . . . ? N3 Co1 P3 C9 15.93(14) . . . . ? N1 Co1 P3 C9 -179.37(13) . . . . ? P1 Co1 P3 C9 -76.23(12) . . . . ? N3 Co1 P3 C8 -104.68(13) . . . . ? N1 Co1 P3 C8 60.02(13) . . . . ? P1 Co1 P3 C8 163.16(12) . . . . ? N3 Co1 P3 C7 139.90(13) . . . . ? N1 Co1 P3 C7 -55.40(13) . . . . ? P1 Co1 P3 C7 47.74(12) . . . . ? N3 Co1 N1 N2 -160.4(3) . . . . ? P3 Co1 N1 N2 102.79(18) . . . . ? P2 Co1 N1 N2 -82.88(18) . . . . ? P1 Co1 N1 N2 10.5(2) . . . . ? N3 Co1 N1 C11 9.1(5) . . . . ? P3 Co1 N1 C11 -87.7(2) . . . . ? P2 Co1 N1 C11 86.7(2) . . . . ? P1 Co1 N1 C11 -179.9(2) . . . . ? C11 N1 N2 C13 -0.6(3) . . . . ? Co1 N1 N2 C13 171.33(17) . . . . ? N1 Co1 N3 N4 164.4(3) . . . . ? P3 Co1 N3 N4 -99.11(17) . . . . ? P2 Co1 N3 N4 87.29(17) . . . . ? P1 Co1 N3 N4 -6.84(17) . . . . ? N1 Co1 N3 C16 -10.5(5) . . . . ? P3 Co1 N3 C16 86.0(3) . . . . ? P2 Co1 N3 C16 -87.6(3) . . . . ? P1 Co1 N3 C16 178.2(3) . . . . ? C16 N3 N4 C18 0.1(3) . . . . ? Co1 N3 N4 C18 -176.22(17) . . . . ? N2 N1 C11 C12 0.7(3) . . . . ? Co1 N1 C11 C12 -169.52(19) . . . . ? N2 N1 C11 C10 178.1(2) . . . . ? Co1 N1 C11 C10 7.9(4) . . . . ? F1 C10 C11 N1 -8.4(4) . . . . ? F3 C10 C11 N1 113.3(3) . . . . ? F2 C10 C11 N1 -128.7(3) . . . . ? F1 C10 C11 C12 168.6(3) . . . . ? F3 C10 C11 C12 -69.8(4) . . . . ? F2 C10 C11 C12 48.3(4) . . . . ? N1 C11 C12 C13 -0.6(3) . . . . ? C10 C11 C12 C13 -177.9(3) . . . . ? N1 N2 C13 C12 0.2(3) . . . . ? N1 N2 C13 C14 -172.6(2) . . . . ? C11 C12 C13 N2 0.2(3) . . . . ? C11 C12 C13 C14 172.3(3) . . . . ? N2 C13 C14 F5 -169.0(2) . . . . ? C12 C13 C14 F5 19.4(4) . . . . ? N2 C13 C14 F6 -47.2(3) . . . . ? C12 C13 C14 F6 141.2(3) . . . . ? N2 C13 C14 F4 72.3(3) . . . . ? C12 C13 C14 F4 -99.2(3) . . . . ? N4 N3 C16 C17 0.1(3) . . . . ? Co1 N3 C16 C17 175.3(2) . . . . ? N4 N3 C16 C15 -178.8(2) . . . . ? Co1 N3 C16 C15 -3.6(4) . . . . ? F8 C15 C16 N3 -172.9(3) . . . . ? F9 C15 C16 N3 66.3(4) . . . . ? F7 C15 C16 N3 -53.7(4) . . . . ? F8 C15 C16 C17 8.5(4) . . . . ? F9 C15 C16 C17 -112.3(3) . . . . ? F7 C15 C16 C17 127.6(3) . . . . ? N3 C16 C17 C18 -0.2(3) . . . . ? C15 C16 C17 C18 178.6(3) . . . . ? N3 N4 C18 C17 -0.2(3) . . . . ? N3 N4 C18 C19 -179.6(2) . . . . ? C16 C17 C18 N4 0.2(3) . . . . ? C16 C17 C18 C19 179.6(3) . . . . ? N4 C18 C19 F12 -8.3(4) . . . . ? C17 C18 C19 F12 172.5(3) . . . . ? N4 C18 C19 F10 -128.8(3) . . . . ? C17 C18 C19 F10 52.0(4) . . . . ? N4 C18 C19 F11 112.7(3) . . . . ? C17 C18 C19 F11 -66.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.431 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.073 data_Co2P5Pz3H2 _database_code_depnum_ccdc_archive 'CCDC 887457' #TrackingRef '3 [CoP4H2][CoPz3P] (3).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [dihydrido-tetrakis(trimethylphosphine)-cobalt(iii)][tris-bis-3,5-(trifluoromethyl)pyrazolate-trimethylphosphine-cobalt(ii)] ; _chemical_name_common ; (dihydrido-tetrakis(trimethylphosphine)-cobalt(iii))(tris-bis- 3,5-(trifluorometh ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co F18 N6 P, C12 H38 Co P4' _chemical_formula_sum 'C30 H50 Co2 F18 N6 P5' _chemical_formula_weight 1109.47 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 '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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 10.0753(2) _cell_length_b 68.7275(12) _cell_length_c 13.7230(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.308(6) _cell_angle_gamma 90.00 _cell_volume 9502.4(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 54652 _cell_measurement_theta_min 6.58 _cell_measurement_theta_max 72.32 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4504 _exptl_absorpt_coefficient_mu 7.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.255 _exptl_absorpt_correction_T_max 0.410 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-Axis Spider ' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 152403 _diffrn_reflns_av_R_equivalents 0.1127 _diffrn_reflns_av_sigmaI/netI 0.1156 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -83 _diffrn_reflns_limit_k_max 78 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 6.58 _diffrn_reflns_theta_max 69.99 _reflns_number_total 17894 _reflns_number_gt 10569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+2.3266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17894 _refine_ls_number_parameters 1201 _refine_ls_number_restraints 204 _refine_ls_R_factor_all 0.1697 _refine_ls_R_factor_gt 0.1018 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.294 _refine_ls_restrained_S_all 1.298 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.21584(8) 0.052137(13) 0.80285(6) 0.0396(3) Uani 1 1 d . . . Co2 Co 0.67108(8) 0.072363(13) 0.27807(6) 0.0397(3) Uani 1 1 d . . . Co3 Co 0.72441(9) 0.199904(14) 0.83504(7) 0.0458(3) Uani 1 1 d . . . Co4 Co 0.14375(8) 0.178888(13) 0.32834(7) 0.0424(3) Uani 1 1 d . . . P1 P 0.22058(15) 0.08044(2) 0.87433(11) 0.0450(4) Uani 1 1 d . . . P2 P 0.29360(14) 0.03286(2) 0.91857(11) 0.0431(4) Uani 1 1 d . . . P3 P 0.39604(14) 0.05280(2) 0.71228(11) 0.0426(4) Uani 1 1 d . . . P4 P 0.09046(14) 0.03243(2) 0.71841(11) 0.0429(4) Uani 1 1 d . . . P5 P 0.50319(14) 0.09624(2) 0.28187(11) 0.0398(4) Uani 1 1 d . . . P6 P 0.72275(15) 0.19663(2) 0.99242(11) 0.0485(5) Uani 1 1 d . . . P7 P 0.88984(15) 0.22044(2) 0.81600(12) 0.0461(4) Uani 1 1 d . . . P8 P 0.82585(17) 0.17281(2) 0.79141(12) 0.0566(5) Uani 1 1 d . . . P9 P 0.60245(17) 0.20515(3) 0.70639(14) 0.0662(6) Uani 1 1 d . . . P10 P -0.00702(15) 0.15267(2) 0.32161(12) 0.0468(5) Uani 1 1 d . . . F1 F 0.8950(4) 0.03480(5) 0.0958(3) 0.0866(13) Uani 1 1 d . . . F2 F 0.6976(3) 0.03288(5) 0.1446(3) 0.0677(11) Uani 1 1 d . . . F3 F 0.7395(4) 0.03058(5) -0.0067(3) 0.0698(11) Uani 1 1 d . . . F4 F 0.7629(9) 0.10661(14) -0.1394(5) 0.103(3) Uani 0.76 1 d PDU A 1 F4B F 0.699(2) 0.1247(4) -0.003(2) 0.069(8) Uani 0.24 1 d PDU A 2 F5 F 0.6548(7) 0.12135(13) -0.0289(7) 0.073(3) Uani 0.76 1 d PDU A 1 F5B F 0.8718(14) 0.1161(4) -0.0748(17) 0.083(8) Uani 0.24 1 d PDU A 2 F6 F 0.8633(7) 0.11966(13) -0.0207(5) 0.094(3) Uani 0.76 1 d PDU A 1 F6B F 0.687(2) 0.1072(4) -0.1286(13) 0.085(8) Uani 0.24 1 d PDU A 2 F7 F 0.8330(3) 0.03450(4) 0.3988(2) 0.0512(9) Uani 1 1 d . . . F8 F 0.7254(3) 0.04675(5) 0.5186(2) 0.0513(9) Uani 1 1 d . . . F9 F 0.7276(3) 0.01573(5) 0.4978(2) 0.0585(10) Uani 1 1 d . . . F10 F 0.2012(3) 0.01649(5) 0.3533(2) 0.0704(11) Uani 1 1 d . . . F11 F 0.2997(3) 0.00485(5) 0.2282(3) 0.0692(11) Uani 1 1 d . . . F12 F 0.2164(3) 0.03340(5) 0.2224(2) 0.0531(9) Uani 1 1 d . . . F13 F 0.9690(3) 0.05693(5) 0.2683(2) 0.0579(10) Uani 1 1 d . . . F14 F 1.1298(4) 0.06271(6) 0.3660(3) 0.0962(14) Uani 1 1 d . . . F15 F 1.0782(4) 0.08309(6) 0.2574(3) 0.1102(18) Uani 1 1 d . . . F16 F 0.9113(3) 0.11525(5) 0.6404(2) 0.0692(11) Uani 1 1 d . . . F17 F 0.7896(5) 0.09151(7) 0.6753(3) 0.125(2) Uani 1 1 d . . . F18 F 0.7087(4) 0.11610(7) 0.6003(3) 0.121(2) Uani 1 1 d . . . F19 F 0.4915(3) 0.16768(5) 0.2542(3) 0.0726(11) Uani 1 1 d . . . F20 F 0.4651(3) 0.19412(5) 0.3294(2) 0.0628(10) Uani 1 1 d . . . F21 F 0.6260(3) 0.17532(5) 0.3682(3) 0.0791(12) Uani 1 1 d . . . F22 F 0.2426(4) 0.11910(6) 0.5908(3) 0.0863(13) Uani 1 1 d . . . F23 F 0.4204(4) 0.12848(6) 0.6559(3) 0.1102(17) Uani 1 1 d . . . F24 F 0.2398(4) 0.14297(5) 0.6863(3) 0.0931(14) Uani 1 1 d . . . F25 F 0.2071(3) 0.23273(5) 0.5595(2) 0.0552(10) Uani 1 1 d . . . F26 F 0.1790(3) 0.20191(5) 0.5766(2) 0.0593(10) Uani 1 1 d . . . F27 F 0.3075(3) 0.21266(4) 0.4649(2) 0.0532(9) Uani 1 1 d . . . F28 F -0.3031(11) 0.23902(17) 0.4074(7) 0.102(4) Uani 0.55 1 d PDU B 1 F29 F -0.3109(13) 0.21845(19) 0.2937(11) 0.086(5) Uani 0.55 1 d PDU B 1 F30 F -0.2245(14) 0.24596(16) 0.2664(9) 0.101(5) Uani 0.55 1 d PDU B 1 F29B F -0.2527(14) 0.24947(17) 0.3720(10) 0.104(5) Uani 0.45 1 d PDU B 2 F30B F -0.3380(15) 0.2219(2) 0.3306(14) 0.080(5) Uani 0.45 1 d PDU B 2 F28B F -0.2116(17) 0.23705(19) 0.2348(8) 0.079(5) Uani 0.45 1 d PDU B 2 F31 F 0.3135(4) 0.22089(5) 0.2210(3) 0.0956(15) Uani 1 1 d . . . F32 F 0.1190(4) 0.22269(5) 0.1693(3) 0.0896(14) Uani 1 1 d . . . F33 F 0.2778(4) 0.22664(5) 0.0732(3) 0.0771(12) Uani 1 1 d . . . F34 F 0.3876(4) 0.13916(5) 0.0253(3) 0.0814(12) Uani 1 1 d . . . F35 F 0.3058(4) 0.15468(5) -0.0957(3) 0.0901(13) Uani 1 1 d . . . F36 F 0.1822(3) 0.13670(5) -0.0082(3) 0.0724(11) Uani 1 1 d . . . N1 N 0.7224(4) 0.07323(7) 0.1375(3) 0.0377(12) Uani 1 1 d . . . N2 N 0.7177(4) 0.09183(7) 0.1053(3) 0.0431(13) Uani 1 1 d . . . N3 N 0.5779(4) 0.04859(6) 0.3257(3) 0.0379(12) Uani 1 1 d . . . N4 N 0.4593(5) 0.04584(7) 0.2799(3) 0.0459(13) Uani 1 1 d . . . N5 N 0.8049(4) 0.08201(6) 0.3719(3) 0.0393(12) Uani 1 1 d . . . N6 N 0.7479(4) 0.09143(7) 0.4483(4) 0.0452(13) Uani 1 1 d . . . N7 N 0.2823(4) 0.16717(7) 0.4133(3) 0.0409(13) Uani 1 1 d . . . N8 N 0.2306(5) 0.15620(7) 0.4864(3) 0.0449(13) Uani 1 1 d . . . N9 N 0.0497(5) 0.20218(6) 0.3788(3) 0.0414(13) Uani 1 1 d . . . N10 N -0.0653(5) 0.20613(7) 0.3317(3) 0.0470(13) Uani 1 1 d . . . N11 N 0.1995(4) 0.18136(8) 0.1895(3) 0.0401(13) Uani 1 1 d . . . N12 N 0.2090(4) 0.16345(7) 0.1477(4) 0.0452(13) Uani 1 1 d . . . C1 C 0.3776(5) 0.09342(8) 0.8946(4) 0.0543(18) Uani 1 1 d . . . H1A H 0.3607 0.1053 0.9317 0.081 Uiso 1 1 calc R . . H1B H 0.4169 0.0968 0.8316 0.081 Uiso 1 1 calc R . . H1C H 0.4389 0.0851 0.9312 0.081 Uiso 1 1 calc R . . C2 C 0.1261(6) 0.09889(8) 0.8100(4) 0.0591(19) Uani 1 1 d . . . H2A H 0.0344 0.0944 0.8013 0.089 Uiso 1 1 calc R . . H2B H 0.1660 0.1012 0.7460 0.089 Uiso 1 1 calc R . . H2C H 0.1269 0.1110 0.8477 0.089 Uiso 1 1 calc R . . C3 C 0.1450(5) 0.08193(8) 0.9943(4) 0.0477(17) Uani 1 1 d . . . H3A H 0.1497 0.0954 1.0180 0.072 Uiso 1 1 calc R . . H3B H 0.1926 0.0734 1.0396 0.072 Uiso 1 1 calc R . . H3C H 0.0519 0.0779 0.9899 0.072 Uiso 1 1 calc R . . C4 C 0.4004(5) 0.04329(8) 1.0132(4) 0.0513(17) Uani 1 1 d . . . H4A H 0.3504 0.0530 1.0501 0.077 Uiso 1 1 calc R . . H4B H 0.4774 0.0495 0.9829 0.077 Uiso 1 1 calc R . . H4C H 0.4305 0.0330 1.0573 0.077 Uiso 1 1 calc R . . C5 C 0.1669(5) 0.02084(8) 0.9914(4) 0.0552(18) Uani 1 1 d . . . H5A H 0.2095 0.0122 1.0388 0.083 Uiso 1 1 calc R . . H5B H 0.1085 0.0132 0.9486 0.083 Uiso 1 1 calc R . . H5C H 0.1144 0.0307 1.0258 0.083 Uiso 1 1 calc R . . C6 C 0.3967(5) 0.01192(7) 0.8847(4) 0.0478(17) Uani 1 1 d . . . H6A H 0.4084 0.0034 0.9414 0.072 Uiso 1 1 calc R . . H6B H 0.4835 0.0165 0.8626 0.072 Uiso 1 1 calc R . . H6C H 0.3531 0.0047 0.8321 0.072 Uiso 1 1 calc R . . C7 C 0.5585(5) 0.05716(8) 0.7684(4) 0.0489(17) Uani 1 1 d . . . H7A H 0.6263 0.0578 0.7176 0.073 Uiso 1 1 calc R . . H7B H 0.5795 0.0465 0.8135 0.073 Uiso 1 1 calc R . . H7C H 0.5567 0.0695 0.8041 0.073 Uiso 1 1 calc R . . C8 C 0.3955(6) 0.07082(8) 0.6160(4) 0.0610(19) Uani 1 1 d . . . H8A H 0.4791 0.0701 0.5801 0.091 Uiso 1 1 calc R . . H8B H 0.3858 0.0838 0.6444 0.091 Uiso 1 1 calc R . . H8C H 0.3212 0.0683 0.5714 0.091 Uiso 1 1 calc R . . C9 C 0.4364(5) 0.03074(7) 0.6438(4) 0.0499(17) Uani 1 1 d . . . H9A H 0.3644 0.0278 0.5977 0.075 Uiso 1 1 calc R . . H9B H 0.4472 0.0198 0.6891 0.075 Uiso 1 1 calc R . . H9C H 0.5191 0.0327 0.6079 0.075 Uiso 1 1 calc R . . C10 C 0.0795(5) 0.03675(8) 0.5872(4) 0.0599(19) Uani 1 1 d . . . H10A H 0.0239 0.0267 0.5571 0.090 Uiso 1 1 calc R . . H10B H 0.1686 0.0363 0.5590 0.090 Uiso 1 1 calc R . . H10C H 0.0400 0.0496 0.5753 0.090 Uiso 1 1 calc R . . C11 C -0.0845(5) 0.03435(8) 0.7503(4) 0.0568(18) Uani 1 1 d . . . H11A H -0.1140 0.0478 0.7422 0.085 Uiso 1 1 calc R . . H11B H -0.0966 0.0304 0.8183 0.085 Uiso 1 1 calc R . . H11C H -0.1371 0.0259 0.7076 0.085 Uiso 1 1 calc R . . C12 C 0.1139(5) 0.00601(7) 0.7201(4) 0.0554(18) Uani 1 1 d . . . H12A H 0.1036 0.0012 0.7868 0.083 Uiso 1 1 calc R . . H12B H 0.2031 0.0029 0.6967 0.083 Uiso 1 1 calc R . . H12C H 0.0476 -0.0001 0.6776 0.083 Uiso 1 1 calc R . . C13 C 0.4023(5) 0.09620(8) 0.3901(4) 0.0493(17) Uani 1 1 d . . . H13A H 0.4590 0.0982 0.4474 0.074 Uiso 1 1 calc R . . H13B H 0.3567 0.0837 0.3957 0.074 Uiso 1 1 calc R . . H13C H 0.3366 0.1067 0.3858 0.074 Uiso 1 1 calc R . . C14 C 0.5572(5) 0.12131(7) 0.2721(4) 0.0512(17) Uani 1 1 d . . . H14A H 0.4796 0.1299 0.2715 0.077 Uiso 1 1 calc R . . H14B H 0.6072 0.1230 0.2117 0.077 Uiso 1 1 calc R . . H14C H 0.6141 0.1246 0.3280 0.077 Uiso 1 1 calc R . . C15 C 0.3846(5) 0.09385(8) 0.1827(4) 0.0476(17) Uani 1 1 d . . . H15A H 0.3191 0.1044 0.1866 0.071 Uiso 1 1 calc R . . H15B H 0.3393 0.0813 0.1876 0.071 Uiso 1 1 calc R . . H15C H 0.4312 0.0946 0.1204 0.071 Uiso 1 1 calc R . . C16 C 0.7711(6) 0.04030(10) 0.0740(5) 0.0479(17) Uani 1 1 d . . . C17 C 0.7559(5) 0.06133(9) 0.0629(4) 0.0353(15) Uani 1 1 d . . . C18 C 0.7742(5) 0.07232(9) -0.0195(4) 0.0406(16) Uani 1 1 d . . . H18 H 0.7979 0.0680 -0.0828 0.049 Uiso 1 1 calc R . . C19 C 0.7499(5) 0.09115(9) 0.0112(4) 0.0369(15) Uani 1 1 d . A . C20 C 0.7553(7) 0.10927(11) -0.0443(5) 0.059(2) Uani 1 1 d DU . . C21 C 0.7199(6) 0.03283(10) 0.4490(5) 0.0456(17) Uani 1 1 d . . . C22 C 0.5998(6) 0.03368(9) 0.3875(4) 0.0359(15) Uani 1 1 d . . . C23 C 0.4954(6) 0.02097(8) 0.3841(4) 0.0403(15) Uani 1 1 d . . . H23 H 0.4839 0.0093 0.4202 0.048 Uiso 1 1 calc R . . C24 C 0.4110(6) 0.02905(9) 0.3161(4) 0.0372(15) Uani 1 1 d . . . C25 C 0.2830(7) 0.02126(11) 0.2802(5) 0.0517(18) Uani 1 1 d . . . C26 C 1.0259(7) 0.07115(12) 0.3196(6) 0.059(2) Uani 1 1 d . . . C27 C 0.9362(6) 0.08023(8) 0.3910(5) 0.0404(16) Uani 1 1 d . . . C28 C 0.9661(6) 0.08845(8) 0.4782(5) 0.0488(17) Uani 1 1 d . . . H28 H 1.0506 0.0894 0.5089 0.059 Uiso 1 1 calc R . . C29 C 0.8447(6) 0.09520(8) 0.5125(4) 0.0409(16) Uani 1 1 d . . . C30 C 0.8122(8) 0.10439(13) 0.6057(6) 0.067(2) Uani 1 1 d . . . C31 C 0.6157(5) 0.21420(8) 1.0533(4) 0.065(2) Uani 1 1 d . . . H31A H 0.6082 0.2108 1.1223 0.097 Uiso 1 1 calc R . . H31B H 0.5275 0.2140 1.0229 0.097 Uiso 1 1 calc R . . H31C H 0.6540 0.2273 1.0472 0.097 Uiso 1 1 calc R . . C32 C 0.8744(5) 0.19904(9) 1.0657(4) 0.0616(19) Uani 1 1 d . . . H32A H 0.9143 0.2118 1.0541 0.092 Uiso 1 1 calc R . . H32B H 0.9374 0.1888 1.0473 0.092 Uiso 1 1 calc R . . H32C H 0.8526 0.1977 1.1349 0.092 Uiso 1 1 calc R . . C33 C 0.6541(5) 0.17372(8) 1.0370(4) 0.0590(19) Uani 1 1 d . . . H33A H 0.6490 0.1741 1.1083 0.089 Uiso 1 1 calc R . . H33B H 0.7114 0.1629 1.0170 0.089 Uiso 1 1 calc R . . H33C H 0.5649 0.1718 1.0097 0.089 Uiso 1 1 calc R . . C34 C 0.8713(6) 0.24295(8) 0.8827(4) 0.0592(19) Uani 1 1 d . . . H34A H 0.9449 0.2517 0.8669 0.089 Uiso 1 1 calc R . . H34B H 0.8719 0.2402 0.9528 0.089 Uiso 1 1 calc R . . H34C H 0.7870 0.2491 0.8645 0.089 Uiso 1 1 calc R . . C35 C 1.0581(5) 0.21268(8) 0.8516(4) 0.0625(19) Uani 1 1 d . . . H35A H 1.1198 0.2236 0.8439 0.094 Uiso 1 1 calc R . . H35B H 1.0861 0.2018 0.8101 0.094 Uiso 1 1 calc R . . H35C H 1.0580 0.2085 0.9198 0.094 Uiso 1 1 calc R . . C36 C 0.9253(6) 0.22952(8) 0.6943(4) 0.0579(18) Uani 1 1 d . . . H36A H 0.8474 0.2364 0.6688 0.087 Uiso 1 1 calc R . . H36B H 0.9465 0.2186 0.6513 0.087 Uiso 1 1 calc R . . H36C H 1.0011 0.2385 0.6973 0.087 Uiso 1 1 calc R . . C37 C 0.7143(6) 0.15250(8) 0.7669(5) 0.077(2) Uani 1 1 d . . . H37A H 0.6582 0.1556 0.7104 0.115 Uiso 1 1 calc R . . H37B H 0.6582 0.1502 0.8239 0.115 Uiso 1 1 calc R . . H37C H 0.7665 0.1408 0.7532 0.115 Uiso 1 1 calc R . . C38 C 0.9285(7) 0.17286(9) 0.6821(4) 0.082(2) Uani 1 1 d . . . H38A H 0.9624 0.1597 0.6703 0.123 Uiso 1 1 calc R . . H38B H 1.0031 0.1818 0.6912 0.123 Uiso 1 1 calc R . . H38C H 0.8749 0.1771 0.6261 0.123 Uiso 1 1 calc R . . C39 C 0.9437(5) 0.16163(8) 0.8759(4) 0.064(2) Uani 1 1 d . . . H39A H 0.8984 0.1584 0.9367 0.096 Uiso 1 1 calc R . . H39B H 1.0161 0.1708 0.8895 0.096 Uiso 1 1 calc R . . H39C H 0.9799 0.1498 0.8467 0.096 Uiso 1 1 calc R . . C40 C 0.4440(7) 0.19221(11) 0.7104(6) 0.119(3) Uani 1 1 d . . . H40A H 0.3878 0.1979 0.7609 0.178 Uiso 1 1 calc R . . H40B H 0.4600 0.1785 0.7255 0.178 Uiso 1 1 calc R . . H40C H 0.3994 0.1933 0.6470 0.178 Uiso 1 1 calc R . . C41 C 0.6556(8) 0.19860(10) 0.5822(4) 0.099(3) Uani 1 1 d . . . H41A H 0.5854 0.2020 0.5356 0.149 Uiso 1 1 calc R . . H41B H 0.6730 0.1846 0.5791 0.149 Uiso 1 1 calc R . . H41C H 0.7368 0.2057 0.5661 0.149 Uiso 1 1 calc R . . C42 C 0.5502(7) 0.22995(9) 0.6861(5) 0.094(3) Uani 1 1 d . . . H42A H 0.6278 0.2380 0.6718 0.142 Uiso 1 1 calc R . . H42B H 0.5061 0.2349 0.7446 0.142 Uiso 1 1 calc R . . H42C H 0.4882 0.2304 0.6309 0.142 Uiso 1 1 calc R . . C43 C -0.1247(5) 0.15380(9) 0.2214(4) 0.064(2) Uani 1 1 d . . . H43A H -0.1748 0.1416 0.2180 0.097 Uiso 1 1 calc R . . H43B H -0.0769 0.1558 0.1602 0.097 Uiso 1 1 calc R . . H43C H -0.1862 0.1647 0.2318 0.097 Uiso 1 1 calc R . . C44 C 0.0721(6) 0.12921(8) 0.3072(4) 0.067(2) Uani 1 1 d . . . H44A H 0.1314 0.1268 0.3628 0.101 Uiso 1 1 calc R . . H44B H 0.1236 0.1291 0.2469 0.101 Uiso 1 1 calc R . . H44C H 0.0042 0.1190 0.3042 0.101 Uiso 1 1 calc R . . C45 C -0.1102(5) 0.14923(9) 0.4288(4) 0.0601(19) Uani 1 1 d . . . H45A H -0.1695 0.1381 0.4184 0.090 Uiso 1 1 calc R . . H45B H -0.1633 0.1610 0.4399 0.090 Uiso 1 1 calc R . . H45C H -0.0536 0.1468 0.4857 0.090 Uiso 1 1 calc R . . C46 C 0.4984(6) 0.17560(11) 0.3432(5) 0.0504(18) Uani 1 1 d . . . C47 C 0.4168(6) 0.16553(8) 0.4165(4) 0.0385(15) Uani 1 1 d . . . C48 C 0.4537(6) 0.15354(8) 0.4906(4) 0.0436(16) Uani 1 1 d . . . H48 H 0.5408 0.1497 0.5091 0.052 Uiso 1 1 calc R . . C49 C 0.3346(6) 0.14820(8) 0.5329(4) 0.0402(16) Uani 1 1 d . . . C50 C 0.3123(8) 0.13496(12) 0.6168(5) 0.060(2) Uani 1 1 d . . . C51 C 0.1900(6) 0.21614(10) 0.5091(5) 0.0483(17) Uani 1 1 d . . . C52 C 0.0775(5) 0.21680(9) 0.4414(4) 0.0348(15) Uani 1 1 d . . . C53 C -0.0195(6) 0.23053(9) 0.4363(4) 0.0443(16) Uani 1 1 d . . . H53 H -0.0256 0.2423 0.4720 0.053 Uiso 1 1 calc R . . C54 C -0.1072(6) 0.22337(9) 0.3671(4) 0.0433(16) Uani 1 1 d . B . C55 C -0.2307(7) 0.23237(11) 0.3305(5) 0.067(2) Uani 1 1 d DU . . C56 C 0.2386(7) 0.21583(10) 0.1478(5) 0.0514(18) Uani 1 1 d . . . C57 C 0.2382(5) 0.19504(9) 0.1243(4) 0.0358(15) Uani 1 1 d . . . C58 C 0.2752(5) 0.18590(9) 0.0382(4) 0.0423(16) Uani 1 1 d . . . H58 H 0.3074 0.1916 -0.0201 0.051 Uiso 1 1 calc R . . C59 C 0.2538(5) 0.16637(10) 0.0580(5) 0.0405(16) Uani 1 1 d . . . C60 C 0.2821(7) 0.14961(11) -0.0047(6) 0.061(2) Uani 1 1 d . . . H1 H 0.097(4) 0.0531(6) 0.863(3) 0.050(14) Uiso 1 1 d . . . H4 H 0.644(5) 0.2180(7) 0.868(4) 0.085(18) Uiso 1 1 d . . . H3 H 0.610(5) 0.1881(7) 0.852(3) 0.080(18) Uiso 1 1 d . . . H2 H 0.149(5) 0.0645(7) 0.735(4) 0.078(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0369(6) 0.0426(7) 0.0393(6) -0.0017(5) 0.0029(5) -0.0004(5) Co2 0.0359(5) 0.0425(7) 0.0407(6) 0.0003(5) 0.0043(4) -0.0002(5) Co3 0.0441(6) 0.0453(7) 0.0481(7) 0.0014(5) -0.0012(5) -0.0020(5) Co4 0.0379(6) 0.0407(7) 0.0487(7) 0.0010(5) 0.0046(5) 0.0019(5) P1 0.0422(10) 0.0459(12) 0.0469(11) -0.0066(9) 0.0016(8) 0.0014(8) P2 0.0416(9) 0.0478(12) 0.0399(10) 0.0016(8) 0.0016(8) -0.0036(8) P3 0.0420(9) 0.0448(12) 0.0410(10) 0.0003(8) 0.0040(8) 0.0022(8) P4 0.0397(9) 0.0434(12) 0.0456(11) -0.0037(8) -0.0010(8) -0.0006(8) P5 0.0352(9) 0.0457(12) 0.0387(10) -0.0023(8) 0.0040(7) -0.0008(8) P6 0.0425(10) 0.0563(13) 0.0469(11) 0.0005(9) 0.0046(8) -0.0067(9) P7 0.0475(10) 0.0416(12) 0.0494(11) 0.0004(9) 0.0075(8) -0.0021(8) P8 0.0723(13) 0.0446(13) 0.0530(12) 0.0018(9) 0.0010(10) 0.0011(10) P9 0.0648(13) 0.0599(14) 0.0737(15) 0.0156(11) -0.0236(11) -0.0075(11) P10 0.0389(9) 0.0487(12) 0.0530(11) 0.0049(9) 0.0044(8) 0.0004(8) F1 0.053(2) 0.051(3) 0.155(4) -0.006(2) -0.011(3) 0.012(2) F2 0.088(3) 0.041(2) 0.074(3) 0.007(2) 0.034(2) 0.006(2) F3 0.111(3) 0.039(2) 0.059(3) -0.014(2) 0.001(2) 0.000(2) F4 0.190(9) 0.065(5) 0.053(4) 0.019(4) 0.050(5) 0.028(7) F4B 0.134(18) 0.050(13) 0.022(11) 0.013(8) 0.038(13) 0.031(14) F5 0.072(4) 0.055(5) 0.091(8) 0.023(4) 0.023(4) 0.015(4) F5B 0.051(11) 0.100(16) 0.099(17) 0.060(14) 0.049(12) 0.012(10) F6 0.091(6) 0.074(5) 0.116(7) 0.038(5) 0.008(4) -0.028(4) F6B 0.113(16) 0.072(14) 0.070(15) 0.018(12) 0.002(12) -0.034(14) F7 0.041(2) 0.058(2) 0.054(2) -0.0001(18) 0.0078(17) 0.0029(17) F8 0.049(2) 0.059(3) 0.045(2) -0.0055(19) -0.0036(17) -0.0007(18) F9 0.056(2) 0.057(3) 0.062(2) 0.018(2) -0.0127(18) -0.0005(19) F10 0.048(2) 0.103(3) 0.061(3) 0.015(2) 0.0069(19) -0.025(2) F11 0.059(2) 0.053(3) 0.096(3) -0.023(2) -0.012(2) 0.000(2) F12 0.048(2) 0.056(3) 0.055(2) -0.0011(19) -0.0013(18) -0.0020(19) F13 0.043(2) 0.068(3) 0.063(3) -0.013(2) 0.0112(18) -0.0043(19) F14 0.053(2) 0.122(4) 0.113(4) -0.049(3) -0.014(2) 0.033(2) F15 0.137(4) 0.056(3) 0.138(4) -0.015(3) 0.102(3) -0.023(3) F16 0.070(3) 0.073(3) 0.064(3) -0.017(2) -0.014(2) 0.003(2) F17 0.195(5) 0.124(4) 0.057(3) -0.017(3) 0.041(3) -0.082(4) F18 0.056(3) 0.212(6) 0.096(3) -0.095(4) -0.015(2) 0.043(3) F19 0.088(3) 0.074(3) 0.056(3) -0.006(2) 0.025(2) -0.008(2) F20 0.056(2) 0.049(3) 0.083(3) 0.012(2) 0.0229(19) 0.003(2) F21 0.030(2) 0.115(3) 0.093(3) 0.039(2) 0.005(2) 0.004(2) F22 0.121(4) 0.073(3) 0.065(3) 0.016(2) 0.006(2) -0.029(3) F23 0.065(3) 0.154(4) 0.112(4) 0.084(3) -0.009(3) 0.005(3) F24 0.143(4) 0.075(3) 0.062(3) 0.008(2) 0.038(3) 0.024(3) F25 0.048(2) 0.064(3) 0.054(2) -0.015(2) -0.0069(17) -0.0016(19) F26 0.062(2) 0.060(3) 0.056(2) 0.014(2) -0.0055(19) 0.0010(19) F27 0.041(2) 0.060(3) 0.058(2) -0.0070(19) 0.0035(17) 0.0045(18) F28 0.081(7) 0.128(11) 0.097(8) 0.014(7) 0.002(6) 0.066(7) F29 0.038(7) 0.092(8) 0.128(11) -0.004(7) -0.012(6) 0.021(6) F30 0.053(5) 0.073(10) 0.176(12) 0.080(9) 0.008(8) 0.019(7) F29B 0.114(11) 0.079(10) 0.117(12) -0.047(9) -0.060(9) 0.066(8) F30B 0.036(7) 0.066(10) 0.138(14) 0.025(8) 0.012(7) -0.001(7) F28B 0.068(8) 0.055(9) 0.113(9) 0.020(7) -0.030(7) 0.023(8) F31 0.136(4) 0.050(3) 0.100(3) -0.024(2) -0.064(3) 0.002(2) F32 0.059(3) 0.044(3) 0.166(4) -0.018(2) 0.033(3) 0.002(2) F33 0.115(3) 0.043(3) 0.073(3) 0.007(2) 0.027(2) -0.002(2) F34 0.064(3) 0.073(3) 0.107(3) -0.038(2) -0.011(2) 0.021(2) F35 0.132(4) 0.072(3) 0.066(3) -0.022(2) 0.031(3) -0.003(3) F36 0.060(2) 0.061(3) 0.096(3) -0.030(2) 0.005(2) -0.011(2) N1 0.037(3) 0.038(4) 0.038(3) 0.004(3) 0.008(2) 0.001(3) N2 0.053(3) 0.037(4) 0.040(3) 0.003(3) 0.014(3) -0.004(3) N3 0.039(3) 0.033(3) 0.042(3) 0.002(3) 0.003(2) 0.001(3) N4 0.039(3) 0.050(4) 0.048(3) 0.000(3) -0.003(3) -0.001(3) N5 0.037(3) 0.037(3) 0.044(3) -0.002(3) -0.004(3) 0.000(2) N6 0.039(3) 0.052(4) 0.045(3) -0.006(3) 0.002(3) 0.000(3) N7 0.033(3) 0.046(4) 0.044(3) 0.007(3) -0.002(2) 0.004(3) N8 0.046(3) 0.045(4) 0.044(3) 0.002(3) 0.003(3) 0.001(3) N9 0.042(3) 0.032(3) 0.050(3) -0.005(3) 0.000(3) 0.001(3) N10 0.037(3) 0.052(4) 0.052(4) 0.000(3) -0.005(3) 0.002(3) N11 0.038(3) 0.037(4) 0.045(3) -0.001(3) 0.004(2) -0.003(3) N12 0.046(3) 0.034(4) 0.055(4) -0.007(3) 0.004(3) -0.001(3) C1 0.043(4) 0.050(5) 0.070(5) -0.014(4) -0.006(3) -0.010(3) C2 0.072(5) 0.040(4) 0.066(5) -0.010(3) 0.001(4) 0.013(4) C3 0.038(4) 0.060(5) 0.045(4) -0.016(3) 0.002(3) 0.004(3) C4 0.051(4) 0.067(5) 0.036(4) 0.000(3) -0.012(3) 0.000(3) C5 0.050(4) 0.073(5) 0.043(4) 0.017(3) 0.009(3) -0.008(3) C6 0.049(4) 0.041(4) 0.054(4) 0.008(3) -0.003(3) 0.002(3) C7 0.032(3) 0.062(5) 0.053(4) 0.001(3) 0.005(3) -0.007(3) C8 0.070(5) 0.063(5) 0.049(4) 0.013(4) 0.006(4) 0.001(4) C9 0.044(4) 0.055(5) 0.051(4) -0.017(3) 0.018(3) -0.002(3) C10 0.061(4) 0.071(5) 0.047(4) -0.007(4) -0.015(3) -0.008(4) C11 0.031(3) 0.063(5) 0.077(5) -0.012(4) 0.004(3) -0.004(3) C12 0.058(4) 0.042(5) 0.065(5) -0.002(3) -0.006(4) 0.000(3) C13 0.041(4) 0.062(5) 0.046(4) 0.002(3) 0.011(3) 0.004(3) C14 0.054(4) 0.038(4) 0.062(4) -0.010(3) 0.012(3) 0.002(3) C15 0.048(4) 0.058(5) 0.037(4) -0.001(3) 0.001(3) 0.004(3) C16 0.045(4) 0.046(5) 0.053(5) -0.010(4) 0.007(4) -0.004(4) C17 0.029(3) 0.038(5) 0.039(4) 0.000(3) 0.003(3) 0.000(3) C18 0.031(3) 0.046(5) 0.045(4) -0.008(4) 0.003(3) 0.002(3) C19 0.034(3) 0.035(5) 0.041(4) 0.009(3) 0.005(3) -0.002(3) C20 0.066(5) 0.053(6) 0.058(5) -0.007(4) 0.012(4) 0.002(5) C21 0.060(5) 0.037(5) 0.040(5) 0.000(4) 0.015(4) 0.005(4) C22 0.035(4) 0.040(4) 0.033(4) -0.006(3) 0.001(3) 0.008(3) C23 0.057(4) 0.030(4) 0.034(4) 0.004(3) 0.011(3) -0.002(3) C24 0.040(4) 0.036(4) 0.036(4) -0.008(3) 0.004(3) -0.001(3) C25 0.052(5) 0.045(5) 0.058(5) -0.005(4) 0.004(4) 0.007(4) C26 0.041(4) 0.060(6) 0.077(6) -0.009(5) 0.001(4) 0.007(4) C27 0.038(4) 0.034(4) 0.049(4) 0.003(3) 0.001(3) 0.001(3) C28 0.036(4) 0.045(5) 0.065(5) 0.005(4) -0.012(3) -0.008(3) C29 0.042(4) 0.039(4) 0.042(4) 0.001(3) -0.002(3) 0.002(3) C30 0.055(5) 0.097(7) 0.049(5) -0.028(5) -0.001(4) -0.020(5) C31 0.062(4) 0.071(5) 0.061(5) -0.013(4) 0.029(4) 0.002(4) C32 0.055(4) 0.087(5) 0.043(4) 0.008(4) -0.015(3) -0.021(4) C33 0.052(4) 0.069(5) 0.056(4) 0.021(4) 0.001(3) -0.010(4) C34 0.071(5) 0.046(5) 0.061(5) -0.012(4) 0.002(4) -0.011(4) C35 0.038(4) 0.069(5) 0.081(5) 0.011(4) 0.003(3) -0.010(3) C36 0.061(4) 0.053(5) 0.060(5) 0.009(4) 0.017(3) 0.005(3) C37 0.105(6) 0.038(5) 0.087(6) -0.009(4) -0.022(5) -0.008(4) C38 0.118(6) 0.060(5) 0.068(5) 0.000(4) 0.041(5) 0.015(4) C39 0.061(4) 0.051(5) 0.081(5) 0.014(4) 0.003(4) 0.012(4) C40 0.085(6) 0.130(8) 0.140(8) 0.056(6) -0.056(5) -0.046(5) C41 0.155(8) 0.086(6) 0.057(5) 0.008(4) -0.038(5) -0.014(5) C42 0.106(6) 0.072(6) 0.106(6) 0.017(5) -0.037(5) 0.023(5) C43 0.044(4) 0.089(6) 0.060(5) 0.014(4) -0.005(3) -0.018(4) C44 0.083(5) 0.031(4) 0.089(5) 0.003(4) 0.021(4) 0.002(4) C45 0.048(4) 0.083(5) 0.050(4) 0.015(4) 0.013(3) -0.010(4) C46 0.042(4) 0.054(6) 0.055(5) 0.004(4) 0.012(4) 0.002(4) C47 0.038(4) 0.038(4) 0.040(4) -0.007(3) 0.001(3) 0.003(3) C48 0.038(4) 0.045(4) 0.048(4) -0.010(3) -0.004(3) 0.008(3) C49 0.043(4) 0.035(4) 0.042(4) 0.000(3) -0.002(3) -0.001(3) C50 0.062(5) 0.063(6) 0.056(6) 0.015(5) 0.003(4) -0.004(5) C51 0.049(4) 0.050(5) 0.046(5) -0.002(4) 0.006(4) -0.002(4) C52 0.034(4) 0.037(4) 0.033(4) 0.003(3) 0.002(3) 0.004(3) C53 0.045(4) 0.042(4) 0.045(4) -0.008(3) 0.000(3) 0.001(3) C54 0.039(4) 0.038(5) 0.053(5) 0.001(3) -0.001(3) 0.009(3) C55 0.064(5) 0.067(7) 0.069(6) -0.016(5) -0.013(5) 0.013(5) C56 0.053(5) 0.035(5) 0.066(6) 0.001(4) 0.016(4) -0.003(4) C57 0.028(3) 0.030(4) 0.049(4) 0.000(3) -0.004(3) 0.000(3) C58 0.035(3) 0.044(5) 0.048(4) -0.001(3) 0.005(3) -0.002(3) C59 0.035(3) 0.040(5) 0.046(4) -0.012(4) 0.006(3) -0.001(3) C60 0.055(5) 0.061(6) 0.066(6) -0.011(5) 0.007(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co1 P1 2.1787(18) . ? Co1 P4 2.1810(18) . ? Co1 P3 2.2063(17) . ? Co1 P2 2.2087(18) . ? Co1 H1 1.46(4) . ? Co1 H2 1.43(5) . ? Co2 N5 1.975(4) . ? Co2 N3 1.996(4) . ? Co2 N1 2.001(4) . ? Co2 P5 2.3574(17) . ? Co3 P6 2.1716(18) . ? Co3 P9 2.176(2) . ? Co3 P7 2.2007(18) . ? Co3 P8 2.208(2) . ? Co3 H4 1.55(5) . ? Co3 H3 1.43(5) . ? Co4 N7 1.985(4) . ? Co4 N9 1.987(5) . ? Co4 N11 1.997(5) . ? Co4 P10 2.3585(18) . ? P1 C2 1.813(5) . ? P1 C3 1.821(5) . ? P1 C1 1.836(5) . ? P2 C5 1.823(5) . ? P2 C4 1.828(5) . ? P2 C6 1.835(5) . ? P3 C8 1.811(5) . ? P3 C7 1.830(5) . ? P3 C9 1.830(5) . ? P4 C11 1.824(5) . ? P4 C10 1.827(5) . ? P4 C12 1.831(5) . ? P5 C13 1.804(5) . ? P5 C14 1.812(5) . ? P5 C15 1.813(5) . ? P6 C31 1.824(5) . ? P6 C33 1.827(5) . ? P6 C32 1.832(5) . ? P7 C34 1.807(5) . ? P7 C36 1.820(5) . ? P7 C35 1.841(5) . ? P8 C37 1.823(6) . ? P8 C39 1.825(5) . ? P8 C38 1.827(6) . ? P9 C42 1.805(6) . ? P9 C40 1.828(6) . ? P9 C41 1.844(7) . ? P10 C44 1.809(5) . ? P10 C43 1.813(5) . ? P10 C45 1.821(5) . ? F1 C16 1.336(6) . ? F2 C16 1.325(6) . ? F3 C16 1.329(6) . ? F4 C20 1.320(8) . ? F4B C20 1.337(14) . ? F5 C20 1.327(8) . ? F5B C20 1.333(12) . ? F6 C20 1.340(8) . ? F6B C20 1.350(13) . ? F7 C21 1.340(6) . ? F8 C21 1.352(6) . ? F9 C21 1.354(6) . ? F10 C25 1.342(6) . ? F11 C25 1.346(6) . ? F12 C25 1.331(6) . ? F13 C26 1.334(7) . ? F14 C26 1.353(7) . ? F15 C26 1.298(7) . ? F16 C30 1.332(7) . ? F17 C30 1.322(8) . ? F18 C30 1.320(8) . ? F19 C46 1.338(7) . ? F20 C46 1.329(6) . ? F21 C46 1.329(6) . ? F22 C50 1.344(7) . ? F23 C50 1.290(7) . ? F24 C50 1.324(7) . ? F25 C51 1.344(6) . ? F26 C51 1.352(6) . ? F27 C51 1.354(6) . ? F28 C55 1.365(10) . ? F29 C55 1.349(11) . ? F30 C55 1.285(10) . ? F29B C55 1.325(10) . ? F30B C55 1.299(11) . ? F28B C55 1.367(11) . ? F31 C56 1.300(7) . ? F32 C56 1.329(6) . ? F33 C56 1.327(6) . ? F34 C60 1.346(7) . ? F35 C60 1.319(7) . ? F36 C60 1.342(7) . ? N1 N2 1.354(5) . ? N1 C17 1.354(6) . ? N2 C19 1.333(6) . ? N3 C22 1.347(6) . ? N3 N4 1.361(5) . ? N4 C24 1.349(6) . ? N5 C27 1.352(6) . ? N5 N6 1.361(5) . ? N6 C29 1.336(6) . ? N7 C47 1.360(6) . ? N7 N8 1.361(5) . ? N8 C49 1.341(6) . ? N9 C52 1.350(6) . ? N9 N10 1.351(5) . ? N10 C54 1.349(6) . ? N11 C57 1.357(6) . ? N11 N12 1.361(5) . ? N12 C59 1.329(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.462(7) . ? C17 C18 1.372(7) . ? C18 C19 1.384(7) . ? C18 H18 0.9500 . ? C19 C20 1.461(8) . ? C21 C22 1.473(7) . ? C22 C23 1.368(7) . ? C23 C24 1.376(7) . ? C23 H23 0.9500 . ? C24 C25 1.479(8) . ? C26 C27 1.475(8) . ? C27 C28 1.356(7) . ? C28 C29 1.393(7) . ? C28 H28 0.9500 . ? C29 C30 1.466(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.475(7) . ? C47 C48 1.359(7) . ? C48 C49 1.385(7) . ? C48 H48 0.9500 . ? C49 C50 1.486(8) . ? C51 C52 1.463(7) . ? C52 C53 1.360(7) . ? C53 C54 1.384(7) . ? C53 H53 0.9500 . ? C54 C55 1.475(8) . ? C56 C57 1.465(7) . ? C57 C58 1.391(7) . ? C58 C59 1.387(7) . ? C58 H58 0.9500 . ? C59 C60 1.467(8) . ? 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 P4 143.59(7) . . ? P1 Co1 P3 102.66(7) . . ? P4 Co1 P3 100.92(7) . . ? P1 Co1 P2 101.83(7) . . ? P4 Co1 P2 102.22(7) . . ? P3 Co1 P2 97.33(7) . . ? P1 Co1 H1 73.8(16) . . ? P4 Co1 H1 81.6(16) . . ? P3 Co1 H1 176.3(16) . . ? P2 Co1 H1 84.8(16) . . ? P1 Co1 H2 76.8(19) . . ? P4 Co1 H2 75.7(19) . . ? P3 Co1 H2 90.3(19) . . ? P2 Co1 H2 172.3(19) . . ? H1 Co1 H2 88(2) . . ? N5 Co2 N3 112.45(19) . . ? N5 Co2 N1 116.09(18) . . ? N3 Co2 N1 117.68(19) . . ? N5 Co2 P5 103.85(14) . . ? N3 Co2 P5 102.94(14) . . ? N1 Co2 P5 100.95(14) . . ? P6 Co3 P9 144.78(8) . . ? P6 Co3 P7 101.21(7) . . ? P9 Co3 P7 102.84(7) . . ? P6 Co3 P8 100.86(7) . . ? P9 Co3 P8 100.37(8) . . ? P7 Co3 P8 99.01(7) . . ? P6 Co3 H4 77.9(18) . . ? P9 Co3 H4 78.9(18) . . ? P7 Co3 H4 85.2(18) . . ? P8 Co3 H4 175.8(18) . . ? P6 Co3 H3 76.9(19) . . ? P9 Co3 H3 76.6(19) . . ? P7 Co3 H3 174.3(19) . . ? P8 Co3 H3 86.6(19) . . ? H4 Co3 H3 89(3) . . ? N7 Co4 N9 117.2(2) . . ? N7 Co4 N11 113.24(19) . . ? N9 Co4 N11 113.7(2) . . ? N7 Co4 P10 99.44(14) . . ? N9 Co4 P10 108.72(14) . . ? N11 Co4 P10 102.24(15) . . ? C2 P1 C3 100.4(3) . . ? C2 P1 C1 100.6(3) . . ? C3 P1 C1 101.5(3) . . ? C2 P1 Co1 113.3(2) . . ? C3 P1 Co1 116.69(19) . . ? C1 P1 Co1 121.25(19) . . ? C5 P2 C4 101.5(3) . . ? C5 P2 C6 100.5(3) . . ? C4 P2 C6 99.0(3) . . ? C5 P2 Co1 114.76(19) . . ? C4 P2 Co1 118.71(19) . . ? C6 P2 Co1 119.17(18) . . ? C8 P3 C7 101.2(3) . . ? C8 P3 C9 101.1(3) . . ? C7 P3 C9 98.7(2) . . ? C8 P3 Co1 115.2(2) . . ? C7 P3 Co1 120.22(18) . . ? C9 P3 Co1 117.25(18) . . ? C11 P4 C10 99.9(3) . . ? C11 P4 C12 101.1(3) . . ? C10 P4 C12 100.4(3) . . ? C11 P4 Co1 112.68(19) . . ? C10 P4 Co1 117.03(19) . . ? C12 P4 Co1 122.33(19) . . ? C13 P5 C14 103.5(3) . . ? C13 P5 C15 104.2(2) . . ? C14 P5 C15 103.2(3) . . ? C13 P5 Co2 115.12(19) . . ? C14 P5 Co2 116.38(18) . . ? C15 P5 Co2 112.99(18) . . ? C31 P6 C33 101.0(3) . . ? C31 P6 C32 100.5(3) . . ? C33 P6 C32 102.1(3) . . ? C31 P6 Co3 113.2(2) . . ? C33 P6 Co3 115.3(2) . . ? C32 P6 Co3 121.72(19) . . ? C34 P7 C36 101.1(3) . . ? C34 P7 C35 102.2(3) . . ? C36 P7 C35 99.1(3) . . ? C34 P7 Co3 114.1(2) . . ? C36 P7 Co3 118.8(2) . . ? C35 P7 Co3 118.66(19) . . ? C37 P8 C39 101.2(3) . . ? C37 P8 C38 101.6(3) . . ? C39 P8 C38 98.8(3) . . ? C37 P8 Co3 114.2(2) . . ? C39 P8 Co3 118.9(2) . . ? C38 P8 Co3 119.1(2) . . ? C42 P9 C40 102.1(3) . . ? C42 P9 C41 100.0(3) . . ? C40 P9 C41 99.6(4) . . ? C42 P9 Co3 116.4(2) . . ? C40 P9 Co3 112.6(2) . . ? C41 P9 Co3 122.9(2) . . ? C44 P10 C43 104.0(3) . . ? C44 P10 C45 103.1(3) . . ? C43 P10 C45 104.1(3) . . ? C44 P10 Co4 113.6(2) . . ? C43 P10 Co4 114.5(2) . . ? C45 P10 Co4 116.0(2) . . ? N2 N1 C17 109.4(5) . . ? N2 N1 Co2 109.5(4) . . ? C17 N1 Co2 141.0(4) . . ? C19 N2 N1 105.9(5) . . ? C22 N3 N4 109.0(5) . . ? C22 N3 Co2 138.8(4) . . ? N4 N3 Co2 112.1(4) . . ? C24 N4 N3 105.4(5) . . ? C27 N5 N6 108.1(5) . . ? C27 N5 Co2 139.4(4) . . ? N6 N5 Co2 111.8(3) . . ? C29 N6 N5 106.8(5) . . ? C47 N7 N8 108.4(5) . . ? C47 N7 Co4 138.6(4) . . ? N8 N7 Co4 112.8(3) . . ? C49 N8 N7 106.1(5) . . ? C52 N9 N10 109.2(5) . . ? C52 N9 Co4 136.4(4) . . ? N10 N9 Co4 113.9(4) . . ? C54 N10 N9 105.9(5) . . ? C57 N11 N12 109.1(5) . . ? C57 N11 Co4 140.5(4) . . ? N12 N11 Co4 110.2(4) . . ? C59 N12 N11 106.2(5) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P5 C13 H13A 109.5 . . ? P5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P5 C14 H14A 109.5 . . ? P5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P5 C15 H15A 109.5 . . ? P5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? F2 C16 F3 106.4(5) . . ? F2 C16 F1 104.6(6) . . ? F3 C16 F1 105.3(5) . . ? F2 C16 C17 113.5(5) . . ? F3 C16 C17 112.7(6) . . ? F1 C16 C17 113.6(5) . . ? N1 C17 C18 109.0(6) . . ? N1 C17 C16 123.0(6) . . ? C18 C17 C16 128.0(6) . . ? C17 C18 C19 103.9(6) . . ? C17 C18 H18 128.1 . . ? C19 C18 H18 128.1 . . ? N2 C19 C18 111.8(5) . . ? N2 C19 C20 119.0(6) . . ? C18 C19 C20 129.2(6) . . ? F4 C20 F5 107.0(8) . . ? F5B C20 F4B 103.5(13) . . ? F4 C20 F6 105.2(7) . . ? F5 C20 F6 104.3(7) . . ? F5B C20 F6B 102.3(11) . . ? F4B C20 F6B 103.7(13) . . ? F4 C20 C19 113.6(7) . . ? F5 C20 C19 114.8(7) . . ? F5B C20 C19 119.9(13) . . ? F4B C20 C19 115.9(15) . . ? F6 C20 C19 111.1(7) . . ? F6B C20 C19 109.6(15) . . ? F7 C21 F8 105.7(5) . . ? F7 C21 F9 106.4(5) . . ? F8 C21 F9 105.3(5) . . ? F7 C21 C22 113.6(5) . . ? F8 C21 C22 114.0(5) . . ? F9 C21 C22 111.2(5) . . ? N3 C22 C23 109.9(5) . . ? N3 C22 C21 121.5(6) . . ? C23 C22 C21 128.6(6) . . ? C22 C23 C24 103.7(5) . . ? C22 C23 H23 128.1 . . ? C24 C23 H23 128.1 . . ? N4 C24 C23 111.9(5) . . ? N4 C24 C25 120.2(6) . . ? C23 C24 C25 127.9(6) . . ? F12 C25 F10 106.8(5) . . ? F12 C25 F11 105.9(6) . . ? F10 C25 F11 105.7(6) . . ? F12 C25 C24 114.1(6) . . ? F10 C25 C24 112.1(6) . . ? F11 C25 C24 111.6(5) . . ? F15 C26 F13 106.9(6) . . ? F15 C26 F14 105.4(6) . . ? F13 C26 F14 105.3(6) . . ? F15 C26 C27 114.9(6) . . ? F13 C26 C27 113.4(6) . . ? F14 C26 C27 110.2(6) . . ? N5 C27 C28 110.2(5) . . ? N5 C27 C26 120.8(6) . . ? C28 C27 C26 128.9(6) . . ? C27 C28 C29 104.2(5) . . ? C27 C28 H28 127.9 . . ? C29 C28 H28 127.9 . . ? N6 C29 C28 110.6(5) . . ? N6 C29 C30 119.6(6) . . ? C28 C29 C30 129.7(6) . . ? F18 C30 F17 108.0(6) . . ? F18 C30 F16 105.6(7) . . ? F17 C30 F16 104.4(6) . . ? F18 C30 C29 113.2(6) . . ? F17 C30 C29 112.5(7) . . ? F16 C30 C29 112.5(6) . . ? P6 C31 H31A 109.5 . . ? P6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P6 C32 H32A 109.5 . . ? P6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P6 C33 H33A 109.5 . . ? P6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P7 C34 H34A 109.5 . . ? P7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? P7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? P7 C35 H35A 109.5 . . ? P7 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P7 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P7 C36 H36A 109.5 . . ? P7 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? P7 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P8 C37 H37A 109.5 . . ? P8 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P8 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P8 C38 H38A 109.5 . . ? P8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P8 C39 H39A 109.5 . . ? P8 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P8 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P9 C40 H40A 109.5 . . ? P9 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P9 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? P9 C41 H41A 109.5 . . ? P9 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P9 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P9 C42 H42A 109.5 . . ? P9 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P9 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P10 C43 H43A 109.5 . . ? P10 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? P10 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? P10 C44 H44A 109.5 . . ? P10 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? P10 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? P10 C45 H45A 109.5 . . ? P10 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? P10 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? F20 C46 F21 107.1(5) . . ? F20 C46 F19 104.4(5) . . ? F21 C46 F19 106.0(5) . . ? F20 C46 C47 113.9(5) . . ? F21 C46 C47 111.0(6) . . ? F19 C46 C47 113.9(6) . . ? N7 C47 C48 110.0(5) . . ? N7 C47 C46 119.9(6) . . ? C48 C47 C46 130.1(6) . . ? C47 C48 C49 103.9(5) . . ? C47 C48 H48 128.0 . . ? C49 C48 H48 128.0 . . ? N8 C49 C48 111.6(5) . . ? N8 C49 C50 119.9(6) . . ? C48 C49 C50 128.5(6) . . ? F23 C50 F24 108.2(6) . . ? F23 C50 F22 105.6(6) . . ? F24 C50 F22 103.9(6) . . ? F23 C50 C49 113.7(6) . . ? F24 C50 C49 112.9(6) . . ? F22 C50 C49 111.8(6) . . ? F25 C51 F26 105.8(5) . . ? F25 C51 F27 105.7(5) . . ? F26 C51 F27 104.7(5) . . ? F25 C51 C52 113.4(6) . . ? F26 C51 C52 113.0(5) . . ? F27 C51 C52 113.4(5) . . ? N9 C52 C53 109.7(5) . . ? N9 C52 C51 122.6(6) . . ? C53 C52 C51 127.5(6) . . ? C52 C53 C54 104.2(5) . . ? C52 C53 H53 127.9 . . ? C54 C53 H53 127.9 . . ? N10 C54 C53 111.0(5) . . ? N10 C54 C55 120.7(6) . . ? C53 C54 C55 128.2(6) . . ? F30 C55 F30B 116.6(15) . . ? F30B C55 F29B 110.6(10) . . ? F30 C55 F29 106.9(10) . . ? F30 C55 F28 108.4(9) . . ? F29 C55 F28 101.9(8) . . ? F30B C55 F28B 104.7(10) . . ? F29B C55 F28B 103.3(9) . . ? F30 C55 C54 119.6(9) . . ? F30B C55 C54 117.8(12) . . ? F29B C55 C54 111.6(8) . . ? F29 C55 C54 109.4(9) . . ? F28 C55 C54 109.3(8) . . ? F28B C55 C54 107.6(9) . . ? F31 C56 F33 105.8(6) . . ? F31 C56 F32 104.9(6) . . ? F33 C56 F32 104.2(6) . . ? F31 C56 C57 115.6(6) . . ? F33 C56 C57 112.1(6) . . ? F32 C56 C57 113.2(5) . . ? N11 C57 C58 109.1(6) . . ? N11 C57 C56 122.1(6) . . ? C58 C57 C56 128.8(6) . . ? C59 C58 C57 103.1(6) . . ? C59 C58 H58 128.4 . . ? C57 C58 H58 128.4 . . ? N12 C59 C58 112.5(6) . . ? N12 C59 C60 119.6(6) . . ? C58 C59 C60 127.9(6) . . ? F35 C60 F36 106.3(6) . . ? F35 C60 F34 106.4(6) . . ? F36 C60 F34 104.4(6) . . ? F35 C60 C59 112.6(6) . . ? F36 C60 C59 113.1(6) . . ? F34 C60 C59 113.3(6) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P4 Co1 P1 C2 -35.6(3) . . . . ? P3 Co1 P1 C2 93.6(2) . . . . ? P2 Co1 P1 C2 -166.0(2) . . . . ? P4 Co1 P1 C3 80.2(2) . . . . ? P3 Co1 P1 C3 -150.6(2) . . . . ? P2 Co1 P1 C3 -50.2(2) . . . . ? P4 Co1 P1 C1 -155.2(2) . . . . ? P3 Co1 P1 C1 -26.1(2) . . . . ? P2 Co1 P1 C1 74.4(2) . . . . ? P1 Co1 P2 C5 95.5(2) . . . . ? P4 Co1 P2 C5 -56.9(2) . . . . ? P3 Co1 P2 C5 -159.9(2) . . . . ? P1 Co1 P2 C4 -24.7(2) . . . . ? P4 Co1 P2 C4 -177.2(2) . . . . ? P3 Co1 P2 C4 79.9(2) . . . . ? P1 Co1 P2 C6 -145.3(2) . . . . ? P4 Co1 P2 C6 62.2(2) . . . . ? P3 Co1 P2 C6 -40.7(2) . . . . ? P1 Co1 P3 C8 -64.8(2) . . . . ? P4 Co1 P3 C8 87.2(2) . . . . ? P2 Co1 P3 C8 -168.8(2) . . . . ? P1 Co1 P3 C7 56.6(2) . . . . ? P4 Co1 P3 C7 -151.3(2) . . . . ? P2 Co1 P3 C7 -47.3(2) . . . . ? P1 Co1 P3 C9 176.4(2) . . . . ? P4 Co1 P3 C9 -31.5(2) . . . . ? P2 Co1 P3 C9 72.5(2) . . . . ? P1 Co1 P4 C11 -32.1(3) . . . . ? P3 Co1 P4 C11 -161.7(2) . . . . ? P2 Co1 P4 C11 98.2(2) . . . . ? P1 Co1 P4 C10 82.8(2) . . . . ? P3 Co1 P4 C10 -46.8(2) . . . . ? P2 Co1 P4 C10 -146.9(2) . . . . ? P1 Co1 P4 C12 -152.9(2) . . . . ? P3 Co1 P4 C12 77.4(2) . . . . ? P2 Co1 P4 C12 -22.6(2) . . . . ? N5 Co2 P5 C13 -73.3(2) . . . . ? N3 Co2 P5 C13 44.1(2) . . . . ? N1 Co2 P5 C13 166.1(2) . . . . ? N5 Co2 P5 C14 48.0(2) . . . . ? N3 Co2 P5 C14 165.4(2) . . . . ? N1 Co2 P5 C14 -72.6(2) . . . . ? N5 Co2 P5 C15 167.1(2) . . . . ? N3 Co2 P5 C15 -75.5(2) . . . . ? N1 Co2 P5 C15 46.5(2) . . . . ? P9 Co3 P6 C31 -42.1(3) . . . . ? P7 Co3 P6 C31 90.2(2) . . . . ? P8 Co3 P6 C31 -168.2(2) . . . . ? P9 Co3 P6 C33 73.5(3) . . . . ? P7 Co3 P6 C33 -154.1(2) . . . . ? P8 Co3 P6 C33 -52.6(2) . . . . ? P9 Co3 P6 C32 -162.0(2) . . . . ? P7 Co3 P6 C32 -29.7(2) . . . . ? P8 Co3 P6 C32 71.9(2) . . . . ? P6 Co3 P7 C34 -56.4(2) . . . . ? P9 Co3 P7 C34 97.7(2) . . . . ? P8 Co3 P7 C34 -159.4(2) . . . . ? P6 Co3 P7 C36 -175.5(2) . . . . ? P9 Co3 P7 C36 -21.4(2) . . . . ? P8 Co3 P7 C36 81.5(2) . . . . ? P6 Co3 P7 C35 64.1(2) . . . . ? P9 Co3 P7 C35 -141.8(2) . . . . ? P8 Co3 P7 C35 -38.9(2) . . . . ? P6 Co3 P8 C37 91.2(2) . . . . ? P9 Co3 P8 C37 -60.5(2) . . . . ? P7 Co3 P8 C37 -165.4(2) . . . . ? P6 Co3 P8 C39 -28.1(2) . . . . ? P9 Co3 P8 C39 -179.9(2) . . . . ? P7 Co3 P8 C39 75.2(2) . . . . ? P6 Co3 P8 C38 -148.6(3) . . . . ? P9 Co3 P8 C38 59.6(3) . . . . ? P7 Co3 P8 C38 -45.3(3) . . . . ? P6 Co3 P9 C42 77.0(3) . . . . ? P7 Co3 P9 C42 -54.9(3) . . . . ? P8 Co3 P9 C42 -156.7(3) . . . . ? P6 Co3 P9 C40 -40.4(3) . . . . ? P7 Co3 P9 C40 -172.3(3) . . . . ? P8 Co3 P9 C40 85.8(3) . . . . ? P6 Co3 P9 C41 -159.4(3) . . . . ? P7 Co3 P9 C41 68.7(3) . . . . ? P8 Co3 P9 C41 -33.2(3) . . . . ? N7 Co4 P10 C44 -42.0(3) . . . . ? N9 Co4 P10 C44 -165.1(3) . . . . ? N11 Co4 P10 C44 74.5(3) . . . . ? N7 Co4 P10 C43 -161.4(3) . . . . ? N9 Co4 P10 C43 75.6(3) . . . . ? N11 Co4 P10 C43 -44.9(3) . . . . ? N7 Co4 P10 C45 77.2(3) . . . . ? N9 Co4 P10 C45 -45.8(3) . . . . ? N11 Co4 P10 C45 -166.3(3) . . . . ? N5 Co2 N1 N2 -74.4(4) . . . . ? N3 Co2 N1 N2 148.2(3) . . . . ? P5 Co2 N1 N2 37.1(3) . . . . ? N5 Co2 N1 C17 108.8(6) . . . . ? N3 Co2 N1 C17 -28.7(6) . . . . ? P5 Co2 N1 C17 -139.7(5) . . . . ? C17 N1 N2 C19 -0.7(6) . . . . ? Co2 N1 N2 C19 -178.6(3) . . . . ? N5 Co2 N3 C22 -24.9(6) . . . . ? N1 Co2 N3 C22 114.0(5) . . . . ? P5 Co2 N3 C22 -136.0(5) . . . . ? N5 Co2 N3 N4 159.0(3) . . . . ? N1 Co2 N3 N4 -62.0(4) . . . . ? P5 Co2 N3 N4 47.9(3) . . . . ? C22 N3 N4 C24 0.3(6) . . . . ? Co2 N3 N4 C24 177.6(3) . . . . ? N3 Co2 N5 C27 93.2(6) . . . . ? N1 Co2 N5 C27 -46.4(6) . . . . ? P5 Co2 N5 C27 -156.2(5) . . . . ? N3 Co2 N5 N6 -76.1(4) . . . . ? N1 Co2 N5 N6 144.3(3) . . . . ? P5 Co2 N5 N6 34.5(4) . . . . ? C27 N5 N6 C29 -0.1(6) . . . . ? Co2 N5 N6 C29 172.6(3) . . . . ? N9 Co4 N7 C47 -108.8(6) . . . . ? N11 Co4 N7 C47 26.6(6) . . . . ? P10 Co4 N7 C47 134.4(6) . . . . ? N9 Co4 N7 N8 77.8(4) . . . . ? N11 Co4 N7 N8 -146.8(3) . . . . ? P10 Co4 N7 N8 -39.0(4) . . . . ? C47 N7 N8 C49 0.4(6) . . . . ? Co4 N7 N8 C49 175.7(3) . . . . ? N7 Co4 N9 C52 27.3(6) . . . . ? N11 Co4 N9 C52 -108.0(5) . . . . ? P10 Co4 N9 C52 138.9(5) . . . . ? N7 Co4 N9 N10 -162.6(3) . . . . ? N11 Co4 N9 N10 62.2(4) . . . . ? P10 Co4 N9 N10 -51.0(4) . . . . ? C52 N9 N10 C54 -0.2(6) . . . . ? Co4 N9 N10 C54 -173.0(3) . . . . ? N7 Co4 N11 C57 -105.9(6) . . . . ? N9 Co4 N11 C57 31.1(6) . . . . ? P10 Co4 N11 C57 148.1(5) . . . . ? N7 Co4 N11 N12 69.2(4) . . . . ? N9 Co4 N11 N12 -153.8(3) . . . . ? P10 Co4 N11 N12 -36.8(3) . . . . ? C57 N11 N12 C59 0.3(6) . . . . ? Co4 N11 N12 C59 -176.4(3) . . . . ? N2 N1 C17 C18 0.3(6) . . . . ? Co2 N1 C17 C18 177.2(4) . . . . ? N2 N1 C17 C16 179.2(5) . . . . ? Co2 N1 C17 C16 -3.9(9) . . . . ? F2 C16 C17 N1 27.8(8) . . . . ? F3 C16 C17 N1 148.9(5) . . . . ? F1 C16 C17 N1 -91.5(7) . . . . ? F2 C16 C17 C18 -153.5(6) . . . . ? F3 C16 C17 C18 -32.4(8) . . . . ? F1 C16 C17 C18 87.2(8) . . . . ? N1 C17 C18 C19 0.1(6) . . . . ? C16 C17 C18 C19 -178.7(5) . . . . ? N1 N2 C19 C18 0.8(6) . . . . ? N1 N2 C19 C20 -179.2(5) . . . . ? C17 C18 C19 N2 -0.6(6) . . . . ? C17 C18 C19 C20 179.4(6) . . . . ? N2 C19 C20 F4 -167.8(7) . . . . ? C18 C19 C20 F4 12.3(10) . . . . ? N2 C19 C20 F5 -44.2(9) . . . . ? C18 C19 C20 F5 135.9(7) . . . . ? N2 C19 C20 F5B 110.8(14) . . . . ? C18 C19 C20 F5B -69.2(15) . . . . ? N2 C19 C20 F4B -14.6(15) . . . . ? C18 C19 C20 F4B 165.5(14) . . . . ? N2 C19 C20 F6 73.9(7) . . . . ? C18 C19 C20 F6 -106.0(8) . . . . ? N2 C19 C20 F6B -131.4(12) . . . . ? C18 C19 C20 F6B 48.6(13) . . . . ? N4 N3 C22 C23 -0.6(6) . . . . ? Co2 N3 C22 C23 -176.7(4) . . . . ? N4 N3 C22 C21 -178.8(5) . . . . ? Co2 N3 C22 C21 5.0(9) . . . . ? F7 C21 C22 N3 -53.8(7) . . . . ? F8 C21 C22 N3 67.4(7) . . . . ? F9 C21 C22 N3 -173.8(5) . . . . ? F7 C21 C22 C23 128.3(6) . . . . ? F8 C21 C22 C23 -110.6(7) . . . . ? F9 C21 C22 C23 8.3(8) . . . . ? N3 C22 C23 C24 0.6(6) . . . . ? C21 C22 C23 C24 178.7(5) . . . . ? N3 N4 C24 C23 0.1(6) . . . . ? N3 N4 C24 C25 -178.5(5) . . . . ? C22 C23 C24 N4 -0.4(6) . . . . ? C22 C23 C24 C25 178.0(6) . . . . ? N4 C24 C25 F12 -8.9(8) . . . . ? C23 C24 C25 F12 172.9(5) . . . . ? N4 C24 C25 F10 -130.4(6) . . . . ? C23 C24 C25 F10 51.3(8) . . . . ? N4 C24 C25 F11 111.1(6) . . . . ? C23 C24 C25 F11 -67.1(8) . . . . ? N6 N5 C27 C28 -0.5(6) . . . . ? Co2 N5 C27 C28 -170.0(4) . . . . ? N6 N5 C27 C26 -177.9(6) . . . . ? Co2 N5 C27 C26 12.5(9) . . . . ? F15 C26 C27 N5 89.9(8) . . . . ? F13 C26 C27 N5 -33.5(9) . . . . ? F14 C26 C27 N5 -151.2(5) . . . . ? F15 C26 C27 C28 -87.0(9) . . . . ? F13 C26 C27 C28 149.6(6) . . . . ? F14 C26 C27 C28 31.8(10) . . . . ? N5 C27 C28 C29 0.8(7) . . . . ? C26 C27 C28 C29 178.0(6) . . . . ? N5 N6 C29 C28 0.6(6) . . . . ? N5 N6 C29 C30 -176.6(6) . . . . ? C27 C28 C29 N6 -0.9(7) . . . . ? C27 C28 C29 C30 176.0(7) . . . . ? N6 C29 C30 F18 -30.7(10) . . . . ? C28 C29 C30 F18 152.7(6) . . . . ? N6 C29 C30 F17 92.1(8) . . . . ? C28 C29 C30 F17 -84.5(9) . . . . ? N6 C29 C30 F16 -150.3(6) . . . . ? C28 C29 C30 F16 33.1(11) . . . . ? N8 N7 C47 C48 0.3(6) . . . . ? Co4 N7 C47 C48 -173.3(4) . . . . ? N8 N7 C47 C46 178.3(5) . . . . ? Co4 N7 C47 C46 4.8(9) . . . . ? F20 C46 C47 N7 47.5(8) . . . . ? F21 C46 C47 N7 168.4(5) . . . . ? F19 C46 C47 N7 -72.1(8) . . . . ? F20 C46 C47 C48 -134.9(6) . . . . ? F21 C46 C47 C48 -14.0(10) . . . . ? F19 C46 C47 C48 105.5(7) . . . . ? N7 C47 C48 C49 -0.7(6) . . . . ? C46 C47 C48 C49 -178.6(6) . . . . ? N7 N8 C49 C48 -0.8(6) . . . . ? N7 N8 C49 C50 -179.1(5) . . . . ? C47 C48 C49 N8 1.0(7) . . . . ? C47 C48 C49 C50 179.1(6) . . . . ? N8 C49 C50 F23 -179.1(6) . . . . ? C48 C49 C50 F23 3.0(11) . . . . ? N8 C49 C50 F24 -55.3(9) . . . . ? C48 C49 C50 F24 126.8(7) . . . . ? N8 C49 C50 F22 61.4(8) . . . . ? C48 C49 C50 F22 -116.6(7) . . . . ? N10 N9 C52 C53 0.2(6) . . . . ? Co4 N9 C52 C53 170.6(4) . . . . ? N10 N9 C52 C51 174.9(5) . . . . ? Co4 N9 C52 C51 -14.7(9) . . . . ? F25 C51 C52 N9 174.8(5) . . . . ? F26 C51 C52 N9 -64.7(7) . . . . ? F27 C51 C52 N9 54.3(8) . . . . ? F25 C51 C52 C53 -11.4(9) . . . . ? F26 C51 C52 C53 109.0(7) . . . . ? F27 C51 C52 C53 -132.0(6) . . . . ? N9 C52 C53 C54 0.0(6) . . . . ? C51 C52 C53 C54 -174.4(6) . . . . ? N9 N10 C54 C53 0.2(6) . . . . ? N9 N10 C54 C55 179.2(5) . . . . ? C52 C53 C54 N10 -0.2(7) . . . . ? C52 C53 C54 C55 -179.0(6) . . . . ? N10 C54 C55 F30 -99.5(11) . . . . ? C53 C54 C55 F30 79.3(12) . . . . ? N10 C54 C55 F30B 52.4(12) . . . . ? C53 C54 C55 F30B -128.9(11) . . . . ? N10 C54 C55 F29B -178.1(10) . . . . ? C53 C54 C55 F29B 0.6(13) . . . . ? N10 C54 C55 F29 24.2(10) . . . . ? C53 C54 C55 F29 -157.1(9) . . . . ? N10 C54 C55 F28 134.9(8) . . . . ? C53 C54 C55 F28 -46.3(11) . . . . ? N10 C54 C55 F28B -65.5(10) . . . . ? C53 C54 C55 F28B 113.2(9) . . . . ? N12 N11 C57 C58 -0.6(6) . . . . ? Co4 N11 C57 C58 174.5(4) . . . . ? N12 N11 C57 C56 179.8(5) . . . . ? Co4 N11 C57 C56 -5.0(9) . . . . ? F31 C56 C57 N11 59.7(8) . . . . ? F33 C56 C57 N11 -178.9(5) . . . . ? F32 C56 C57 N11 -61.4(8) . . . . ? F31 C56 C57 C58 -119.8(7) . . . . ? F33 C56 C57 C58 1.6(9) . . . . ? F32 C56 C57 C58 119.2(7) . . . . ? N11 C57 C58 C59 0.7(6) . . . . ? C56 C57 C58 C59 -179.8(6) . . . . ? N11 N12 C59 C58 0.1(6) . . . . ? N11 N12 C59 C60 176.6(5) . . . . ? C57 C58 C59 N12 -0.5(6) . . . . ? C57 C58 C59 C60 -176.6(6) . . . . ? N12 C59 C60 F35 170.1(5) . . . . ? C58 C59 C60 F35 -14.0(10) . . . . ? N12 C59 C60 F36 49.6(9) . . . . ? C58 C59 C60 F36 -134.6(6) . . . . ? N12 C59 C60 F34 -69.0(8) . . . . ? C58 C59 C60 F34 106.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.430 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.078 data_CoPz3(OPMe3)3Li _database_code_depnum_ccdc_archive 'CCDC 887458' #TrackingRef '4 CoPz3(OPMe3)3Li (4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; lithium-bis(trimethylphosphineoxid-\m-trimethylphosphineoxide- \m-3,5-bis(trifluoromethyl)pyrazolate- bis(3,5-bis(trifluoromethyl)pyrazolate)cobalt(ii) ; _chemical_name_common ; lithium-bis(trimethylphosphineoxid-mu-trimethylphosphineoxide- mu-3,5-bis(trifluoromethyl)pyrazolate-bis(3,5- bis(trifluoromethyl)pyrazolate)cobalt(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 Co F18 Li N6 O3 P3' _chemical_formula_sum 'C24 H30 Co F18 Li N6 O3 P3' _chemical_formula_weight 951.32 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.371(3) _cell_length_b 12.277(3) _cell_length_c 24.941(8) _cell_angle_alpha 90.00 _cell_angle_beta 115.58(2) _cell_angle_gamma 90.00 _cell_volume 3969.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15011 _cell_measurement_theta_min 1.8104 _cell_measurement_theta_max 31.4404 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.2960 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.773 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43036 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9118 _reflns_number_gt 8067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+3.8889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9118 _refine_ls_number_parameters 572 _refine_ls_number_restraints 330 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.204 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.15826(3) 0.43150(3) 0.190688(18) 0.02122(12) Uani 1 1 d . . . P1 P 0.03395(7) 0.29879(7) 0.25103(4) 0.0286(2) Uani 1 1 d . . . P3 P 0.16279(7) 0.47929(8) 0.44084(4) 0.0299(2) Uani 1 1 d U . . P2 P 0.42449(7) 0.28840(8) 0.38280(4) 0.0344(2) Uani 1 1 d . . . Li1 Li 0.2203(4) 0.4394(5) 0.3320(3) 0.0280(12) Uani 1 1 d . . . F1 F 0.18651(17) 0.60584(17) 0.11737(9) 0.0371(5) Uani 1 1 d . . . F2 F 0.3016(2) 0.7316(2) 0.14321(10) 0.0527(7) Uani 1 1 d . . . F3 F 0.1485(2) 0.7682(2) 0.13204(10) 0.0556(7) Uani 1 1 d . . . F4 F 0.3673(10) 0.5975(8) 0.4084(6) 0.051(3) Uani 0.44 1 d PDU A 1 F5 F 0.4573(6) 0.7174(10) 0.3923(7) 0.081(4) Uani 0.44 1 d PDU A 1 F6 F 0.3169(8) 0.7611(9) 0.3956(6) 0.085(5) Uani 0.44 1 d PDU A 1 F4B F 0.4401(6) 0.7539(7) 0.3931(6) 0.072(3) Uani 0.56 1 d PDU A 2 F6B F 0.3914(8) 0.5999(5) 0.4112(5) 0.052(3) Uani 0.56 1 d PDU A 2 F5B F 0.2932(6) 0.7365(6) 0.3918(4) 0.0464(18) Uani 0.56 1 d PDU A 2 F7 F 0.4129(2) 0.4922(2) 0.21666(16) 0.0712(9) Uani 1 1 d . . . F8 F 0.3546(2) 0.4738(2) 0.12345(16) 0.0783(11) Uani 1 1 d . . . F9 F 0.49583(16) 0.39723(19) 0.17939(12) 0.0459(6) Uani 1 1 d . . . F10 F 0.1968(5) 0.0067(8) 0.1856(3) 0.0568(19) Uani 0.58 1 d PDU B 1 F11 F 0.2402(5) -0.0001(7) 0.11547(19) 0.0577(19) Uani 0.58 1 d PDU B 1 F12 F 0.3526(4) -0.0203(6) 0.2034(3) 0.0575(19) Uani 0.58 1 d PDU B 1 F11B F 0.2366(8) -0.0045(12) 0.2073(5) 0.082(4) Uani 0.42 1 d PDU B 2 F12B F 0.2001(8) 0.0098(12) 0.1164(3) 0.108(5) Uani 0.42 1 d PDU B 2 F10B F 0.3524(7) -0.0208(11) 0.1780(5) 0.089(4) Uani 0.42 1 d PDU B 2 F13 F 0.15365(16) 0.38040(19) 0.05748(9) 0.0397(5) Uani 1 1 d . . . F14 F 0.07448(19) 0.23041(18) 0.05585(10) 0.0423(5) Uani 1 1 d . . . F15 F 0.01841(17) 0.33466(19) -0.02117(9) 0.0403(5) Uani 1 1 d . . . F16 F -0.25453(18) 0.4957(2) 0.11303(11) 0.0529(7) Uani 1 1 d . . . F17 F -0.31562(17) 0.4570(2) 0.01990(12) 0.0585(7) Uani 1 1 d . . . F18 F -0.24934(19) 0.6142(2) 0.05162(12) 0.0564(7) Uani 1 1 d . . . O1 O 0.11814(16) 0.37641(18) 0.25299(10) 0.0248(5) Uani 1 1 d . . . O2 O 0.32323(18) 0.3366(2) 0.37244(11) 0.0366(6) Uani 1 1 d . . . O3 O 0.15014(19) 0.4809(2) 0.37815(10) 0.0312(5) Uani 1 1 d . . . N1 N 0.2217(2) 0.5716(2) 0.23155(11) 0.0229(5) Uani 1 1 d . . . N2 N 0.2586(2) 0.5696(2) 0.29184(11) 0.0240(6) Uani 1 1 d . . . N3 N 0.2599(2) 0.3245(2) 0.18731(12) 0.0243(6) Uani 1 1 d . . . N4 N 0.2247(2) 0.2218(2) 0.18624(12) 0.0253(6) Uani 1 1 d . . . N5 N 0.0278(2) 0.4348(2) 0.11616(11) 0.0247(6) Uani 1 1 d . . . N6 N -0.0524(2) 0.4789(2) 0.12364(12) 0.0282(6) Uani 1 1 d . . . C1 C -0.0204(3) 0.2198(3) 0.18439(17) 0.0356(8) Uani 1 1 d . . . H1A H -0.0619 0.2670 0.1509 0.053 Uiso 1 1 calc R . . H1B H -0.0644 0.1626 0.1886 0.053 Uiso 1 1 calc R . . H1C H 0.0351 0.1865 0.1772 0.053 Uiso 1 1 calc R . . C2 C 0.0860(4) 0.2070(4) 0.3118(2) 0.0573(13) Uani 1 1 d . . . H2A H 0.1361 0.1590 0.3067 0.086 Uiso 1 1 calc R . . H2B H 0.0303 0.1631 0.3134 0.086 Uiso 1 1 calc R . . H2C H 0.1204 0.2482 0.3489 0.086 Uiso 1 1 calc R . . C3 C -0.0671(3) 0.3743(4) 0.25689(18) 0.0429(10) Uani 1 1 d . . . H3A H -0.0393 0.4152 0.2943 0.064 Uiso 1 1 calc R . . H3B H -0.1207 0.3241 0.2562 0.064 Uiso 1 1 calc R . . H3C H -0.0970 0.4251 0.2234 0.064 Uiso 1 1 calc R . . C4 C 0.4931(4) 0.2436(5) 0.4574(2) 0.0692(16) Uani 1 1 d . . . H4A H 0.5017 0.3045 0.4845 0.104 Uiso 1 1 calc R . . H4B H 0.5611 0.2164 0.4635 0.104 Uiso 1 1 calc R . . H4C H 0.4545 0.1850 0.4654 0.104 Uiso 1 1 calc R . . C5 C 0.4147(4) 0.1726(4) 0.3376(2) 0.0584(13) Uani 1 1 d . . . H5A H 0.3769 0.1146 0.3467 0.088 Uiso 1 1 calc R . . H5B H 0.4840 0.1468 0.3456 0.088 Uiso 1 1 calc R . . H5C H 0.3777 0.1928 0.2956 0.088 Uiso 1 1 calc R . . C6 C 0.5053(4) 0.3846(5) 0.3696(3) 0.0794(19) Uani 1 1 d . . . H6A H 0.4732 0.4065 0.3277 0.119 Uiso 1 1 calc R . . H6B H 0.5726 0.3513 0.3791 0.119 Uiso 1 1 calc R . . H6C H 0.5146 0.4488 0.3948 0.119 Uiso 1 1 calc R . . C7 C 0.2624(5) 0.3919(5) 0.4878(2) 0.084(2) Uani 1 1 d U . . H7A H 0.2474 0.3171 0.4728 0.126 Uiso 1 1 calc R . . H7B H 0.2668 0.3947 0.5281 0.126 Uiso 1 1 calc R . . H7C H 0.3282 0.4153 0.4887 0.126 Uiso 1 1 calc R . . C8 C 0.0483(5) 0.4369(6) 0.4451(2) 0.081(2) Uani 1 1 d U . . H8A H -0.0083 0.4860 0.4214 0.122 Uiso 1 1 calc R . . H8B H 0.0588 0.4388 0.4866 0.122 Uiso 1 1 calc R . . H8C H 0.0311 0.3625 0.4297 0.122 Uiso 1 1 calc R . . C9 C 0.1895(4) 0.6104(4) 0.4750(2) 0.0543(12) Uani 1 1 d U . . H9A H 0.2546 0.6379 0.4765 0.081 Uiso 1 1 calc R . . H9B H 0.1951 0.6048 0.5155 0.081 Uiso 1 1 calc R . . H9C H 0.1334 0.6606 0.4518 0.081 Uiso 1 1 calc R . . C10 C 0.2221(3) 0.6921(3) 0.15266(15) 0.0302(7) Uani 1 1 d . . . C11 C 0.2528(2) 0.6649(3) 0.21566(14) 0.0232(6) Uani 1 1 d . . . C12 C 0.3113(2) 0.7266(3) 0.26565(14) 0.0256(7) Uani 1 1 d . . . H12 H 0.3429 0.7955 0.2678 0.031 Uiso 1 1 calc R . . C13 C 0.3122(2) 0.6625(3) 0.31177(14) 0.0241(6) Uani 1 1 d . A . C14 C 0.3608(2) 0.6865(3) 0.37612(15) 0.0334(8) Uani 1 1 d DU . . C15 C 0.4017(3) 0.4195(3) 0.17503(19) 0.0390(9) Uani 1 1 d . . . C16 C 0.3459(2) 0.3200(3) 0.17779(15) 0.0272(7) Uani 1 1 d . . . C17 C 0.3684(3) 0.2132(3) 0.17045(16) 0.0308(7) Uani 1 1 d . . . H17 H 0.4240 0.1858 0.1634 0.037 Uiso 1 1 calc R . . C18 C 0.2892(3) 0.1554(3) 0.17590(15) 0.0269(7) Uani 1 1 d . B . C19 C 0.2694(2) 0.0364(3) 0.16993(14) 0.0317(7) Uani 1 1 d DU . . C20 C 0.0595(3) 0.3359(3) 0.03824(14) 0.0317(8) Uani 1 1 d . . . C21 C -0.0077(3) 0.3941(3) 0.06016(14) 0.0264(7) Uani 1 1 d . . . C22 C -0.1130(3) 0.4114(3) 0.03022(15) 0.0316(8) Uani 1 1 d . . . H22 H -0.1584 0.3917 -0.0094 0.038 Uiso 1 1 calc R . . C23 C -0.1359(3) 0.4646(3) 0.07203(15) 0.0294(7) Uani 1 1 d . . . C24 C -0.2374(3) 0.5077(3) 0.06418(18) 0.0388(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0211(2) 0.0203(2) 0.0209(2) -0.00220(16) 0.00781(16) -0.00051(16) P1 0.0268(4) 0.0273(5) 0.0298(4) 0.0019(4) 0.0104(3) -0.0061(3) P3 0.0383(5) 0.0273(5) 0.0255(4) 0.0025(4) 0.0151(4) 0.0037(4) P2 0.0280(4) 0.0391(5) 0.0314(5) -0.0028(4) 0.0085(4) 0.0071(4) Li1 0.029(3) 0.027(3) 0.027(3) 0.001(2) 0.011(2) 0.001(2) F1 0.0525(13) 0.0312(11) 0.0227(10) -0.0042(8) 0.0118(9) -0.0094(10) F2 0.0618(15) 0.0636(17) 0.0334(12) 0.0021(11) 0.0213(11) -0.0309(13) F3 0.0737(17) 0.0392(13) 0.0342(12) 0.0075(10) 0.0048(12) 0.0218(12) F4 0.059(6) 0.067(6) 0.019(4) 0.002(4) 0.010(4) -0.037(4) F5 0.052(4) 0.160(10) 0.029(4) -0.036(7) 0.015(4) -0.061(5) F6 0.108(9) 0.059(6) 0.048(5) -0.032(5) -0.005(5) 0.032(6) F4B 0.091(5) 0.095(5) 0.036(3) -0.033(4) 0.033(4) -0.077(4) F6B 0.068(6) 0.040(4) 0.028(3) -0.002(3) 0.002(3) 0.015(4) F5B 0.053(3) 0.062(4) 0.029(3) -0.023(3) 0.023(3) -0.009(3) F7 0.0671(18) 0.0448(15) 0.128(3) -0.0394(17) 0.0673(19) -0.0278(14) F8 0.0410(14) 0.0579(18) 0.112(3) 0.0464(18) 0.0099(15) -0.0084(13) F9 0.0307(11) 0.0368(12) 0.0776(17) 0.0039(12) 0.0303(12) 0.0014(10) F10 0.069(3) 0.033(3) 0.100(5) -0.011(4) 0.067(4) -0.013(3) F11 0.118(5) 0.029(3) 0.033(3) -0.011(2) 0.040(3) -0.012(4) F12 0.049(3) 0.025(3) 0.071(4) 0.010(3) 0.000(3) 0.008(2) F11B 0.158(10) 0.035(5) 0.092(7) 0.001(5) 0.090(7) -0.015(7) F12B 0.129(9) 0.036(5) 0.079(7) -0.007(5) -0.029(6) -0.018(6) F10B 0.067(6) 0.044(5) 0.175(11) -0.019(8) 0.069(7) 0.011(4) F13 0.0335(11) 0.0534(14) 0.0328(11) -0.0036(10) 0.0147(9) -0.0003(10) F14 0.0582(14) 0.0308(11) 0.0353(12) 0.0002(9) 0.0178(11) 0.0082(10) F15 0.0442(12) 0.0507(14) 0.0210(10) -0.0034(9) 0.0095(9) 0.0037(11) F16 0.0336(12) 0.0728(18) 0.0545(15) -0.0008(13) 0.0211(11) 0.0048(12) F17 0.0253(11) 0.0714(18) 0.0584(16) -0.0195(14) -0.0012(11) -0.0029(11) F18 0.0434(14) 0.0439(14) 0.0719(18) 0.0078(13) 0.0155(13) 0.0144(11) O1 0.0219(10) 0.0268(12) 0.0244(11) -0.0026(9) 0.0089(9) -0.0032(9) O2 0.0263(12) 0.0407(15) 0.0395(14) 0.0063(12) 0.0112(11) 0.0076(11) O3 0.0362(13) 0.0327(13) 0.0266(12) 0.0016(10) 0.0153(10) 0.0064(11) N1 0.0261(13) 0.0221(13) 0.0204(13) 0.0005(10) 0.0100(11) -0.0007(11) N2 0.0273(13) 0.0241(14) 0.0200(13) -0.0030(10) 0.0096(11) -0.0047(11) N3 0.0220(12) 0.0232(14) 0.0277(14) -0.0012(11) 0.0108(11) 0.0002(11) N4 0.0271(13) 0.0246(14) 0.0243(13) -0.0006(11) 0.0111(11) 0.0010(11) N5 0.0260(13) 0.0248(14) 0.0200(13) -0.0025(11) 0.0068(11) -0.0011(11) N6 0.0244(13) 0.0274(15) 0.0286(14) -0.0018(12) 0.0073(11) 0.0016(11) C1 0.0304(17) 0.0332(19) 0.042(2) -0.0073(16) 0.0139(16) -0.0085(15) C2 0.059(3) 0.043(2) 0.049(3) 0.014(2) 0.003(2) -0.016(2) C3 0.0315(19) 0.061(3) 0.040(2) -0.0079(19) 0.0192(17) -0.0108(18) C4 0.055(3) 0.091(4) 0.039(2) -0.004(3) 0.000(2) 0.036(3) C5 0.062(3) 0.060(3) 0.042(2) -0.012(2) 0.011(2) 0.015(2) C6 0.054(3) 0.064(3) 0.144(6) 0.006(4) 0.064(4) 0.008(3) C7 0.122(5) 0.091(4) 0.030(2) 0.011(3) 0.024(3) 0.067(4) C8 0.084(4) 0.123(5) 0.044(3) -0.001(3) 0.035(3) -0.047(4) C9 0.091(4) 0.039(2) 0.041(2) -0.0051(19) 0.037(2) -0.005(2) C10 0.0372(18) 0.0236(16) 0.0255(17) -0.0005(13) 0.0095(14) -0.0036(14) C11 0.0252(15) 0.0196(15) 0.0231(15) 0.0012(12) 0.0088(12) -0.0007(12) C12 0.0242(15) 0.0238(16) 0.0285(16) -0.0031(13) 0.0110(13) -0.0041(13) C13 0.0236(15) 0.0250(16) 0.0233(15) -0.0058(12) 0.0099(12) -0.0054(13) C14 0.0384(19) 0.0332(19) 0.0273(17) -0.0082(14) 0.0129(15) -0.0112(16) C15 0.0266(17) 0.032(2) 0.058(3) 0.0011(18) 0.0187(17) 0.0007(15) C16 0.0245(15) 0.0239(16) 0.0336(18) -0.0003(14) 0.0130(14) 0.0005(13) C17 0.0317(17) 0.0288(18) 0.0374(19) -0.0012(15) 0.0201(15) 0.0057(14) C18 0.0287(16) 0.0256(17) 0.0283(16) -0.0024(13) 0.0142(13) 0.0016(13) C19 0.0366(18) 0.0282(18) 0.0335(18) -0.0002(14) 0.0183(15) 0.0002(15) C20 0.0364(18) 0.0348(19) 0.0198(15) -0.0004(14) 0.0081(14) -0.0025(15) C21 0.0306(16) 0.0228(16) 0.0215(15) -0.0008(12) 0.0073(13) -0.0033(13) C22 0.0325(17) 0.0302(18) 0.0242(16) -0.0008(14) 0.0049(14) -0.0027(14) C23 0.0258(16) 0.0278(17) 0.0277(17) -0.0007(14) 0.0050(13) -0.0009(13) C24 0.0260(17) 0.040(2) 0.041(2) -0.0033(17) 0.0054(15) -0.0027(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co1 N5 1.991(3) . ? Co1 N3 1.993(3) . ? Co1 O1 1.994(2) . ? Co1 N1 2.006(3) . ? Co1 Li1 3.242(6) . ? P1 O1 1.524(2) . ? P1 C2 1.774(4) . ? P1 C3 1.781(4) . ? P1 C1 1.787(4) . ? P1 Li1 3.092(6) . ? P3 O3 1.494(2) . ? P3 C7 1.768(5) . ? P3 C8 1.772(5) . ? P3 C9 1.784(4) . ? P2 O2 1.486(3) . ? P2 C4 1.776(5) . ? P2 C5 1.782(5) . ? P2 C6 1.784(5) . ? Li1 O2 1.873(6) . ? Li1 O3 1.899(6) . ? Li1 O1 2.034(6) . ? Li1 N2 2.082(6) . ? F1 C10 1.330(4) . ? F2 C10 1.352(4) . ? F3 C10 1.337(4) . ? F4 C14 1.336(6) . ? F5 C14 1.322(6) . ? F6 C14 1.318(6) . ? F4B C14 1.322(6) . ? F6B C14 1.324(6) . ? F5B C14 1.343(5) . ? F7 C15 1.326(5) . ? F8 C15 1.344(5) . ? F9 C15 1.338(4) . ? F10 C19 1.315(5) . ? F11 C19 1.315(5) . ? F12 C19 1.323(5) . ? F11B C19 1.313(6) . ? F12B C19 1.317(6) . ? F10B C19 1.322(6) . ? F13 C20 1.341(4) . ? F14 C20 1.355(4) . ? F15 C20 1.338(4) . ? F16 C24 1.351(5) . ? F17 C24 1.341(4) . ? F18 C24 1.339(5) . ? N1 C11 1.350(4) . ? N1 N2 1.362(4) . ? N2 C13 1.346(4) . ? N3 N4 1.354(4) . ? N3 C16 1.357(4) . ? N4 C18 1.339(4) . ? N5 N6 1.357(4) . ? N5 C21 1.358(4) . ? N6 C23 1.340(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.475(4) . ? C11 C12 1.390(4) . ? C12 C13 1.389(5) . ? C12 H12 0.9500 . ? C13 C14 1.477(4) . ? C15 C16 1.478(5) . ? C16 C17 1.382(5) . ? C17 C18 1.397(5) . ? C17 H17 0.9500 . ? C18 C19 1.483(5) . ? C20 C21 1.483(5) . ? C21 C22 1.384(5) . ? C22 C23 1.385(5) . ? C22 H22 0.9500 . ? C23 C24 1.482(5) . ? 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 N5 Co1 N3 112.70(11) . . ? N5 Co1 O1 105.17(10) . . ? N3 Co1 O1 105.84(10) . . ? N5 Co1 N1 119.69(11) . . ? N3 Co1 N1 113.94(11) . . ? O1 Co1 N1 96.65(10) . . ? N5 Co1 Li1 136.10(13) . . ? N3 Co1 Li1 101.71(13) . . ? O1 Co1 Li1 36.84(12) . . ? N1 Co1 Li1 64.58(13) . . ? O1 P1 C2 109.48(18) . . ? O1 P1 C3 109.65(17) . . ? C2 P1 C3 108.6(2) . . ? O1 P1 C1 113.04(16) . . ? C2 P1 C1 107.7(2) . . ? C3 P1 C1 108.30(18) . . ? C2 P1 Li1 82.53(18) . . ? C3 P1 Li1 99.38(17) . . ? C1 P1 Li1 144.90(17) . . ? O3 P3 C7 113.54(19) . . ? O3 P3 C8 111.7(2) . . ? C7 P3 C8 106.8(3) . . ? O3 P3 C9 113.08(18) . . ? C7 P3 C9 106.6(3) . . ? C8 P3 C9 104.5(3) . . ? O2 P2 C4 111.4(2) . . ? O2 P2 C5 113.8(2) . . ? C4 P2 C5 105.8(2) . . ? O2 P2 C6 111.8(2) . . ? C4 P2 C6 106.7(3) . . ? C5 P2 C6 106.9(3) . . ? O2 Li1 O3 110.9(3) . . ? O2 Li1 O1 109.7(3) . . ? O3 Li1 O1 109.8(3) . . ? O2 Li1 N2 117.7(3) . . ? O3 Li1 N2 113.9(3) . . ? O1 Li1 N2 93.2(2) . . ? O2 Li1 P1 103.6(2) . . ? O3 Li1 P1 90.5(2) . . ? O1 Li1 P1 25.27(10) . . ? N2 Li1 P1 116.7(2) . . ? O2 Li1 Co1 110.4(2) . . ? O3 Li1 Co1 134.3(3) . . ? O1 Li1 Co1 36.00(12) . . ? N2 Li1 Co1 60.40(16) . . ? P1 Li1 Co1 61.26(11) . . ? P1 O1 Co1 132.81(13) . . ? P1 O1 Li1 120.0(2) . . ? Co1 O1 Li1 107.16(19) . . ? P2 O2 Li1 148.0(2) . . ? P3 O3 Li1 140.8(2) . . ? C11 N1 N2 108.6(2) . . ? C11 N1 Co1 135.5(2) . . ? N2 N1 Co1 114.88(19) . . ? C13 N2 N1 106.3(3) . . ? C13 N2 Li1 134.5(3) . . ? N1 N2 Li1 119.1(2) . . ? N4 N3 C16 108.6(3) . . ? N4 N3 Co1 109.93(19) . . ? C16 N3 Co1 140.7(2) . . ? C18 N4 N3 106.7(3) . . ? N6 N5 C21 108.9(3) . . ? N6 N5 Co1 113.2(2) . . ? C21 N5 Co1 137.5(2) . . ? C23 N6 N5 106.1(3) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F1 C10 F3 106.7(3) . . ? F1 C10 F2 106.4(3) . . ? F3 C10 F2 105.7(3) . . ? F1 C10 C11 112.2(3) . . ? F3 C10 C11 113.0(3) . . ? F2 C10 C11 112.4(3) . . ? N1 C11 C12 110.4(3) . . ? N1 C11 C10 121.4(3) . . ? C12 C11 C10 128.2(3) . . ? C13 C12 C11 102.7(3) . . ? C13 C12 H12 128.7 . . ? C11 C12 H12 128.7 . . ? N2 C13 C12 112.1(3) . . ? N2 C13 C14 119.8(3) . . ? C12 C13 C14 128.2(3) . . ? F6 C14 F5 107.1(6) . . ? F4B C14 F6B 107.3(5) . . ? F6 C14 F4 105.5(6) . . ? F5 C14 F4 105.1(6) . . ? F4B C14 F5B 104.6(5) . . ? F6B C14 F5B 104.5(5) . . ? F6 C14 C13 117.5(7) . . ? F4B C14 C13 114.3(6) . . ? F5 C14 C13 109.2(7) . . ? F6B C14 C13 115.1(6) . . ? F4 C14 C13 111.6(7) . . ? F5B C14 C13 110.2(4) . . ? F7 C15 F9 107.3(3) . . ? F7 C15 F8 104.8(4) . . ? F9 C15 F8 104.6(3) . . ? F7 C15 C16 113.9(3) . . ? F9 C15 C16 112.2(3) . . ? F8 C15 C16 113.3(3) . . ? N3 C16 C17 110.1(3) . . ? N3 C16 C15 121.9(3) . . ? C17 C16 C15 128.0(3) . . ? C16 C17 C18 102.8(3) . . ? C16 C17 H17 128.6 . . ? C18 C17 H17 128.6 . . ? N4 C18 C17 111.7(3) . . ? N4 C18 C19 120.0(3) . . ? C17 C18 C19 128.2(3) . . ? F10 C19 F11 105.8(5) . . ? F11B C19 F12B 106.2(6) . . ? F11B C19 F10B 105.3(6) . . ? F12B C19 F10B 105.1(6) . . ? F10 C19 F12 106.4(5) . . ? F11 C19 F12 105.7(5) . . ? F11B C19 C18 114.7(7) . . ? F10 C19 C18 112.7(5) . . ? F11 C19 C18 113.7(5) . . ? F12B C19 C18 112.0(7) . . ? F10B C19 C18 112.8(7) . . ? F12 C19 C18 111.9(5) . . ? F15 C20 F13 107.2(3) . . ? F15 C20 F14 106.3(3) . . ? F13 C20 F14 106.2(3) . . ? F15 C20 C21 111.5(3) . . ? F13 C20 C21 112.9(3) . . ? F14 C20 C21 112.2(3) . . ? N5 C21 C22 109.6(3) . . ? N5 C21 C20 122.7(3) . . ? C22 C21 C20 127.5(3) . . ? C21 C22 C23 103.1(3) . . ? C21 C22 H22 128.5 . . ? C23 C22 H22 128.5 . . ? N6 C23 C22 112.3(3) . . ? N6 C23 C24 120.1(3) . . ? C22 C23 C24 127.5(3) . . ? F18 C24 F17 106.5(3) . . ? F18 C24 F16 105.2(3) . . ? F17 C24 F16 106.1(3) . . ? F18 C24 C23 113.5(3) . . ? F17 C24 C23 111.7(3) . . ? F16 C24 C23 113.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 Li1 O2 -107.5(3) . . . . ? C2 P1 Li1 O2 33.8(3) . . . . ? C3 P1 Li1 O2 141.5(3) . . . . ? C1 P1 Li1 O2 -76.5(4) . . . . ? O1 P1 Li1 O3 140.9(3) . . . . ? C2 P1 Li1 O3 -77.9(3) . . . . ? C3 P1 Li1 O3 29.8(2) . . . . ? C1 P1 Li1 O3 171.9(2) . . . . ? C2 P1 Li1 O1 141.2(3) . . . . ? C3 P1 Li1 O1 -111.1(3) . . . . ? C1 P1 Li1 O1 31.0(4) . . . . ? O1 P1 Li1 N2 23.6(2) . . . . ? C2 P1 Li1 N2 164.8(3) . . . . ? C3 P1 Li1 N2 -87.5(3) . . . . ? C1 P1 Li1 N2 54.6(4) . . . . ? O1 P1 Li1 Co1 -1.47(18) . . . . ? C2 P1 Li1 Co1 139.7(2) . . . . ? C3 P1 Li1 Co1 -112.55(16) . . . . ? C1 P1 Li1 Co1 29.5(3) . . . . ? N5 Co1 Li1 O2 136.6(2) . . . . ? N3 Co1 Li1 O2 -5.0(3) . . . . ? O1 Co1 Li1 O2 95.8(3) . . . . ? N1 Co1 Li1 O2 -116.2(3) . . . . ? N5 Co1 Li1 O3 -16.7(5) . . . . ? N3 Co1 Li1 O3 -158.4(3) . . . . ? O1 Co1 Li1 O3 -57.5(3) . . . . ? N1 Co1 Li1 O3 90.5(4) . . . . ? N5 Co1 Li1 O1 40.8(3) . . . . ? N3 Co1 Li1 O1 -100.85(19) . . . . ? N1 Co1 Li1 O1 148.0(2) . . . . ? N5 Co1 Li1 N2 -112.35(19) . . . . ? N3 Co1 Li1 N2 106.04(17) . . . . ? O1 Co1 Li1 N2 -153.1(3) . . . . ? N1 Co1 Li1 N2 -5.08(14) . . . . ? N5 Co1 Li1 P1 41.8(2) . . . . ? N3 Co1 Li1 P1 -99.78(11) . . . . ? O1 Co1 Li1 P1 1.07(13) . . . . ? N1 Co1 Li1 P1 149.09(14) . . . . ? C2 P1 O1 Co1 135.9(2) . . . . ? C3 P1 O1 Co1 -105.0(2) . . . . ? C1 P1 O1 Co1 15.9(3) . . . . ? Li1 P1 O1 Co1 177.1(3) . . . . ? C2 P1 O1 Li1 -41.2(3) . . . . ? C3 P1 O1 Li1 77.8(3) . . . . ? C1 P1 O1 Li1 -161.2(2) . . . . ? N5 Co1 O1 P1 30.6(2) . . . . ? N3 Co1 O1 P1 -89.0(2) . . . . ? N1 Co1 O1 P1 153.80(19) . . . . ? Li1 Co1 O1 P1 -177.4(3) . . . . ? N5 Co1 O1 Li1 -152.0(2) . . . . ? N3 Co1 O1 Li1 88.5(2) . . . . ? N1 Co1 O1 Li1 -28.8(2) . . . . ? O2 Li1 O1 P1 80.0(3) . . . . ? O3 Li1 O1 P1 -42.1(4) . . . . ? N2 Li1 O1 P1 -158.99(18) . . . . ? Co1 Li1 O1 P1 177.8(3) . . . . ? O2 Li1 O1 Co1 -97.8(3) . . . . ? O3 Li1 O1 Co1 140.1(2) . . . . ? N2 Li1 O1 Co1 23.2(2) . . . . ? P1 Li1 O1 Co1 -177.8(3) . . . . ? C4 P2 O2 Li1 147.4(5) . . . . ? C5 P2 O2 Li1 -93.1(5) . . . . ? C6 P2 O2 Li1 28.1(6) . . . . ? O3 Li1 O2 P2 -151.5(3) . . . . ? O1 Li1 O2 P2 87.1(5) . . . . ? N2 Li1 O2 P2 -17.7(7) . . . . ? P1 Li1 O2 P2 112.7(4) . . . . ? Co1 Li1 O2 P2 48.7(5) . . . . ? C7 P3 O3 Li1 -14.9(5) . . . . ? C8 P3 O3 Li1 -135.8(4) . . . . ? C9 P3 O3 Li1 106.7(4) . . . . ? O2 Li1 O3 P3 18.7(5) . . . . ? O1 Li1 O3 P3 140.1(3) . . . . ? N2 Li1 O3 P3 -116.8(4) . . . . ? P1 Li1 O3 P3 123.5(3) . . . . ? Co1 Li1 O3 P3 171.9(2) . . . . ? N5 Co1 N1 C11 -55.2(3) . . . . ? N3 Co1 N1 C11 82.5(3) . . . . ? O1 Co1 N1 C11 -166.9(3) . . . . ? Li1 Co1 N1 C11 174.5(3) . . . . ? N5 Co1 N1 N2 137.8(2) . . . . ? N3 Co1 N1 N2 -84.5(2) . . . . ? O1 Co1 N1 N2 26.1(2) . . . . ? Li1 Co1 N1 N2 7.5(2) . . . . ? C11 N1 N2 C13 -0.2(3) . . . . ? Co1 N1 N2 C13 170.3(2) . . . . ? C11 N1 N2 Li1 177.5(3) . . . . ? Co1 N1 N2 Li1 -12.1(3) . . . . ? O2 Li1 N2 C13 -76.6(5) . . . . ? O3 Li1 N2 C13 55.8(5) . . . . ? O1 Li1 N2 C13 169.2(3) . . . . ? P1 Li1 N2 C13 159.3(3) . . . . ? Co1 Li1 N2 C13 -175.4(4) . . . . ? O2 Li1 N2 N1 106.6(4) . . . . ? O3 Li1 N2 N1 -121.0(3) . . . . ? O1 Li1 N2 N1 -7.7(3) . . . . ? P1 Li1 N2 N1 -17.6(4) . . . . ? Co1 Li1 N2 N1 7.8(2) . . . . ? N5 Co1 N3 N4 -68.1(2) . . . . ? O1 Co1 N3 N4 46.4(2) . . . . ? N1 Co1 N3 N4 151.30(19) . . . . ? Li1 Co1 N3 N4 84.1(2) . . . . ? N5 Co1 N3 C16 99.9(4) . . . . ? O1 Co1 N3 C16 -145.6(3) . . . . ? N1 Co1 N3 C16 -40.7(4) . . . . ? Li1 Co1 N3 C16 -107.9(4) . . . . ? C16 N3 N4 C18 -0.2(3) . . . . ? Co1 N3 N4 C18 171.8(2) . . . . ? N3 Co1 N5 N6 160.3(2) . . . . ? O1 Co1 N5 N6 45.4(2) . . . . ? N1 Co1 N5 N6 -61.6(2) . . . . ? Li1 Co1 N5 N6 21.5(3) . . . . ? N3 Co1 N5 C21 -10.5(4) . . . . ? O1 Co1 N5 C21 -125.3(3) . . . . ? N1 Co1 N5 C21 127.7(3) . . . . ? Li1 Co1 N5 C21 -149.2(3) . . . . ? C21 N5 N6 C23 0.0(4) . . . . ? Co1 N5 N6 C23 -173.4(2) . . . . ? N2 N1 C11 C12 0.0(4) . . . . ? Co1 N1 C11 C12 -167.5(2) . . . . ? N2 N1 C11 C10 -178.2(3) . . . . ? Co1 N1 C11 C10 14.3(5) . . . . ? F1 C10 C11 N1 -16.3(5) . . . . ? F3 C10 C11 N1 104.4(4) . . . . ? F2 C10 C11 N1 -136.1(3) . . . . ? F1 C10 C11 C12 165.9(3) . . . . ? F3 C10 C11 C12 -73.5(4) . . . . ? F2 C10 C11 C12 46.0(5) . . . . ? N1 C11 C12 C13 0.1(4) . . . . ? C10 C11 C12 C13 178.1(3) . . . . ? N1 N2 C13 C12 0.2(4) . . . . ? Li1 N2 C13 C12 -176.9(3) . . . . ? N1 N2 C13 C14 178.6(3) . . . . ? Li1 N2 C13 C14 1.5(5) . . . . ? C11 C12 C13 N2 -0.2(4) . . . . ? C11 C12 C13 C14 -178.4(3) . . . . ? N2 C13 C14 F6 -105.6(7) . . . . ? C12 C13 C14 F6 72.5(7) . . . . ? N2 C13 C14 F4B 155.9(5) . . . . ? C12 C13 C14 F4B -26.0(7) . . . . ? N2 C13 C14 F5 132.2(7) . . . . ? C12 C13 C14 F5 -49.7(7) . . . . ? N2 C13 C14 F6B 31.2(6) . . . . ? C12 C13 C14 F6B -150.7(6) . . . . ? N2 C13 C14 F4 16.5(7) . . . . ? C12 C13 C14 F4 -165.4(7) . . . . ? N2 C13 C14 F5B -86.7(5) . . . . ? C12 C13 C14 F5B 91.4(5) . . . . ? N4 N3 C16 C17 -0.2(4) . . . . ? Co1 N3 C16 C17 -168.3(3) . . . . ? N4 N3 C16 C15 178.6(3) . . . . ? Co1 N3 C16 C15 10.6(6) . . . . ? F7 C15 C16 N3 43.2(5) . . . . ? F9 C15 C16 N3 165.3(3) . . . . ? F8 C15 C16 N3 -76.5(5) . . . . ? F7 C15 C16 C17 -138.3(4) . . . . ? F9 C15 C16 C17 -16.2(6) . . . . ? F8 C15 C16 C17 102.0(5) . . . . ? N3 C16 C17 C18 0.4(4) . . . . ? C15 C16 C17 C18 -178.3(4) . . . . ? N3 N4 C18 C17 0.5(4) . . . . ? N3 N4 C18 C19 -177.8(3) . . . . ? C16 C17 C18 N4 -0.5(4) . . . . ? C16 C17 C18 C19 177.5(3) . . . . ? N4 C18 C19 F11B -40.0(7) . . . . ? C17 C18 C19 F11B 142.0(6) . . . . ? N4 C18 C19 F10 -10.7(5) . . . . ? C17 C18 C19 F10 171.3(5) . . . . ? N4 C18 C19 F11 109.6(5) . . . . ? C17 C18 C19 F11 -68.3(6) . . . . ? N4 C18 C19 F12B 81.1(7) . . . . ? C17 C18 C19 F12B -96.9(7) . . . . ? N4 C18 C19 F10B -160.6(6) . . . . ? C17 C18 C19 F10B 21.5(7) . . . . ? N4 C18 C19 F12 -130.6(4) . . . . ? C17 C18 C19 F12 51.4(6) . . . . ? N6 N5 C21 C22 -0.1(4) . . . . ? Co1 N5 C21 C22 170.9(3) . . . . ? N6 N5 C21 C20 -177.4(3) . . . . ? Co1 N5 C21 C20 -6.4(5) . . . . ? F15 C20 C21 N5 -160.0(3) . . . . ? F13 C20 C21 N5 -39.1(5) . . . . ? F14 C20 C21 N5 80.9(4) . . . . ? F15 C20 C21 C22 23.3(5) . . . . ? F13 C20 C21 C22 144.2(3) . . . . ? F14 C20 C21 C22 -95.8(4) . . . . ? N5 C21 C22 C23 0.2(4) . . . . ? C20 C21 C22 C23 177.2(3) . . . . ? N5 N6 C23 C22 0.1(4) . . . . ? N5 N6 C23 C24 -177.7(3) . . . . ? C21 C22 C23 N6 -0.2(4) . . . . ? C21 C22 C23 C24 177.4(4) . . . . ? N6 C23 C24 F18 80.3(5) . . . . ? C22 C23 C24 F18 -97.0(5) . . . . ? N6 C23 C24 F17 -159.2(3) . . . . ? C22 C23 C24 F17 23.4(6) . . . . ? N6 C23 C24 F16 -39.5(5) . . . . ? C22 C23 C24 F16 143.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.470 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.084 data_Co2Pz4P2Li2O2H2 _database_code_depnum_ccdc_archive 'CCDC 887459' #TrackingRef '5 Co2Pz4(LiOH)2(PMe3)2 (5).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Co2 F24 Li2 N8 O2 P2' _chemical_formula_sum 'C26 H24 Co2 F24 Li2 N8 O2 P2' _chemical_formula_weight 1130.21 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.313(2) _cell_length_b 11.028(5) _cell_length_c 11.569(5) _cell_angle_alpha 102.591(5) _cell_angle_beta 90.458(7) _cell_angle_gamma 112.259(17) _cell_volume 1067.8(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6021 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.7 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7085 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3686 _reflns_number_gt 3056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+4.3270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3686 _refine_ls_number_parameters 330 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.71586(7) 0.09942(7) 0.33590(6) 0.0226(2) Uani 1 1 d . . . P1 P 0.78786(16) 0.28315(15) 0.24467(13) 0.0289(4) Uani 1 1 d . . . F1 F 1.2015(4) 0.3115(3) 0.3977(3) 0.0422(9) Uani 1 1 d . . . F2 F 1.2357(4) 0.1409(4) 0.4325(3) 0.0448(9) Uani 1 1 d . . . F3 F 1.0502(4) 0.1116(4) 0.3043(3) 0.0381(8) Uani 1 1 d . . . F4 F 0.9606(8) 0.1660(9) 0.8644(6) 0.066(2) Uani 0.72 1 d PDU A 1 F4B F 1.0144(11) 0.2659(19) 0.8713(11) 0.071(6) Uani 0.28 1 d PDU A 2 F5 F 0.9145(14) 0.3366(6) 0.8552(7) 0.110(4) Uani 0.72 1 d PDU A 1 F5B F 0.800(2) 0.0989(10) 0.8272(15) 0.071(5) Uani 0.28 1 d PDU A 2 F6 F 0.7352(6) 0.1437(9) 0.8138(6) 0.080(3) Uani 0.72 1 d PDU A 1 F6B F 0.8119(18) 0.2930(15) 0.8288(12) 0.046(4) Uani 0.28 1 d PDU A 2 F7 F 0.8970(4) 0.0069(4) 0.0875(3) 0.0487(10) Uani 1 1 d . . . F8 F 0.7735(4) -0.1720(4) -0.0523(3) 0.0456(9) Uani 1 1 d . . . F9 F 0.6797(5) -0.0192(4) 0.0034(3) 0.0500(10) Uani 1 1 d . . . F10 F 0.3264(4) -0.4111(4) 0.3347(4) 0.0503(10) Uani 1 1 d U . . F11 F 0.5254(5) -0.4612(4) 0.3384(4) 0.0671(13) Uani 1 1 d U . . F12 F 0.3698(5) -0.5346(4) 0.1796(4) 0.0582(12) Uani 1 1 d U . . O1 O 0.5296(4) 0.0828(4) 0.4128(3) 0.0269(8) Uani 1 1 d . . . H1 H 0.4602 0.1226 0.3835 0.032 Uiso 1 1 calc R . . N1 N 0.8676(5) 0.1555(4) 0.4823(4) 0.0237(9) Uani 1 1 d . . . N2 N 0.8038(5) 0.1650(4) 0.5875(4) 0.0245(10) Uani 1 1 d . . . N3 N 0.6504(5) -0.0916(4) 0.2376(4) 0.0234(9) Uani 1 1 d . . . N4 N 0.5606(5) -0.1822(4) 0.2976(4) 0.0244(10) Uani 1 1 d . . . C1 C 0.6403(8) 0.2836(8) 0.1419(6) 0.0509(18) Uani 1 1 d . . . H1A H 0.6754 0.3713 0.1214 0.076 Uiso 1 1 calc R . . H1B H 0.5428 0.2675 0.1792 0.076 Uiso 1 1 calc R . . H1C H 0.6229 0.2123 0.0695 0.076 Uiso 1 1 calc R . . C2 C 0.8235(10) 0.4321(7) 0.3626(6) 0.056(2) Uani 1 1 d . . . H2A H 0.8416 0.5096 0.3280 0.084 Uiso 1 1 calc R . . H2B H 0.9156 0.4496 0.4154 0.084 Uiso 1 1 calc R . . H2C H 0.7328 0.4177 0.4082 0.084 Uiso 1 1 calc R . . C3 C 0.9612(8) 0.3279(7) 0.1668(6) 0.0479(17) Uani 1 1 d . . . H3A H 0.9480 0.2551 0.0965 0.072 Uiso 1 1 calc R . . H3B H 1.0514 0.3416 0.2198 0.072 Uiso 1 1 calc R . . H3C H 0.9780 0.4113 0.1419 0.072 Uiso 1 1 calc R . . C4 C 1.1266(6) 0.1850(6) 0.4106(5) 0.0284(12) Uani 1 1 d . . . C5 C 1.0204(6) 0.1791(5) 0.5069(5) 0.0242(11) Uani 1 1 d . . . C6 C 1.0582(6) 0.2031(6) 0.6273(5) 0.0285(12) Uani 1 1 d . . . H6 H 1.1558 0.2218 0.6684 0.034 Uiso 1 1 calc R . . C7 C 0.9172(6) 0.1930(5) 0.6739(5) 0.0271(12) Uani 1 1 d . A . C8 C 0.8842(6) 0.2115(5) 0.8002(5) 0.0382(14) Uani 1 1 d DU . . C9 C 0.7557(6) -0.0870(6) 0.0422(5) 0.0346(14) Uani 1 1 d . . . C10 C 0.6724(6) -0.1608(5) 0.1321(5) 0.0269(12) Uani 1 1 d . . . C11 C 0.5990(6) -0.2962(6) 0.1206(5) 0.0290(12) Uani 1 1 d . . . H11 H 0.5949 -0.3675 0.0557 0.035 Uiso 1 1 calc R . . C12 C 0.5309(6) -0.3049(5) 0.2275(5) 0.0253(11) Uani 1 1 d . . . C13 C 0.4383(7) -0.4274(6) 0.2702(6) 0.0354(14) Uani 1 1 d U . . Li1 Li 0.5675(10) 0.1116(9) 0.5804(8) 0.030(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0099(4) 0.0244(4) 0.0304(4) 0.0083(3) 0.0099(3) 0.0021(3) P1 0.0210(7) 0.0289(8) 0.0348(8) 0.0125(6) 0.0060(6) 0.0048(6) F1 0.0296(19) 0.0336(19) 0.057(2) 0.0189(16) 0.0223(16) 0.0010(15) F2 0.0269(19) 0.070(3) 0.054(2) 0.0261(19) 0.0188(16) 0.0308(19) F3 0.0232(17) 0.047(2) 0.0344(18) 0.0052(15) 0.0134(13) 0.0054(15) F4 0.069(5) 0.121(6) 0.037(3) 0.034(4) 0.020(3) 0.062(5) F4B 0.037(8) 0.154(16) 0.016(6) -0.002(10) -0.002(6) 0.042(10) F5 0.226(12) 0.040(4) 0.049(5) 0.008(3) 0.050(7) 0.036(6) F5B 0.101(14) 0.052(9) 0.049(9) 0.037(7) 0.041(10) 0.005(9) F6 0.034(3) 0.160(9) 0.041(3) 0.036(4) 0.019(3) 0.026(4) F6B 0.058(9) 0.089(13) 0.019(7) 0.015(7) 0.022(6) 0.057(9) F7 0.0274(19) 0.049(2) 0.041(2) 0.0052(16) 0.0149(15) -0.0140(16) F8 0.039(2) 0.043(2) 0.0385(19) 0.0030(16) 0.0234(16) 0.0016(17) F9 0.049(2) 0.051(2) 0.053(2) 0.0281(19) 0.0207(18) 0.014(2) F10 0.044(2) 0.035(2) 0.072(3) 0.0209(18) 0.0433(19) 0.0104(17) F11 0.051(3) 0.054(3) 0.102(3) 0.051(3) 0.003(2) 0.009(2) F12 0.054(3) 0.027(2) 0.063(3) 0.0013(18) 0.025(2) -0.0118(18) O1 0.0113(17) 0.027(2) 0.042(2) 0.0113(16) 0.0118(15) 0.0044(15) N1 0.012(2) 0.026(2) 0.031(2) 0.0098(18) 0.0101(17) 0.0035(18) N2 0.016(2) 0.026(2) 0.032(2) 0.0126(19) 0.0140(17) 0.0057(18) N3 0.011(2) 0.024(2) 0.031(2) 0.0090(18) 0.0110(17) 0.0003(17) N4 0.008(2) 0.025(2) 0.037(2) 0.0115(19) 0.0088(17) -0.0005(17) C1 0.044(4) 0.058(5) 0.059(4) 0.025(4) -0.001(3) 0.023(4) C2 0.077(6) 0.031(4) 0.053(4) 0.007(3) 0.004(4) 0.015(4) C3 0.036(4) 0.047(4) 0.063(4) 0.038(3) 0.022(3) 0.006(3) C4 0.018(3) 0.032(3) 0.037(3) 0.013(2) 0.008(2) 0.008(2) C5 0.013(2) 0.021(3) 0.037(3) 0.012(2) 0.009(2) 0.003(2) C6 0.019(3) 0.032(3) 0.036(3) 0.013(2) 0.007(2) 0.009(2) C7 0.019(3) 0.025(3) 0.033(3) 0.009(2) 0.008(2) 0.003(2) C8 0.036(3) 0.045(4) 0.038(3) 0.016(3) 0.010(3) 0.017(3) C9 0.021(3) 0.038(3) 0.032(3) 0.005(3) 0.012(2) -0.001(3) C10 0.013(2) 0.027(3) 0.033(3) 0.004(2) 0.010(2) 0.002(2) C11 0.016(3) 0.033(3) 0.030(3) 0.000(2) 0.007(2) 0.005(2) C12 0.011(2) 0.026(3) 0.035(3) 0.007(2) 0.008(2) 0.003(2) C13 0.025(3) 0.028(3) 0.048(3) 0.007(3) 0.012(3) 0.007(3) Li1 0.015(4) 0.029(5) 0.041(5) 0.007(4) 0.013(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co1 O1 1.921(3) . ? Co1 N3 2.018(4) . ? Co1 N1 2.023(4) . ? Co1 P1 2.3629(18) . ? Co1 Li1 3.113(9) 2_656 ? Co1 Li1 3.157(9) . ? P1 C2 1.808(7) . ? P1 C3 1.810(6) . ? P1 C1 1.813(6) . ? F1 C4 1.345(6) . ? F2 C4 1.326(6) . ? F3 C4 1.338(6) . ? F4 C8 1.317(6) . ? F4B C8 1.313(7) . ? F5 C8 1.307(6) . ? F5B C8 1.300(7) . ? F6 C8 1.334(6) . ? F6B C8 1.305(7) . ? F7 C9 1.341(6) . ? F8 C9 1.333(7) . ? F9 C9 1.344(7) . ? F10 C13 1.330(7) . ? F11 C13 1.329(7) . ? F12 C13 1.335(7) . ? O1 Li1 1.904(10) . ? O1 Li1 2.007(10) 2_656 ? O1 H1 1.0000 . ? N1 N2 1.360(6) . ? N1 C5 1.361(6) . ? N2 C7 1.346(7) . ? N2 Li1 2.047(10) . ? N3 C10 1.353(7) . ? N3 N4 1.363(6) . ? N4 C12 1.341(7) . ? N4 Li1 2.067(10) 2_656 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.492(7) . ? C5 C6 1.377(8) . ? C6 C7 1.398(7) . ? C6 H6 0.9500 . ? C7 C8 1.482(8) . ? C9 C10 1.500(8) . ? C10 C11 1.361(8) . ? C11 C12 1.400(7) . ? C11 H11 0.9500 . ? C12 C13 1.493(8) . ? 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 O1 Co1 N3 99.53(16) . . ? O1 Co1 N1 98.80(17) . . ? N3 Co1 N1 117.23(18) . . ? O1 Co1 P1 109.95(12) . . ? N3 Co1 P1 120.99(13) . . ? N1 Co1 P1 107.42(13) . . ? O1 Co1 Li1 38.6(2) . 2_656 ? N3 Co1 Li1 65.4(2) . 2_656 ? N1 Co1 Li1 98.3(2) . 2_656 ? P1 Co1 Li1 143.09(18) . 2_656 ? O1 Co1 Li1 34.2(2) . . ? N3 Co1 Li1 112.1(2) . . ? N1 Co1 Li1 64.7(2) . . ? P1 Co1 Li1 121.15(18) . . ? Li1 Co1 Li1 48.9(3) 2_656 . ? C2 P1 C3 103.9(4) . . ? C2 P1 C1 103.6(4) . . ? C3 P1 C1 103.3(3) . . ? C2 P1 Co1 106.4(2) . . ? C3 P1 Co1 121.0(2) . . ? C1 P1 Co1 116.6(3) . . ? Li1 O1 Co1 111.3(3) . . ? Li1 O1 Li1 83.0(4) . 2_656 ? Co1 O1 Li1 104.8(3) . 2_656 ? Li1 O1 H1 117.4 . . ? Co1 O1 H1 117.4 . . ? Li1 O1 H1 117.4 2_656 . ? N2 N1 C5 107.5(4) . . ? N2 N1 Co1 115.0(3) . . ? C5 N1 Co1 137.3(4) . . ? C7 N2 N1 107.1(4) . . ? C7 N2 Li1 134.9(4) . . ? N1 N2 Li1 117.4(4) . . ? C10 N3 N4 108.3(4) . . ? C10 N3 Co1 140.4(4) . . ? N4 N3 Co1 111.2(3) . . ? C12 N4 N3 106.3(4) . . ? C12 N4 Li1 131.8(4) . 2_656 ? N3 N4 Li1 115.2(4) . 2_656 ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? F2 C4 F3 107.5(4) . . ? F2 C4 F1 106.6(4) . . ? F3 C4 F1 106.1(4) . . ? F2 C4 C5 111.7(4) . . ? F3 C4 C5 112.3(4) . . ? F1 C4 C5 112.1(4) . . ? N1 C5 C6 111.2(5) . . ? N1 C5 C4 121.0(5) . . ? C6 C5 C4 127.7(5) . . ? C5 C6 C7 102.6(5) . . ? C5 C6 H6 128.7 . . ? C7 C6 H6 128.7 . . ? N2 C7 C6 111.5(5) . . ? N2 C7 C8 120.1(5) . . ? C6 C7 C8 128.4(5) . . ? F5B C8 F6B 107.2(7) . . ? F5B C8 F4B 107.4(7) . . ? F6B C8 F4B 105.8(7) . . ? F5 C8 F4 106.7(5) . . ? F5 C8 F6 105.2(6) . . ? F4 C8 F6 103.6(5) . . ? F5B C8 C7 113.0(8) . . ? F6B C8 C7 112.4(7) . . ? F5 C8 C7 114.2(5) . . ? F4B C8 C7 110.7(8) . . ? F4 C8 C7 113.2(5) . . ? F6 C8 C7 113.0(5) . . ? F8 C9 F7 108.3(4) . . ? F8 C9 F9 107.7(5) . . ? F7 C9 F9 104.9(5) . . ? F8 C9 C10 111.0(5) . . ? F7 C9 C10 112.1(5) . . ? F9 C9 C10 112.5(5) . . ? N3 C10 C11 110.8(5) . . ? N3 C10 C9 120.2(5) . . ? C11 C10 C9 128.7(5) . . ? C10 C11 C12 103.1(5) . . ? C10 C11 H11 128.4 . . ? C12 C11 H11 128.4 . . ? N4 C12 C11 111.4(5) . . ? N4 C12 C13 119.5(5) . . ? C11 C12 C13 129.1(5) . . ? F11 C13 F10 106.3(5) . . ? F11 C13 F12 106.4(5) . . ? F10 C13 F12 107.1(5) . . ? F11 C13 C12 112.6(5) . . ? F10 C13 C12 112.5(5) . . ? F12 C13 C12 111.5(5) . . ? O1 Li1 O1 97.0(4) . 2_656 ? O1 Li1 N2 97.3(4) . . ? O1 Li1 N2 107.4(4) 2_656 . ? O1 Li1 N4 123.8(5) . 2_656 ? O1 Li1 N4 97.3(4) 2_656 2_656 ? N2 Li1 N4 128.8(5) . 2_656 ? O1 Li1 Li1 50.2(3) . 2_656 ? O1 Li1 Li1 46.8(3) 2_656 2_656 ? N2 Li1 Li1 108.9(5) . 2_656 ? N4 Li1 Li1 120.4(5) 2_656 2_656 ? O1 Li1 Co1 107.6(4) . 2_656 ? O1 Li1 Co1 36.62(18) 2_656 2_656 ? N2 Li1 Co1 137.1(4) . 2_656 ? N4 Li1 Co1 62.0(2) 2_656 2_656 ? Li1 Li1 Co1 66.5(4) 2_656 2_656 ? O1 Li1 Co1 34.54(19) . . ? O1 Li1 Co1 103.2(3) 2_656 . ? N2 Li1 Co1 62.9(3) . . ? N4 Li1 Co1 151.5(4) 2_656 . ? Li1 Li1 Co1 64.7(4) 2_656 . ? Co1 Li1 Co1 131.1(3) 2_656 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 P1 C2 60.8(3) . . . . ? N3 Co1 P1 C2 175.9(3) . . . . ? N1 Co1 P1 C2 -45.7(3) . . . . ? Li1 Co1 P1 C2 86.4(4) 2_656 . . . ? Li1 Co1 P1 C2 24.8(4) . . . . ? O1 Co1 P1 C3 178.8(3) . . . . ? N3 Co1 P1 C3 -66.1(3) . . . . ? N1 Co1 P1 C3 72.3(3) . . . . ? Li1 Co1 P1 C3 -155.6(4) 2_656 . . . ? Li1 Co1 P1 C3 142.8(3) . . . . ? O1 Co1 P1 C1 -54.2(3) . . . . ? N3 Co1 P1 C1 60.9(3) . . . . ? N1 Co1 P1 C1 -160.7(3) . . . . ? Li1 Co1 P1 C1 -28.6(4) 2_656 . . . ? Li1 Co1 P1 C1 -90.2(3) . . . . ? N3 Co1 O1 Li1 115.5(4) . . . . ? N1 Co1 O1 Li1 -4.2(4) . . . . ? P1 Co1 O1 Li1 -116.4(3) . . . . ? Li1 Co1 O1 Li1 88.2(5) 2_656 . . . ? N3 Co1 O1 Li1 27.3(3) . . . 2_656 ? N1 Co1 O1 Li1 -92.4(3) . . . 2_656 ? P1 Co1 O1 Li1 155.4(3) . . . 2_656 ? Li1 Co1 O1 Li1 -88.2(5) . . . 2_656 ? O1 Co1 N1 N2 0.5(4) . . . . ? N3 Co1 N1 N2 -105.1(4) . . . . ? P1 Co1 N1 N2 114.7(3) . . . . ? Li1 Co1 N1 N2 -38.5(4) 2_656 . . . ? Li1 Co1 N1 N2 -2.1(3) . . . . ? O1 Co1 N1 C5 174.7(5) . . . . ? N3 Co1 N1 C5 69.2(6) . . . . ? P1 Co1 N1 C5 -71.0(5) . . . . ? Li1 Co1 N1 C5 135.7(5) 2_656 . . . ? Li1 Co1 N1 C5 172.1(6) . . . . ? C5 N1 N2 C7 -0.4(6) . . . . ? Co1 N1 N2 C7 175.5(3) . . . . ? C5 N1 N2 Li1 -172.6(4) . . . . ? Co1 N1 N2 Li1 3.3(5) . . . . ? O1 Co1 N3 C10 147.4(6) . . . . ? N1 Co1 N3 C10 -107.5(6) . . . . ? P1 Co1 N3 C10 27.1(6) . . . . ? Li1 Co1 N3 C10 165.7(6) 2_656 . . . ? Li1 Co1 N3 C10 -179.5(6) . . . . ? O1 Co1 N3 N4 -36.7(3) . . . . ? N1 Co1 N3 N4 68.4(4) . . . . ? P1 Co1 N3 N4 -157.0(3) . . . . ? Li1 Co1 N3 N4 -18.4(3) 2_656 . . . ? Li1 Co1 N3 N4 -3.5(4) . . . . ? C10 N3 N4 C12 0.5(5) . . . . ? Co1 N3 N4 C12 -176.8(3) . . . . ? C10 N3 N4 Li1 -154.3(4) . . . 2_656 ? Co1 N3 N4 Li1 28.4(5) . . . 2_656 ? N2 N1 C5 C6 0.5(6) . . . . ? Co1 N1 C5 C6 -174.1(4) . . . . ? N2 N1 C5 C4 -176.0(4) . . . . ? Co1 N1 C5 C4 9.5(8) . . . . ? F2 C4 C5 N1 -148.0(5) . . . . ? F3 C4 C5 N1 -27.0(7) . . . . ? F1 C4 C5 N1 92.4(6) . . . . ? F2 C4 C5 C6 36.2(8) . . . . ? F3 C4 C5 C6 157.2(5) . . . . ? F1 C4 C5 C6 -83.4(7) . . . . ? N1 C5 C6 C7 -0.3(6) . . . . ? C4 C5 C6 C7 175.8(5) . . . . ? N1 N2 C7 C6 0.3(6) . . . . ? Li1 N2 C7 C6 170.4(5) . . . . ? N1 N2 C7 C8 179.1(4) . . . . ? Li1 N2 C7 C8 -10.7(9) . . . . ? C5 C6 C7 N2 0.0(6) . . . . ? C5 C6 C7 C8 -178.7(5) . . . . ? N2 C7 C8 F5B 73.2(11) . . . . ? C6 C7 C8 F5B -108.1(11) . . . . ? N2 C7 C8 F6B -48.3(10) . . . . ? C6 C7 C8 F6B 130.4(10) . . . . ? N2 C7 C8 F5 -92.6(8) . . . . ? C6 C7 C8 F5 86.0(9) . . . . ? N2 C7 C8 F4B -166.4(10) . . . . ? C6 C7 C8 F4B 12.3(11) . . . . ? N2 C7 C8 F4 144.9(6) . . . . ? C6 C7 C8 F4 -36.4(8) . . . . ? N2 C7 C8 F6 27.5(8) . . . . ? C6 C7 C8 F6 -153.8(7) . . . . ? N4 N3 C10 C11 -0.1(6) . . . . ? Co1 N3 C10 C11 175.9(4) . . . . ? N4 N3 C10 C9 174.7(5) . . . . ? Co1 N3 C10 C9 -9.3(9) . . . . ? F8 C9 C10 N3 176.4(5) . . . . ? F7 C9 C10 N3 55.1(7) . . . . ? F9 C9 C10 N3 -62.9(7) . . . . ? F8 C9 C10 C11 -9.9(8) . . . . ? F7 C9 C10 C11 -131.2(6) . . . . ? F9 C9 C10 C11 110.9(6) . . . . ? N3 C10 C11 C12 -0.3(6) . . . . ? C9 C10 C11 C12 -174.5(6) . . . . ? N3 N4 C12 C11 -0.7(6) . . . . ? Li1 N4 C12 C11 148.1(5) 2_656 . . . ? N3 N4 C12 C13 178.0(5) . . . . ? Li1 N4 C12 C13 -33.2(8) 2_656 . . . ? C10 C11 C12 N4 0.7(6) . . . . ? C10 C11 C12 C13 -177.9(5) . . . . ? N4 C12 C13 F11 -84.2(6) . . . . ? C11 C12 C13 F11 94.3(7) . . . . ? N4 C12 C13 F10 35.9(7) . . . . ? C11 C12 C13 F10 -145.7(6) . . . . ? N4 C12 C13 F12 156.3(5) . . . . ? C11 C12 C13 F12 -25.3(8) . . . . ? Co1 O1 Li1 O1 -103.2(3) . . . 2_656 ? Li1 O1 Li1 O1 0.0 2_656 . . 2_656 ? Co1 O1 Li1 N2 5.4(5) . . . . ? Li1 O1 Li1 N2 108.6(5) 2_656 . . . ? Co1 O1 Li1 N4 153.2(4) . . . 2_656 ? Li1 O1 Li1 N4 -103.6(6) 2_656 . . 2_656 ? Co1 O1 Li1 Li1 -103.2(3) . . . 2_656 ? Co1 O1 Li1 Co1 -139.2(2) . . . 2_656 ? Li1 O1 Li1 Co1 -36.0(2) 2_656 . . 2_656 ? Li1 O1 Li1 Co1 103.2(3) 2_656 . . . ? C7 N2 Li1 O1 -175.0(5) . . . . ? N1 N2 Li1 O1 -5.6(6) . . . . ? C7 N2 Li1 O1 -75.3(7) . . . 2_656 ? N1 N2 Li1 O1 94.1(5) . . . 2_656 ? C7 N2 Li1 N4 39.7(10) . . . 2_656 ? N1 N2 Li1 N4 -151.0(6) . . . 2_656 ? C7 N2 Li1 Li1 -124.7(7) . . . 2_656 ? N1 N2 Li1 Li1 44.7(8) . . . 2_656 ? C7 N2 Li1 Co1 -49.2(9) . . . 2_656 ? N1 N2 Li1 Co1 120.1(6) . . . 2_656 ? C7 N2 Li1 Co1 -171.5(6) . . . . ? N1 N2 Li1 Co1 -2.2(4) . . . . ? N3 Co1 Li1 O1 -73.8(4) . . . . ? N1 Co1 Li1 O1 175.4(4) . . . . ? P1 Co1 Li1 O1 79.6(3) . . . . ? Li1 Co1 Li1 O1 -55.8(4) 2_656 . . . ? O1 Co1 Li1 O1 83.0(4) . . . 2_656 ? N3 Co1 Li1 O1 9.2(4) . . . 2_656 ? N1 Co1 Li1 O1 -101.6(4) . . . 2_656 ? P1 Co1 Li1 O1 162.6(2) . . . 2_656 ? Li1 Co1 Li1 O1 27.2(2) 2_656 . . 2_656 ? O1 Co1 Li1 N2 -174.0(5) . . . . ? N3 Co1 Li1 N2 112.2(3) . . . . ? N1 Co1 Li1 N2 1.4(2) . . . . ? P1 Co1 Li1 N2 -94.4(3) . . . . ? Li1 Co1 Li1 N2 130.2(6) 2_656 . . . ? O1 Co1 Li1 N4 -51.8(8) . . . 2_656 ? N3 Co1 Li1 N4 -125.6(8) . . . 2_656 ? N1 Co1 Li1 N4 123.6(9) . . . 2_656 ? P1 Co1 Li1 N4 27.8(9) . . . 2_656 ? Li1 Co1 Li1 N4 -107.6(10) 2_656 . . 2_656 ? O1 Co1 Li1 Li1 55.8(4) . . . 2_656 ? N3 Co1 Li1 Li1 -18.0(5) . . . 2_656 ? N1 Co1 Li1 Li1 -128.7(5) . . . 2_656 ? P1 Co1 Li1 Li1 135.4(3) . . . 2_656 ? O1 Co1 Li1 Co1 55.8(4) . . . 2_656 ? N3 Co1 Li1 Co1 -18.0(5) . . . 2_656 ? N1 Co1 Li1 Co1 -128.7(5) . . . 2_656 ? P1 Co1 Li1 Co1 135.4(3) . . . 2_656 ? Li1 Co1 Li1 Co1 0.0 2_656 . . 2_656 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.675 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.117 data_CoOPME3Pz2 _database_code_depnum_ccdc_archive 'CCDC 887460' #TrackingRef '6 Co(OPMe3)2Pz2 (6).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(trimethylphosphine-oxide)-bis(3,5-bis(trifluoromethyl)pyrazolate)cobalt(ii) ; _chemical_name_common ;bis(trimethylphosphine-oxide)-bis(3,5- bis(trifluoromethyl)pyrazolate)cobalt(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H20 Co F12 N4 O2 P2' _chemical_formula_sum 'C16 H20 Co F12 N4 O2 P2' _chemical_formula_weight 649.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1321(13) _cell_length_b 10.2434(13) _cell_length_c 13.9848(17) _cell_angle_alpha 99.582(3) _cell_angle_beta 104.265(4) _cell_angle_gamma 101.473(4) _cell_volume 1342.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9159 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.77 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.523 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCX-Mini with Mercury CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4713 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4713 _reflns_number_gt 3468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+4.2924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4713 _refine_ls_number_parameters 399 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.2012 _refine_ls_goodness_of_fit_ref 1.271 _refine_ls_restrained_S_all 1.295 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.89684(10) 0.20526(10) 0.29742(8) 0.0376(3) Uani 1 1 d . . . P1 P 0.5604(2) 0.1880(2) 0.25680(18) 0.0488(6) Uani 1 1 d . . . P2 P 1.0870(2) 0.2462(2) 0.53578(17) 0.0499(6) Uani 1 1 d . . . F1 F 0.7969(13) 0.2552(9) 0.0945(11) 0.067(4) Uani 0.57 1 d PDU A 1 F1B F 0.8947(19) 0.4043(19) 0.0125(9) 0.114(6) Uani 0.43 1 d PDU A 2 F2 F 0.8119(14) 0.4590(12) 0.0734(10) 0.127(5) Uani 0.57 1 d PDU A 1 F2B F 0.7800(16) 0.4194(17) 0.1203(11) 0.123(7) Uani 0.43 1 d PDU A 2 F3 F 0.9371(13) 0.3402(13) 0.0179(7) 0.091(4) Uani 0.57 1 d PDU A 1 F3B F 0.8358(19) 0.2350(9) 0.0771(16) 0.066(5) Uani 0.43 1 d PDU A 2 F4 F 1.4238(12) 0.6490(16) 0.3133(11) 0.098(4) Uani 0.55 1 d PU A 1 F4B F 1.373(2) 0.729(2) 0.3246(17) 0.117(5) Uani 0.45 1 d PU A 2 F5 F 1.3145(16) 0.7553(13) 0.3995(15) 0.099(4) Uani 0.55 1 d PU A 1 F5B F 1.422(2) 0.576(3) 0.4114(19) 0.092(6) Uani 0.45 1 d PU A 2 F6 F 1.398(2) 0.598(2) 0.4477(14) 0.105(6) Uani 0.55 1 d PU A 1 F6B F 1.3052(19) 0.7050(19) 0.4534(14) 0.100(5) Uani 0.45 1 d PU A 2 F7 F 1.0908(7) 0.1151(8) 0.1113(6) 0.112(3) Uani 1 1 d U . . F8 F 1.1548(6) 0.0832(7) 0.2564(5) 0.093(2) Uani 1 1 d U . . F9 F 1.1427(7) -0.0707(8) 0.1301(7) 0.135(3) Uani 1 1 d U . . F10 F 0.6091(7) -0.3750(7) 0.1693(5) 0.100(2) Uani 1 1 d . . . F11 F 0.5868(7) -0.3731(6) 0.0142(5) 0.104(2) Uani 1 1 d . . . F12 F 0.4850(6) -0.2568(7) 0.0967(6) 0.108(2) Uani 1 1 d . . . O1 O 0.7165(5) 0.2491(5) 0.2896(5) 0.0527(15) Uani 1 1 d . . . O2 O 0.9766(6) 0.1937(6) 0.4363(4) 0.0550(15) Uani 1 1 d . . . N1 N 1.0199(6) 0.3601(6) 0.2675(5) 0.0438(15) Uani 1 1 d . . . N2 N 1.1405(7) 0.4312(7) 0.3399(5) 0.0475(16) Uani 1 1 d . . . N3 N 0.8615(6) 0.0217(6) 0.2091(5) 0.0397(15) Uani 1 1 d . . . N4 N 0.7326(6) -0.0630(6) 0.1944(5) 0.0433(15) Uani 1 1 d . . . C1 C 0.8869(10) 0.3707(8) 0.0981(7) 0.078(3) Uani 1 1 d DU . . C2 C 1.0056(9) 0.4224(8) 0.1892(6) 0.051(2) Uani 1 1 d . A . C3 C 1.1202(10) 0.5355(10) 0.2088(7) 0.063(2) Uani 1 1 d . . . H3 H 1.1398 0.5971 0.1673 0.076 Uiso 1 1 calc R A . C4 C 1.1969(8) 0.5332(8) 0.3050(7) 0.049(2) Uani 1 1 d . A . C5 C 1.3283(11) 0.6351(11) 0.3670(9) 0.073(3) Uani 1 1 d U . . C6 C 1.0773(10) 0.0189(11) 0.1633(8) 0.066(3) Uani 1 1 d U . . C7 C 0.9337(8) -0.0451(8) 0.1582(6) 0.0446(19) Uani 1 1 d . . . C8 C 0.8519(9) -0.1736(8) 0.1067(6) 0.050(2) Uani 1 1 d . . . H8 H 0.8755 -0.2425 0.0645 0.061 Uiso 1 1 calc R . . C9 C 0.7285(8) -0.1782(8) 0.1311(6) 0.0452(19) Uani 1 1 d . . . C10 C 0.6039(11) -0.2944(10) 0.1043(8) 0.069(3) Uani 1 1 d . . . C11 C 0.4914(10) 0.1129(11) 0.1258(7) 0.069(3) Uani 1 1 d . . . H11A H 0.4992 0.1843 0.0874 0.104 Uiso 1 1 calc R . . H11B H 0.3923 0.0648 0.1108 0.104 Uiso 1 1 calc R . . H11C H 0.5446 0.0478 0.1066 0.104 Uiso 1 1 calc R . . C12 C 0.5128(10) 0.0606(11) 0.3236(8) 0.068(3) Uani 1 1 d . . . H12A H 0.5502 -0.0178 0.3044 0.102 Uiso 1 1 calc R . . H12B H 0.4100 0.0308 0.3064 0.102 Uiso 1 1 calc R . . H12C H 0.5519 0.0989 0.3967 0.102 Uiso 1 1 calc R . . C13 C 0.4743(10) 0.3185(10) 0.2839(10) 0.081(3) Uani 1 1 d . . . H13A H 0.5092 0.3615 0.3564 0.121 Uiso 1 1 calc R . . H13B H 0.3727 0.2786 0.2653 0.121 Uiso 1 1 calc R . . H13C H 0.4936 0.3875 0.2449 0.121 Uiso 1 1 calc R . . C14 C 1.2423(11) 0.1980(15) 0.5272(12) 0.130(6) Uani 1 1 d . . . H14A H 1.2305 0.1009 0.5277 0.195 Uiso 1 1 calc R . . H14B H 1.3212 0.2527 0.5851 0.195 Uiso 1 1 calc R . . H14C H 1.2613 0.2138 0.4642 0.195 Uiso 1 1 calc R . . C15 C 1.1264(13) 0.4254(10) 0.5814(8) 0.080(3) Uani 1 1 d . . . H15A H 1.1644 0.4715 0.5343 0.120 Uiso 1 1 calc R . . H15B H 1.1962 0.4518 0.6482 0.120 Uiso 1 1 calc R . . H15C H 1.0405 0.4522 0.5869 0.120 Uiso 1 1 calc R . . C16 C 1.0263(14) 0.1729(12) 0.6284(8) 0.091(4) Uani 1 1 d . . . H16A H 0.9340 0.1892 0.6278 0.136 Uiso 1 1 calc R . . H16B H 1.0932 0.2148 0.6954 0.136 Uiso 1 1 calc R . . H16C H 1.0182 0.0742 0.6130 0.136 Uiso 1 1 calc R . . 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 0.0257(5) 0.0365(5) 0.0410(6) 0.0038(4) 0.0036(4) -0.0018(4) P1 0.0274(11) 0.0534(13) 0.0612(14) 0.0104(11) 0.0078(10) 0.0085(9) P2 0.0435(13) 0.0472(12) 0.0440(12) 0.0004(10) -0.0040(10) 0.0063(10) F1 0.042(7) 0.087(7) 0.051(6) 0.018(6) 0.005(5) -0.020(5) F1B 0.108(11) 0.131(11) 0.062(8) 0.061(8) -0.030(8) -0.029(9) F2 0.132(9) 0.095(8) 0.099(10) 0.016(7) -0.070(8) 0.043(7) F2B 0.122(11) 0.113(11) 0.081(11) 0.013(9) -0.067(9) 0.038(9) F3 0.099(9) 0.107(9) 0.049(6) 0.034(6) -0.006(6) 0.005(7) F3B 0.041(9) 0.078(8) 0.061(9) 0.000(7) 0.006(7) -0.002(6) F4 0.044(6) 0.110(9) 0.115(8) -0.001(8) 0.032(6) -0.028(6) F4B 0.096(10) 0.086(9) 0.117(10) 0.014(9) 0.003(9) -0.050(8) F5 0.076(7) 0.051(7) 0.135(11) -0.023(7) 0.013(8) -0.005(6) F5B 0.050(8) 0.080(8) 0.113(12) -0.024(9) -0.008(8) 0.016(6) F6 0.072(9) 0.091(9) 0.099(10) 0.003(8) -0.023(8) -0.025(8) F6B 0.076(8) 0.079(10) 0.100(10) -0.031(8) 0.008(8) -0.015(8) F7 0.082(5) 0.132(6) 0.120(6) 0.048(5) 0.048(4) -0.022(4) F8 0.036(3) 0.127(5) 0.084(4) -0.007(4) 0.009(3) -0.012(3) F9 0.064(4) 0.106(5) 0.220(9) -0.042(5) 0.077(5) 0.009(4) F10 0.091(5) 0.076(4) 0.114(5) 0.046(4) 0.007(4) -0.013(4) F11 0.108(5) 0.065(4) 0.088(5) -0.015(3) 0.004(4) -0.033(4) F12 0.038(3) 0.091(4) 0.163(7) 0.024(5) 0.001(4) -0.017(3) O1 0.026(3) 0.050(3) 0.074(4) 0.002(3) 0.012(3) 0.005(2) O2 0.047(3) 0.056(3) 0.043(3) 0.009(3) -0.006(3) -0.005(3) N1 0.030(3) 0.046(4) 0.045(4) 0.004(3) 0.005(3) -0.003(3) N2 0.035(4) 0.045(4) 0.053(4) 0.002(3) 0.008(3) 0.003(3) N3 0.027(3) 0.040(3) 0.040(3) 0.000(3) -0.001(3) 0.002(3) N4 0.028(3) 0.039(3) 0.056(4) 0.012(3) 0.006(3) -0.002(3) C1 0.072(6) 0.094(6) 0.053(5) 0.023(5) -0.003(5) 0.008(5) C2 0.049(5) 0.047(5) 0.046(5) 0.011(4) 0.006(4) -0.004(4) C3 0.063(6) 0.060(6) 0.058(6) 0.025(5) 0.012(5) -0.006(5) C4 0.036(4) 0.044(4) 0.060(5) 0.015(4) 0.013(4) -0.007(4) C5 0.053(5) 0.059(5) 0.089(6) 0.013(5) 0.010(5) -0.010(4) C6 0.050(6) 0.069(6) 0.072(6) -0.004(5) 0.025(5) 0.006(5) C7 0.038(4) 0.052(5) 0.035(4) 0.002(4) 0.007(3) 0.004(4) C8 0.052(5) 0.046(5) 0.045(5) -0.001(4) 0.010(4) 0.008(4) C9 0.041(5) 0.040(4) 0.041(4) 0.009(4) -0.002(4) -0.003(4) C10 0.052(6) 0.050(5) 0.074(7) 0.007(5) -0.009(5) -0.016(5) C11 0.047(6) 0.086(7) 0.060(6) 0.015(5) -0.009(5) 0.015(5) C12 0.050(6) 0.085(7) 0.068(6) 0.016(5) 0.020(5) 0.008(5) C13 0.046(6) 0.066(6) 0.129(10) 0.015(6) 0.017(6) 0.027(5) C14 0.038(6) 0.141(12) 0.159(13) -0.046(10) -0.017(7) 0.028(7) C15 0.098(9) 0.059(6) 0.063(6) 0.007(5) 0.013(6) -0.011(6) C16 0.112(10) 0.087(8) 0.057(6) 0.032(6) -0.006(6) 0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co1 O2 1.944(5) . ? Co1 O1 1.949(5) . ? Co1 N3 1.983(6) . ? Co1 N1 1.984(6) . ? P1 O1 1.502(5) . ? P1 C11 1.767(9) . ? P1 C13 1.775(9) . ? P1 C12 1.785(10) . ? P2 O2 1.490(6) . ? P2 C14 1.765(11) . ? P2 C15 1.769(10) . ? P2 C16 1.775(11) . ? F1 C1 1.327(8) . ? F1B C1 1.315(8) . ? F2 C1 1.328(8) . ? F2B C1 1.359(9) . ? F3 C1 1.357(8) . ? F3B C1 1.337(9) . ? F4 C5 1.364(17) . ? F4B C5 1.27(2) . ? F5 C5 1.287(17) . ? F5B C5 1.31(3) . ? F6 C5 1.33(2) . ? F6B C5 1.40(2) . ? F7 C6 1.323(12) . ? F8 C6 1.323(11) . ? F9 C6 1.321(11) . ? F10 C10 1.325(11) . ? F11 C10 1.329(12) . ? F12 C10 1.321(12) . ? N1 C2 1.348(10) . ? N1 N2 1.356(9) . ? N2 C4 1.314(10) . ? N3 C7 1.343(9) . ? N3 N4 1.363(8) . ? N4 C9 1.339(10) . ? C1 C2 1.455(13) . ? C2 C3 1.403(12) . ? C3 C4 1.385(12) . ? C3 H3 0.9500 . ? C4 C5 1.480(12) . ? C6 C7 1.451(12) . ? C7 C8 1.376(11) . ? C8 C9 1.368(11) . ? C8 H8 0.9500 . ? C9 C10 1.474(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 O2 Co1 O1 107.0(3) . . ? O2 Co1 N3 107.7(3) . . ? O1 Co1 N3 108.3(2) . . ? O2 Co1 N1 108.9(2) . . ? O1 Co1 N1 107.3(3) . . ? N3 Co1 N1 117.1(3) . . ? O1 P1 C11 113.5(4) . . ? O1 P1 C13 109.1(4) . . ? C11 P1 C13 107.3(5) . . ? O1 P1 C12 111.6(4) . . ? C11 P1 C12 107.7(5) . . ? C13 P1 C12 107.4(5) . . ? O2 P2 C14 109.7(5) . . ? O2 P2 C15 114.1(5) . . ? C14 P2 C15 109.4(6) . . ? O2 P2 C16 108.9(5) . . ? C14 P2 C16 108.7(7) . . ? C15 P2 C16 105.9(5) . . ? P1 O1 Co1 143.2(4) . . ? P2 O2 Co1 150.6(4) . . ? C2 N1 N2 108.0(6) . . ? C2 N1 Co1 133.2(5) . . ? N2 N1 Co1 118.5(5) . . ? C4 N2 N1 106.8(7) . . ? C7 N3 N4 108.7(6) . . ? C7 N3 Co1 136.3(5) . . ? N4 N3 Co1 115.0(5) . . ? C9 N4 N3 105.6(6) . . ? F1 C1 F2 107.2(8) . . ? F1B C1 F3B 107.1(9) . . ? F1 C1 F3 104.3(7) . . ? F2 C1 F3 104.0(7) . . ? F1B C1 F2B 105.1(8) . . ? F3B C1 F2B 103.2(8) . . ? F1B C1 C2 120.6(10) . . ? F1 C1 C2 116.2(9) . . ? F2 C1 C2 115.5(9) . . ? F3B C1 C2 113.5(12) . . ? F3 C1 C2 108.4(9) . . ? F2B C1 C2 105.6(10) . . ? N1 C2 C3 110.5(8) . . ? N1 C2 C1 121.9(7) . . ? C3 C2 C1 127.5(8) . . ? C4 C3 C2 101.1(7) . . ? C4 C3 H3 129.5 . . ? C2 C3 H3 129.5 . . ? N2 C4 C3 113.6(7) . . ? N2 C4 C5 121.1(8) . . ? C3 C4 C5 125.2(8) . . ? F4B C5 F5 63.1(13) . . ? F4B C5 F5B 116.1(19) . . ? F5 C5 F5B 126.8(15) . . ? F4B C5 F6 128.4(15) . . ? F5 C5 F6 106.1(15) . . ? F4B C5 F4 47.2(12) . . ? F5 C5 F4 107.4(13) . . ? F6 C5 F4 102.0(14) . . ? F4B C5 F6B 104.5(16) . . ? F5B C5 F6B 98.4(16) . . ? F4B C5 C4 115.2(12) . . ? F5 C5 C4 115.5(11) . . ? F5B C5 C4 111.5(14) . . ? F6 C5 C4 114.5(12) . . ? F4 C5 C4 110.2(10) . . ? F6B C5 C4 109.3(11) . . ? F9 C6 F8 106.8(9) . . ? F9 C6 F7 106.0(9) . . ? F8 C6 F7 103.2(8) . . ? F9 C6 C7 112.2(8) . . ? F8 C6 C7 112.8(8) . . ? F7 C6 C7 115.1(9) . . ? N3 C7 C8 110.0(7) . . ? N3 C7 C6 120.7(7) . . ? C8 C7 C6 129.3(8) . . ? C9 C8 C7 103.4(7) . . ? C9 C8 H8 128.3 . . ? C7 C8 H8 128.3 . . ? N4 C9 C8 112.4(7) . . ? N4 C9 C10 118.9(8) . . ? C8 C9 C10 128.5(8) . . ? F12 C10 F10 106.0(9) . . ? F12 C10 F11 105.2(8) . . ? F10 C10 F11 106.7(8) . . ? F12 C10 C9 113.4(8) . . ? F10 C10 C9 114.1(8) . . ? F11 C10 C9 110.9(9) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C14 H14A 109.5 . . ? P2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P2 C15 H15A 109.5 . . ? P2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 P1 O1 Co1 -61.3(8) . . . . ? C13 P1 O1 Co1 179.1(7) . . . . ? C12 P1 O1 Co1 60.6(8) . . . . ? O2 Co1 O1 P1 -100.6(7) . . . . ? N3 Co1 O1 P1 15.3(7) . . . . ? N1 Co1 O1 P1 142.6(6) . . . . ? C14 P2 O2 Co1 -76.6(10) . . . . ? C15 P2 O2 Co1 46.5(10) . . . . ? C16 P2 O2 Co1 164.5(8) . . . . ? O1 Co1 O2 P2 -114.1(8) . . . . ? N3 Co1 O2 P2 129.6(8) . . . . ? N1 Co1 O2 P2 1.6(9) . . . . ? O2 Co1 N1 C2 -170.6(7) . . . . ? O1 Co1 N1 C2 -55.1(8) . . . . ? N3 Co1 N1 C2 66.9(8) . . . . ? O2 Co1 N1 N2 3.0(6) . . . . ? O1 Co1 N1 N2 118.5(5) . . . . ? N3 Co1 N1 N2 -119.5(5) . . . . ? C2 N1 N2 C4 -0.3(9) . . . . ? Co1 N1 N2 C4 -175.4(5) . . . . ? O2 Co1 N3 C7 -90.4(8) . . . . ? O1 Co1 N3 C7 154.2(7) . . . . ? N1 Co1 N3 C7 32.8(8) . . . . ? O2 Co1 N3 N4 89.0(5) . . . . ? O1 Co1 N3 N4 -26.4(6) . . . . ? N1 Co1 N3 N4 -147.9(5) . . . . ? C7 N3 N4 C9 -2.3(8) . . . . ? Co1 N3 N4 C9 178.1(5) . . . . ? N2 N1 C2 C3 1.2(10) . . . . ? Co1 N1 C2 C3 175.3(6) . . . . ? N2 N1 C2 C1 179.4(7) . . . . ? Co1 N1 C2 C1 -6.5(13) . . . . ? F1B C1 C2 N1 -159.0(11) . . . . ? F1 C1 C2 N1 -3.0(13) . . . . ? F2 C1 C2 N1 123.9(10) . . . . ? F3B C1 C2 N1 -29.9(13) . . . . ? F3 C1 C2 N1 -119.9(9) . . . . ? F2B C1 C2 N1 82.4(11) . . . . ? F1B C1 C2 C3 18.9(15) . . . . ? F1 C1 C2 C3 174.9(10) . . . . ? F2 C1 C2 C3 -58.2(13) . . . . ? F3B C1 C2 C3 148.0(11) . . . . ? F3 C1 C2 C3 58.0(12) . . . . ? F2B C1 C2 C3 -99.7(12) . . . . ? N1 C2 C3 C4 -1.5(10) . . . . ? C1 C2 C3 C4 -179.6(9) . . . . ? N1 N2 C4 C3 -0.7(10) . . . . ? N1 N2 C4 C5 177.8(8) . . . . ? C2 C3 C4 N2 1.4(11) . . . . ? C2 C3 C4 C5 -177.0(9) . . . . ? N2 C4 C5 F4B 179.7(17) . . . . ? C3 C4 C5 F4B -2(2) . . . . ? N2 C4 C5 F5 -109.5(15) . . . . ? C3 C4 C5 F5 68.8(18) . . . . ? N2 C4 C5 F5B 44.7(18) . . . . ? C3 C4 C5 F5B -137.0(16) . . . . ? N2 C4 C5 F6 14.2(17) . . . . ? C3 C4 C5 F6 -167.5(14) . . . . ? N2 C4 C5 F4 128.5(12) . . . . ? C3 C4 C5 F4 -53.2(16) . . . . ? N2 C4 C5 F6B -62.9(16) . . . . ? C3 C4 C5 F6B 115.4(15) . . . . ? N4 N3 C7 C8 1.7(9) . . . . ? Co1 N3 C7 C8 -178.9(6) . . . . ? N4 N3 C7 C6 -177.6(8) . . . . ? Co1 N3 C7 C6 1.7(13) . . . . ? F9 C6 C7 N3 164.5(9) . . . . ? F8 C6 C7 N3 43.9(13) . . . . ? F7 C6 C7 N3 -74.1(11) . . . . ? F9 C6 C7 C8 -14.7(15) . . . . ? F8 C6 C7 C8 -135.4(10) . . . . ? F7 C6 C7 C8 106.6(11) . . . . ? N3 C7 C8 C9 -0.4(9) . . . . ? C6 C7 C8 C9 178.9(9) . . . . ? N3 N4 C9 C8 2.2(9) . . . . ? N3 N4 C9 C10 176.8(7) . . . . ? C7 C8 C9 N4 -1.1(10) . . . . ? C7 C8 C9 C10 -175.1(9) . . . . ? N4 C9 C10 F12 35.5(12) . . . . ? C8 C9 C10 F12 -150.9(9) . . . . ? N4 C9 C10 F10 -86.0(11) . . . . ? C8 C9 C10 F10 87.6(12) . . . . ? N4 C9 C10 F11 153.6(8) . . . . ? C8 C9 C10 F11 -32.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.581 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.108