# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hani Amouri' _publ_contact_author_email HANI.AMOURI@UPMC.FR _publ_section_title ; A Unique type of a Dicobalt Cage Templated by weakly Coordinated Hexafluorophosphate Anion: Design, Structure and Solid-State NMR Investigations. ; _publ_author_name 'Hani Amouri' # Attachment '2009_amouri_Dalton.cif' #=============================================================================== data_cd047 _database_code_depnum_ccdc_archive 'CCDC 725319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H110 Co2 N18 O8, 4(F6 P), C2 H3 N' _chemical_formula_sum 'C110 H113 Co2 F24 N19 O8 P4' _chemical_formula_weight 2526.93 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' 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' 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' _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 14.301(1) _cell_length_b 15.560(1) _cell_length_c 26.631(1) _cell_angle_alpha 89.288(1) _cell_angle_beta 86.027(1) _cell_angle_gamma 70.023(1) _cell_volume 5555.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 18232 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description coin _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9131 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60290 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.35 _reflns_number_total 20326 _reflns_number_gt 13618 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. One highly disordered PF6- molecule was accounted for using the Platon SQUEEZE function. No model was found to explain the disorder. The very large ellipsoids for P1 and P2 could be explain by a disorder on the PF6- position, but no good model can be found. The short contact H17C..H43B can be explain by the rotation of the two CH3 fragment (C17 et C43). The best solution of the refinement give a short distance between two hydrogen atoms. The high value of wR2 can be explain by the weak intensity of the diffraction for high theta. The diffraction were measured up to 25\^A\%. # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.153 0.913 0.221 160.8 35.0 2 0.000 0.500 0.500 40.4 9.7 3 -0.153 0.087 0.779 160.8 36.2 4 0.278 0.751 0.715 10.7 2.6 5 0.443 0.830 0.022 28.3 2.8 6 0.472 0.528 0.394 19.6 0.3 7 0.528 0.472 0.606 19.6 -0.3 8 0.557 0.170 0.978 28.3 2.4 9 0.722 0.249 0.285 10.7 3.0 _platon_squeeze_details ; _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^)+(0.1849P)^2^+2.3249P] 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 SHELXL _refine_ls_extinction_coef 0.0016(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 20326 _refine_ls_number_parameters 1464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2828 _refine_ls_wR_factor_gt 0.2628 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.109 _refine_ls_shift/su_mean 0.002 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 0.53993(5) -0.01919(5) 0.63547(2) 0.0423(2) Uani 1 1 d . . . P1 P 0.5000 0.0000 0.5000 0.229(4) Uani 1 2 d S . . F1 F 0.5142(4) -0.0058(3) 0.54623(14) 0.0929(14) Uani 1 1 d . . . F2 F 0.3827(5) 0.0740(4) 0.51233(19) 0.1273(19) Uani 1 1 d . . . F3 F 0.5520(5) 0.0817(4) 0.4959(2) 0.1166(17) Uani 1 1 d . . . O1 O 0.8743(3) 0.0412(3) 0.45784(16) 0.0590(10) Uani 1 1 d . . . O2 O 0.5976(3) 0.3821(3) 0.49801(18) 0.0675(12) Uani 1 1 d . . . O3 O 0.0077(3) 0.2510(4) 0.5645(2) 0.0922(16) Uani 1 1 d . . . O4 O 0.3245(3) 0.3643(3) 0.5114(2) 0.0827(15) Uani 1 1 d . . . N1 N 0.6808(3) -0.0118(3) 0.61664(15) 0.0437(10) Uani 1 1 d . . . N2 N 0.7961(3) 0.0444(3) 0.58602(15) 0.0450(10) Uani 1 1 d . . . N3 N 0.3977(3) -0.0266(3) 0.64512(14) 0.0418(10) Uani 1 1 d . . . N4 N 0.2729(3) -0.0804(3) 0.63815(14) 0.0432(10) Uani 1 1 d . . . N5 N 0.4804(3) 0.1235(3) 0.63878(15) 0.0456(10) Uani 1 1 d . . . N6 N 0.3721(4) 0.2617(3) 0.62899(15) 0.0501(11) Uani 1 1 d . . . N7 N 0.2961(3) 0.2925(3) 0.40820(15) 0.0486(11) Uani 1 1 d . . . N8 N 0.5977(3) -0.1593(3) 0.62271(15) 0.0420(10) Uani 1 1 d . . . N106 N 0.5663(3) -0.0339(3) 0.71364(17) 0.0480(10) Uani 1 1 d . . . C1 C 0.7002(4) 0.0495(4) 0.58767(18) 0.0429(12) Uani 1 1 d . . . H1 H 0.6512 0.0934 0.5696 0.052 Uiso 1 1 calc R . . C2 C 0.7738(4) -0.0634(4) 0.63511(19) 0.0455(12) Uani 1 1 d . . . C3 C 0.8001(4) -0.1389(4) 0.6668(2) 0.0478(12) Uani 1 1 d . . . H3 H 0.7518 -0.1637 0.6805 0.057 Uiso 1 1 calc R . . C4 C 0.8972(4) -0.1755(4) 0.6774(2) 0.0601(15) Uani 1 1 d . . . H4 H 0.9169 -0.2266 0.6991 0.072 Uiso 1 1 calc R . . C5 C 0.9687(5) -0.1399(5) 0.6572(2) 0.0665(17) Uani 1 1 d . . . H5 H 1.0361 -0.1672 0.6653 0.080 Uiso 1 1 calc R . . C6 C 0.9432(4) -0.0661(5) 0.6260(2) 0.0605(16) Uani 1 1 d . . . H6 H 0.9917 -0.0420 0.6118 0.073 Uiso 1 1 calc R . . C7 C 0.8442(4) -0.0283(4) 0.61585(19) 0.0477(13) Uani 1 1 d . . . C8 C 0.8435(4) 0.1025(4) 0.5588(2) 0.0556(14) Uani 1 1 d . . . H8A H 0.9089 0.0633 0.5434 0.067 Uiso 1 1 calc R . . H8B H 0.8560 0.1441 0.5833 0.067 Uiso 1 1 calc R . . C9 C 0.7835(4) 0.1592(4) 0.51819(18) 0.0447(12) Uani 1 1 d . . . C10 C 0.8019(4) 0.1250(3) 0.46890(18) 0.0435(12) Uani 1 1 d . . . C11 C 0.7533(4) 0.1766(4) 0.42934(18) 0.0446(12) Uani 1 1 d . . . C12 C 0.6847(4) 0.2639(4) 0.4382(2) 0.0468(13) Uani 1 1 d . . . C13 C 0.6656(4) 0.2978(4) 0.4878(2) 0.0459(12) Uani 1 1 d . . . C14 C 0.8423(5) -0.0371(4) 0.4626(2) 0.0603(15) Uani 1 1 d . . . H14A H 0.8843 -0.0812 0.4855 0.091 Uiso 1 1 calc R . . H14B H 0.8482 -0.0658 0.4295 0.091 Uiso 1 1 calc R . . H14C H 0.7726 -0.0174 0.4761 0.091 Uiso 1 1 calc R . . C15 C 0.6273(5) 0.3228(5) 0.3981(3) 0.0676(18) Uani 1 1 d . . . H15A H 0.6714 0.3469 0.3771 0.101 Uiso 1 1 calc R . . H15B H 0.5721 0.3737 0.4138 0.101 Uiso 1 1 calc R . . H15C H 0.6007 0.2864 0.3772 0.101 Uiso 1 1 calc R . . C16 C 0.6425(5) 0.4533(4) 0.4927(3) 0.082(2) Uani 1 1 d . . . H16A H 0.6825 0.4515 0.5213 0.122 Uiso 1 1 calc R . . H16B H 0.5898 0.5133 0.4917 0.122 Uiso 1 1 calc R . . H16C H 0.6853 0.4430 0.4614 0.122 Uiso 1 1 calc R . . C17 C 0.6841(5) 0.2839(5) 0.5804(2) 0.0671(17) Uani 1 1 d . . . H17A H 0.6935 0.2343 0.6047 0.101 Uiso 1 1 calc R . . H17B H 0.6139 0.3235 0.5826 0.101 Uiso 1 1 calc R . . H17C H 0.7259 0.3198 0.5881 0.101 Uiso 1 1 calc R . . C18 C 0.3653(4) -0.0823(4) 0.62026(17) 0.0423(12) Uani 1 1 d . . . H18 H 0.4024 -0.1198 0.5928 0.051 Uiso 1 1 calc R . . C19 C 0.3229(4) 0.0145(4) 0.68267(18) 0.0431(12) Uani 1 1 d . . . C20 C 0.3167(4) 0.0771(4) 0.72043(18) 0.0467(12) Uani 1 1 d . . . H20 H 0.3690 0.1008 0.7240 0.056 Uiso 1 1 calc R . . C21 C 0.2320(5) 0.1037(4) 0.7524(2) 0.0578(15) Uani 1 1 d . . . H21 H 0.2272 0.1455 0.7790 0.069 Uiso 1 1 calc R . . C22 C 0.1531(4) 0.0723(4) 0.7477(2) 0.0539(14) Uani 1 1 d . . . H22 H 0.0959 0.0933 0.7707 0.065 Uiso 1 1 calc R . . C23 C 0.1565(4) 0.0110(4) 0.71003(19) 0.0501(13) Uani 1 1 d . . . H23 H 0.1024 -0.0101 0.7059 0.060 Uiso 1 1 calc R . . C24 C 0.2435(4) -0.0186(3) 0.67823(17) 0.0413(11) Uani 1 1 d . . . C25 C 0.7808(4) 0.1389(4) 0.37582(19) 0.0545(14) Uani 1 1 d . . . H25A H 0.7672 0.1908 0.3522 0.065 Uiso 1 1 calc R . . H25B H 0.8532 0.1040 0.3722 0.065 Uiso 1 1 calc R . . C26 C 0.3977(4) 0.1732(4) 0.61859(19) 0.0476(13) Uani 1 1 d . . . H26 H 0.3604 0.1482 0.5987 0.057 Uiso 1 1 calc R . . C27 C 0.5097(4) 0.1851(4) 0.66541(17) 0.0419(11) Uani 1 1 d . . . C28 C 0.5940(4) 0.1719(4) 0.69365(19) 0.0516(14) Uani 1 1 d . . . H28 H 0.6416 0.1129 0.6983 0.062 Uiso 1 1 calc R . . C29 C 0.6027(5) 0.2489(4) 0.7138(2) 0.0555(14) Uani 1 1 d . . . H29 H 0.6573 0.2425 0.7336 0.067 Uiso 1 1 calc R . . C30 C 0.5352(5) 0.3366(4) 0.7066(2) 0.0572(15) Uani 1 1 d . . . H30 H 0.5463 0.3875 0.7210 0.069 Uiso 1 1 calc R . . C31 C 0.4534(5) 0.3512(4) 0.67945(19) 0.0546(14) Uani 1 1 d . . . H31 H 0.4072 0.4108 0.6747 0.066 Uiso 1 1 calc R . . C32 C 0.4416(4) 0.2725(4) 0.65888(18) 0.0487(13) Uani 1 1 d . . . C33 C 0.2858(6) 0.3380(5) 0.6148(3) 0.081(2) Uani 1 1 d . . . H33A H 0.3087 0.3882 0.6025 0.097 Uiso 1 1 calc R . . H33B H 0.2404 0.3607 0.6453 0.097 Uiso 1 1 calc R . . C34 C 0.2277(5) 0.3153(4) 0.5749(2) 0.0544(14) Uani 1 1 d . . . C35 C 0.2484(4) 0.3332(4) 0.5256(2) 0.0521(13) Uani 1 1 d . . . C36 C 0.1887(4) 0.3260(4) 0.48827(19) 0.0510(13) Uani 1 1 d . . . C37 C 0.1083(4) 0.2952(4) 0.4998(2) 0.0563(15) Uani 1 1 d . . . C38 C 0.0893(4) 0.2783(4) 0.5502(2) 0.0565(15) Uani 1 1 d . . . C39 C 0.1482(5) 0.2864(4) 0.5880(2) 0.0540(14) Uani 1 1 d . . . C40 C 0.4213(4) 0.2971(5) 0.5074(3) 0.0664(17) Uani 1 1 d . . . H40A H 0.4578 0.3028 0.5363 0.100 Uiso 1 1 calc R . . H40B H 0.4572 0.3060 0.4762 0.100 Uiso 1 1 calc R . . H40C H 0.4158 0.2360 0.5070 0.100 Uiso 1 1 calc R . . C41 C 0.2082(6) 0.3575(5) 0.4360(2) 0.078(2) Uani 1 1 d . . . H41A H 0.1488 0.3666 0.4168 0.094 Uiso 1 1 calc R . . H41B H 0.2180 0.4172 0.4386 0.094 Uiso 1 1 calc R . . C42 C 0.0441(6) 0.2796(6) 0.4613(3) 0.090(2) Uani 1 1 d . . . H42A H 0.0084 0.2401 0.4753 0.134 Uiso 1 1 calc R . . H42B H 0.0861 0.2500 0.4314 0.134 Uiso 1 1 calc R . . H42C H -0.0040 0.3384 0.4519 0.134 Uiso 1 1 calc R . . C43 C -0.0817(6) 0.3270(7) 0.5745(5) 0.139(4) Uani 1 1 d . . . H43A H -0.0669 0.3746 0.5928 0.209 Uiso 1 1 calc R . . H43B H -0.1301 0.3071 0.5950 0.209 Uiso 1 1 calc R . . H43C H -0.1098 0.3516 0.5427 0.209 Uiso 1 1 calc R . . C44 C 0.1221(7) 0.2674(6) 0.6413(3) 0.101(3) Uani 1 1 d . . . H44A H 0.0855 0.3252 0.6590 0.152 Uiso 1 1 calc R . . H44B H 0.1833 0.2357 0.6580 0.152 Uiso 1 1 calc R . . H44C H 0.0803 0.2288 0.6418 0.152 Uiso 1 1 calc R . . C45 C 0.6703(4) -0.2003(4) 0.58894(19) 0.0485(13) Uani 1 1 d . . . H45 H 0.6969 -0.1680 0.5647 0.058 Uiso 1 1 calc R . . C46 C 0.5828(4) -0.2318(3) 0.65136(17) 0.0401(11) Uani 1 1 d . . . C47 C 0.5186(4) -0.2294(4) 0.69335(19) 0.0453(12) Uani 1 1 d . . . H47 H 0.4748 -0.1734 0.7078 0.054 Uiso 1 1 calc R . . C48 C 0.5220(4) -0.3119(4) 0.7126(2) 0.0537(14) Uani 1 1 d . . . H48 H 0.4795 -0.3128 0.7415 0.064 Uiso 1 1 calc R . . C49 C 0.5848(4) -0.3951(4) 0.6918(2) 0.0521(13) Uani 1 1 d . . . H49 H 0.5831 -0.4504 0.7066 0.063 Uiso 1 1 calc R . . C50 C 0.3528(4) 0.3135(4) 0.36889(18) 0.0444(12) Uani 1 1 d . . . C51 C 0.6493(4) -0.3987(4) 0.65028(19) 0.0485(13) Uani 1 1 d . . . H51 H 0.6922 -0.4550 0.6356 0.058 Uiso 1 1 calc R . . C52 C 0.7130(4) 0.2446(4) 0.5287(2) 0.0481(13) Uani 1 1 d . . . C106 C 0.5975(4) -0.0544(4) 0.7516(2) 0.0483(13) Uani 1 1 d . . . C107 C 0.6400(5) -0.0853(5) 0.7997(2) 0.074(2) Uani 1 1 d . . . H10A H 0.6318 -0.1438 0.8084 0.111 Uiso 1 1 calc R . . H10B H 0.6056 -0.0397 0.8260 0.111 Uiso 1 1 calc R . . H10C H 0.7111 -0.0930 0.7970 0.111 Uiso 1 1 calc R . . Co2 Co 0.98546(4) 0.67925(4) -0.08794(2) 0.02821(19) Uani 1 1 d . . . P2 P 1.0000 0.5000 0.0000 0.300(6) Uani 1 2 d S . . F4 F 0.9931(4) 0.5620(3) -0.02958(15) 0.0731(12) Uani 1 1 d . . . F5 F 0.9095(4) 0.4734(4) -0.0286(2) 0.1194(18) Uani 1 1 d . . . F6 F 0.9100(4) 0.5736(4) 0.03997(19) 0.1152(16) Uani 1 1 d . . . O5 O 0.5966(2) 0.7971(2) 0.12551(13) 0.0460(8) Uani 1 1 d . . . O6 O 0.9895(2) 0.7183(3) 0.16595(12) 0.0466(9) Uani 1 1 d . . . O7 O 0.5842(2) 0.5997(2) 0.02403(13) 0.0452(8) Uani 1 1 d . . . O8 O 0.6940(3) 0.3710(3) -0.14165(14) 0.0532(10) Uani 1 1 d . . . N9 N 0.9946(3) 0.7610(2) -0.02771(13) 0.0297(8) Uani 1 1 d . . . N10 N 0.9577(3) 0.8307(2) 0.04705(12) 0.0287(8) Uani 1 1 d . . . N11 N 0.8296(3) 0.7239(2) -0.07544(13) 0.0306(8) Uani 1 1 d . . . N12 N 0.6758(3) 0.7166(2) -0.07009(14) 0.0316(8) Uani 1 1 d . . . N13 N 0.7026(2) 0.4072(2) 0.07258(13) 0.0300(8) Uani 1 1 d . . . N14 N 1.1435(2) 0.6226(2) -0.09622(12) 0.0280(8) Uani 1 1 d . . . N15 N 0.9793(3) 0.5856(2) -0.14298(13) 0.0296(8) Uani 1 1 d . . . N16 N 0.9587(3) 0.5334(2) 0.19468(12) 0.0314(8) Uani 1 1 d . . . N108 N 0.9901(3) 0.7772(3) -0.14363(15) 0.0361(9) Uani 1 1 d . . . C53 C 0.9403(3) 0.7723(3) 0.01501(16) 0.0298(9) Uani 1 1 d . . . H53 H 0.8933 0.7424 0.0226 0.036 Uiso 1 1 calc R . . C54 C 1.0523(3) 0.8179(3) -0.02391(15) 0.0278(9) Uani 1 1 d . . . C55 C 1.1234(3) 0.8338(3) -0.05728(16) 0.0332(10) Uani 1 1 d . . . H55 H 1.1401 0.8050 -0.0895 0.040 Uiso 1 1 calc R . . C56 C 1.1688(3) 0.8933(3) -0.04175(18) 0.0364(10) Uani 1 1 d . . . H56 H 1.2175 0.9057 -0.0639 0.044 Uiso 1 1 calc R . . C57 C 1.1450(3) 0.9354(3) 0.00545(18) 0.0376(11) Uani 1 1 d . . . H57 H 1.1781 0.9759 0.0145 0.045 Uiso 1 1 calc R . . C58 C 1.0755(3) 0.9206(3) 0.03953(17) 0.0352(10) Uani 1 1 d . . . H58 H 1.0600 0.9490 0.0719 0.042 Uiso 1 1 calc R . . C59 C 1.0288(3) 0.8607(3) 0.02329(16) 0.0290(9) Uani 1 1 d . . . C60 C 0.9091(4) 0.8623(3) 0.09808(16) 0.0355(10) Uani 1 1 d . . . H60A H 0.8646 0.9267 0.0962 0.043 Uiso 1 1 calc R . . H60B H 0.9612 0.8601 0.1212 0.043 Uiso 1 1 calc R . . C61 C 0.8497(3) 0.8057(3) 0.11925(15) 0.0315(10) Uani 1 1 d . . . C62 C 0.7511(3) 0.8244(3) 0.10933(15) 0.0322(10) Uani 1 1 d . . . C63 C 0.6957(3) 0.7755(3) 0.13472(16) 0.0359(10) Uani 1 1 d . . . C64 C 0.7381(4) 0.7068(3) 0.16835(16) 0.0371(11) Uani 1 1 d . . . C65 C 0.8387(4) 0.6865(3) 0.17759(16) 0.0355(10) Uani 1 1 d . . . C66 C 0.8931(3) 0.7355(3) 0.15268(15) 0.0335(10) Uani 1 1 d . . . C67 C 0.6994(4) 0.8983(3) 0.07314(18) 0.0426(12) Uani 1 1 d . . . H67A H 0.6598 0.9539 0.0921 0.064 Uiso 1 1 calc R . . H67B H 0.6554 0.8774 0.0536 0.064 Uiso 1 1 calc R . . H67C H 0.7494 0.9113 0.0503 0.064 Uiso 1 1 calc R . . C68 C 0.5302(4) 0.8587(4) 0.1629(2) 0.0572(15) Uani 1 1 d . . . H68A H 0.5380 0.8295 0.1959 0.086 Uiso 1 1 calc R . . H68B H 0.4611 0.8734 0.1539 0.086 Uiso 1 1 calc R . . H68C H 0.5462 0.9150 0.1642 0.086 Uiso 1 1 calc R . . C69 C 0.6764(4) 0.6544(4) 0.1937(2) 0.0526(13) Uani 1 1 d . . . H69A H 0.6445 0.6849 0.2255 0.079 Uiso 1 1 calc R . . H69B H 0.7197 0.5919 0.2003 0.079 Uiso 1 1 calc R . . H69C H 0.6250 0.6527 0.1716 0.079 Uiso 1 1 calc R . . C70 C 0.8886(4) 0.6195(3) 0.21679(17) 0.0429(12) Uani 1 1 d . . . H70A H 0.9251 0.6476 0.2378 0.051 Uiso 1 1 calc R . . H70B H 0.8370 0.6060 0.2390 0.051 Uiso 1 1 calc R . . C71 C 1.0461(3) 0.5053(3) -0.15063(15) 0.0290(9) Uani 1 1 d . . . H71 H 1.0940 0.4764 -0.1272 0.035 Uiso 1 1 calc R . . C72 C 1.0377(3) 0.4716(3) 0.21816(16) 0.0346(10) Uani 1 1 d . . . C73 C 1.0761(4) 0.4781(4) 0.26379(19) 0.0495(13) Uani 1 1 d . . . H73 H 1.0491 0.5301 0.2854 0.059 Uiso 1 1 calc R . . C74 C 1.1577(5) 0.4023(4) 0.2755(2) 0.0590(16) Uani 1 1 d . . . H74 H 1.1865 0.4019 0.3066 0.071 Uiso 1 1 calc R . . C75 C 1.0226(4) 0.8131(4) -0.1735(2) 0.0463(12) Uani 1 1 d . . . C76 C 1.1980(4) 0.3279(4) 0.2433(2) 0.0502(14) Uani 1 1 d . . . H76 H 1.2553 0.2792 0.2524 0.060 Uiso 1 1 calc R . . C77 C 1.1575(3) 0.3217(3) 0.19816(18) 0.0385(11) Uani 1 1 d . . . H77 H 1.1834 0.2690 0.1770 0.046 Uiso 1 1 calc R . . C78 C 0.9233(3) 0.6027(3) -0.18555(16) 0.0310(10) Uani 1 1 d . . . C79 C 0.7753(3) 0.6695(3) -0.07411(15) 0.0300(9) Uani 1 1 d . . . H79 H 0.8030 0.6046 -0.0758 0.036 Uiso 1 1 calc R . . C80 C 0.7603(3) 0.8129(3) -0.07261(15) 0.0285(9) Uani 1 1 d . . . C81 C 0.7735(3) 0.8974(3) -0.07417(16) 0.0353(10) Uani 1 1 d . . . H81 H 0.8383 0.9018 -0.0780 0.042 Uiso 1 1 calc R . . C82 C 0.6901(4) 0.9739(3) -0.07000(18) 0.0381(11) Uani 1 1 d . . . H82 H 0.6969 1.0325 -0.0713 0.046 Uiso 1 1 calc R . . C83 C 0.5943(4) 0.9674(3) -0.06384(18) 0.0428(12) Uani 1 1 d . . . H83 H 0.5384 1.0222 -0.0599 0.051 Uiso 1 1 calc R . . C84 C 0.5783(3) 0.8861(3) -0.06323(17) 0.0368(10) Uani 1 1 d . . . H84 H 0.5133 0.8824 -0.0596 0.044 Uiso 1 1 calc R . . C85 C 0.6641(3) 0.8087(3) -0.06833(16) 0.0316(10) Uani 1 1 d . . . C86 C 0.5930(3) 0.6815(3) -0.0701(2) 0.0412(12) Uani 1 1 d . . . H86A H 0.5593 0.6996 -0.1018 0.049 Uiso 1 1 calc R . . H86B H 0.5439 0.7105 -0.0419 0.049 Uiso 1 1 calc R . . C87 C 0.6242(3) 0.5787(3) -0.06525(18) 0.0351(10) Uani 1 1 d . . . C88 C 0.6181(3) 0.5428(3) -0.01761(18) 0.0365(11) Uani 1 1 d . . . C89 C 0.6349(3) 0.4503(3) -0.01102(17) 0.0331(10) Uani 1 1 d . . . C90 C 0.6617(3) 0.3913(3) -0.05256(18) 0.0366(11) Uani 1 1 d . . . C91 C 0.6671(3) 0.4282(3) -0.10002(17) 0.0378(11) Uani 1 1 d . . . C92 C 0.6508(3) 0.5214(3) -0.10715(18) 0.0366(11) Uani 1 1 d . . . C93 C 0.6632(4) 0.5557(4) -0.15927(19) 0.0513(13) Uani 1 1 d . . . H93A H 0.6041 0.6084 -0.1659 0.077 Uiso 1 1 calc R . . H93B H 0.6713 0.5070 -0.1839 0.077 Uiso 1 1 calc R . . H93C H 0.7223 0.5742 -0.1620 0.077 Uiso 1 1 calc R . . C94 C 0.6580(4) 0.6283(4) 0.0466(2) 0.0487(13) Uani 1 1 d . . . H94A H 0.7249 0.5897 0.0337 0.073 Uiso 1 1 calc R . . H94B H 0.6515 0.6224 0.0833 0.073 Uiso 1 1 calc R . . H94C H 0.6477 0.6923 0.0382 0.073 Uiso 1 1 calc R . . C95 C 0.6195(3) 0.4162(4) 0.04063(18) 0.0402(11) Uani 1 1 d . . . H95A H 0.5571 0.4588 0.0572 0.048 Uiso 1 1 calc R . . H95B H 0.6113 0.3558 0.0376 0.048 Uiso 1 1 calc R . . C96 C 0.6866(4) 0.2885(3) -0.0468(2) 0.0518(14) Uani 1 1 d . . . H96A H 0.6247 0.2744 -0.0433 0.078 Uiso 1 1 calc R . . H96B H 0.7240 0.2682 -0.0168 0.078 Uiso 1 1 calc R . . H96C H 0.7271 0.2568 -0.0766 0.078 Uiso 1 1 calc R . . C97 C 0.6120(5) 0.3452(4) -0.1585(3) 0.0669(18) Uani 1 1 d . . . H97A H 0.5692 0.3393 -0.1292 0.100 Uiso 1 1 calc R . . H97B H 0.6390 0.2866 -0.1767 0.100 Uiso 1 1 calc R . . H97C H 0.5727 0.3923 -0.1808 0.100 Uiso 1 1 calc R . . C98 C 1.2002(3) 0.6134(3) -0.05835(16) 0.0305(9) Uani 1 1 d . . . H98 H 1.1748 0.6206 -0.0242 0.037 Uiso 1 1 calc R . . C99 C 0.6940(3) 0.4117(3) 0.12466(17) 0.0332(10) Uani 1 1 d . . . C100 C 0.6117(4) 0.4306(3) 0.15893(18) 0.0402(11) Uani 1 1 d . . . H100 H 0.5463 0.4440 0.1482 0.048 Uiso 1 1 calc R . . C101 C 0.6290(4) 0.4290(3) 0.20860(19) 0.0429(12) Uani 1 1 d . . . H101 H 0.5742 0.4415 0.2330 0.052 Uiso 1 1 calc R . . C102 C 0.7252(4) 0.4093(3) 0.22479(18) 0.0421(11) Uani 1 1 d . . . H102 H 0.7341 0.4095 0.2598 0.051 Uiso 1 1 calc R . . C103 C 0.8077(4) 0.3896(3) 0.19057(16) 0.0368(10) Uani 1 1 d . . . H103 H 0.8732 0.3749 0.2015 0.044 Uiso 1 1 calc R . . C104 C 1.2089(3) 0.6079(3) -0.13947(15) 0.0295(9) Uani 1 1 d . . . C105 C 1.0705(6) 0.8551(5) -0.2116(3) 0.081(2) Uani 1 1 d . . . H10D H 1.0794 0.9093 -0.1972 0.122 Uiso 1 1 calc R . . H10E H 1.0286 0.8733 -0.2402 0.122 Uiso 1 1 calc R . . H10F H 1.1357 0.8112 -0.2231 0.122 Uiso 1 1 calc R . . C108 C 1.0689(4) 0.6665(4) 0.1296(2) 0.0558(14) Uani 1 1 d . . . H10G H 1.0402 0.6430 0.1028 0.084 Uiso 1 1 calc R . . H10H H 1.1161 0.6152 0.1465 0.084 Uiso 1 1 calc R . . H10I H 1.1037 0.7063 0.1151 0.084 Uiso 1 1 calc R . . P3 P 0.63838(11) 0.14366(11) 0.16448(6) 0.0534(4) Uani 1 1 d . . . F7 F 0.7400(3) 0.0603(3) 0.15458(13) 0.0733(10) Uani 1 1 d . . . F8 F 0.6968(4) 0.2087(3) 0.14938(19) 0.0998(14) Uani 1 1 d . . . F9 F 0.6156(3) 0.1377(3) 0.10795(15) 0.0937(14) Uani 1 1 d . . . F10 F 0.5827(4) 0.0733(4) 0.1780(2) 0.1292(19) Uani 1 1 d . . . F11 F 0.6605(3) 0.1474(4) 0.22072(14) 0.1068(17) Uani 1 1 d . . . F12 F 0.5359(3) 0.2256(3) 0.17367(14) 0.0905(13) Uani 1 1 d . . . P4 P 0.87322(17) 0.41698(16) 0.35143(8) 0.0863(6) Uani 1 1 d . . . F13 F 0.9880(4) 0.3869(4) 0.3594(2) 0.1171(17) Uani 1 1 d . . . F14 F 0.8957(4) 0.3580(4) 0.30297(19) 0.1192(19) Uani 1 1 d . . . F15 F 0.8743(5) 0.5026(4) 0.3192(3) 0.153(3) Uani 1 1 d . . . F16 F 0.8528(4) 0.4720(4) 0.4017(2) 0.1211(17) Uani 1 1 d . . . F17 F 0.8657(4) 0.3309(4) 0.3807(2) 0.1269(18) Uani 1 1 d . . . F18 F 0.7572(3) 0.4498(3) 0.34668(18) 0.1012(14) Uani 1 1 d . . . N150 N 0.2337(9) 0.6128(7) 0.3138(6) 0.175(5) Uani 1 1 d . . . C151 C 0.1815(7) 0.6637(8) 0.2897(4) 0.100(3) Uani 1 1 d . . . C152 C 0.1138(13) 0.7236(12) 0.2648(7) 0.223(10) Uani 1 1 d . . . H15D H 0.0829 0.6919 0.2432 0.335 Uiso 1 1 calc R . . H15E H 0.1451 0.7601 0.2439 0.335 Uiso 1 1 calc R . . H15F H 0.0627 0.7640 0.2886 0.335 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 0.0403(4) 0.0398(4) 0.0489(4) -0.0005(3) -0.0011(3) -0.0169(3) P1 0.305(12) 0.130(5) 0.229(9) -0.010(6) -0.017(8) -0.043(7) F1 0.120(4) 0.105(4) 0.0427(19) 0.003(2) -0.013(2) -0.024(3) F2 0.142(5) 0.107(4) 0.098(3) -0.011(3) -0.003(3) 0.003(4) F3 0.153(5) 0.096(4) 0.113(4) 0.004(3) -0.005(3) -0.058(4) O1 0.047(2) 0.044(2) 0.082(3) 0.0059(19) 0.008(2) -0.0127(19) O2 0.046(2) 0.038(2) 0.119(4) -0.006(2) 0.001(2) -0.0156(19) O3 0.047(3) 0.076(3) 0.152(5) 0.004(3) 0.009(3) -0.023(2) O4 0.046(2) 0.047(3) 0.153(5) 0.004(3) 0.012(3) -0.017(2) N1 0.040(2) 0.045(3) 0.046(2) 0.0063(19) -0.0078(19) -0.013(2) N2 0.042(2) 0.056(3) 0.039(2) 0.0102(19) -0.0015(18) -0.021(2) N3 0.046(2) 0.038(2) 0.041(2) -0.0034(18) 0.0032(19) -0.016(2) N4 0.044(2) 0.054(3) 0.036(2) -0.0050(18) 0.0058(18) -0.024(2) N5 0.049(3) 0.046(3) 0.046(2) 0.0029(19) -0.007(2) -0.021(2) N6 0.065(3) 0.042(3) 0.042(2) -0.0075(19) -0.012(2) -0.014(2) N7 0.053(3) 0.044(3) 0.040(2) 0.0057(19) 0.004(2) -0.006(2) N8 0.041(2) 0.042(2) 0.041(2) 0.0023(18) 0.0034(19) -0.013(2) N106 0.048(3) 0.046(3) 0.053(3) 0.001(2) -0.001(2) -0.021(2) C1 0.040(3) 0.047(3) 0.042(3) 0.006(2) -0.005(2) -0.015(2) C2 0.040(3) 0.048(3) 0.049(3) 0.003(2) -0.004(2) -0.017(2) C3 0.041(3) 0.047(3) 0.055(3) 0.009(2) -0.003(2) -0.015(2) C4 0.053(4) 0.063(4) 0.060(3) 0.022(3) -0.009(3) -0.016(3) C5 0.046(3) 0.080(5) 0.074(4) 0.028(3) -0.024(3) -0.018(3) C6 0.043(3) 0.077(4) 0.066(4) 0.013(3) -0.002(3) -0.026(3) C7 0.043(3) 0.052(3) 0.046(3) 0.006(2) -0.010(2) -0.013(3) C8 0.047(3) 0.068(4) 0.058(3) 0.022(3) -0.006(3) -0.028(3) C9 0.041(3) 0.052(3) 0.045(3) 0.007(2) -0.006(2) -0.022(3) C10 0.046(3) 0.038(3) 0.047(3) 0.001(2) 0.003(2) -0.017(2) C11 0.041(3) 0.057(3) 0.044(3) 0.001(2) -0.002(2) -0.027(3) C12 0.047(3) 0.043(3) 0.057(3) 0.010(2) -0.013(2) -0.024(3) C13 0.039(3) 0.037(3) 0.064(3) -0.004(2) 0.000(2) -0.017(2) C14 0.068(4) 0.048(3) 0.065(4) 0.000(3) 0.007(3) -0.021(3) C15 0.059(4) 0.072(4) 0.084(4) 0.032(3) -0.024(3) -0.035(3) C16 0.050(4) 0.039(4) 0.154(7) -0.009(4) -0.001(4) -0.014(3) C17 0.059(4) 0.087(5) 0.062(4) -0.028(3) 0.014(3) -0.036(4) C18 0.046(3) 0.047(3) 0.034(2) -0.007(2) 0.004(2) -0.017(2) C19 0.046(3) 0.042(3) 0.039(3) -0.001(2) 0.002(2) -0.013(2) C20 0.052(3) 0.045(3) 0.042(3) -0.004(2) 0.001(2) -0.016(3) C21 0.072(4) 0.049(3) 0.044(3) -0.007(2) 0.004(3) -0.012(3) C22 0.052(3) 0.048(3) 0.049(3) 0.001(2) 0.008(3) -0.004(3) C23 0.049(3) 0.058(4) 0.042(3) 0.004(2) 0.007(2) -0.019(3) C24 0.045(3) 0.041(3) 0.035(2) 0.002(2) 0.001(2) -0.011(2) C25 0.054(3) 0.076(4) 0.043(3) -0.006(3) 0.002(2) -0.036(3) C26 0.049(3) 0.049(3) 0.044(3) -0.008(2) -0.009(2) -0.014(3) C27 0.048(3) 0.045(3) 0.036(2) -0.001(2) 0.003(2) -0.020(2) C28 0.059(3) 0.064(4) 0.043(3) 0.001(2) -0.009(2) -0.034(3) C29 0.061(4) 0.066(4) 0.045(3) -0.009(3) -0.006(3) -0.029(3) C30 0.072(4) 0.060(4) 0.047(3) -0.017(3) 0.004(3) -0.035(3) C31 0.075(4) 0.051(3) 0.040(3) -0.007(2) -0.006(3) -0.024(3) C32 0.065(4) 0.046(3) 0.036(3) -0.004(2) -0.001(2) -0.020(3) C33 0.089(5) 0.051(4) 0.095(5) -0.015(3) -0.051(4) -0.004(4) C34 0.062(4) 0.044(3) 0.051(3) -0.002(2) -0.013(3) -0.009(3) C35 0.040(3) 0.039(3) 0.075(4) -0.004(3) 0.002(3) -0.011(2) C36 0.054(3) 0.046(3) 0.044(3) 0.002(2) 0.003(2) -0.006(3) C37 0.051(3) 0.047(3) 0.061(3) -0.008(3) -0.011(3) -0.003(3) C38 0.041(3) 0.044(3) 0.081(4) -0.007(3) 0.017(3) -0.014(3) C39 0.058(4) 0.049(3) 0.043(3) -0.003(2) 0.004(3) -0.004(3) C40 0.042(3) 0.067(4) 0.094(5) 0.005(3) 0.003(3) -0.025(3) C41 0.090(5) 0.056(4) 0.058(4) 0.016(3) 0.020(3) 0.010(4) C42 0.081(5) 0.094(6) 0.086(5) -0.006(4) -0.040(4) -0.013(4) C43 0.046(5) 0.119(8) 0.243(13) -0.047(8) 0.043(6) -0.026(5) C44 0.120(7) 0.093(6) 0.059(4) 0.004(4) 0.027(4) -0.002(5) C45 0.048(3) 0.049(3) 0.046(3) 0.011(2) 0.001(2) -0.015(3) C46 0.038(3) 0.044(3) 0.040(2) -0.002(2) -0.001(2) -0.017(2) C47 0.048(3) 0.046(3) 0.047(3) 0.004(2) 0.001(2) -0.022(3) C48 0.058(4) 0.062(4) 0.045(3) 0.006(3) -0.001(3) -0.026(3) C49 0.056(3) 0.043(3) 0.057(3) 0.011(3) -0.004(3) -0.019(3) C50 0.053(3) 0.042(3) 0.038(2) 0.004(2) -0.008(2) -0.014(3) C51 0.052(3) 0.041(3) 0.050(3) 0.005(2) -0.009(3) -0.012(3) C52 0.046(3) 0.053(3) 0.053(3) -0.006(2) 0.003(2) -0.027(3) C106 0.055(3) 0.041(3) 0.046(3) -0.004(2) -0.004(3) -0.012(3) C107 0.079(5) 0.066(4) 0.054(3) -0.002(3) -0.017(3) 0.008(3) Co2 0.0190(3) 0.0317(4) 0.0341(3) -0.0050(2) -0.0020(2) -0.0087(2) P2 0.270(13) 0.365(19) 0.240(12) -0.059(12) -0.015(10) -0.075(13) F4 0.100(3) 0.060(2) 0.062(2) 0.0356(18) -0.009(2) -0.032(2) F5 0.127(4) 0.135(4) 0.127(4) 0.039(3) -0.051(3) -0.076(4) F6 0.131(4) 0.101(4) 0.098(3) 0.000(3) 0.014(3) -0.023(3) O5 0.0300(18) 0.052(2) 0.051(2) -0.0113(16) 0.0020(15) -0.0089(16) O6 0.0286(17) 0.059(2) 0.0469(19) -0.0040(16) -0.0047(15) -0.0077(16) O7 0.0295(17) 0.049(2) 0.058(2) -0.0178(17) 0.0020(15) -0.0140(16) O8 0.0378(19) 0.059(2) 0.058(2) -0.0192(18) -0.0099(17) -0.0088(17) N9 0.0261(18) 0.032(2) 0.0336(19) -0.0018(15) -0.0020(15) -0.0136(16) N10 0.0254(18) 0.030(2) 0.0317(18) -0.0027(15) 0.0018(15) -0.0105(16) N11 0.0227(18) 0.031(2) 0.0382(19) -0.0050(15) -0.0025(15) -0.0094(16) N12 0.0214(18) 0.030(2) 0.045(2) 0.0009(16) -0.0037(15) -0.0101(15) N13 0.0212(18) 0.033(2) 0.0374(19) 0.0003(15) -0.0045(15) -0.0112(16) N14 0.0224(18) 0.033(2) 0.0287(17) -0.0007(15) 0.0007(14) -0.0099(16) N15 0.0243(18) 0.032(2) 0.0316(18) 0.0015(15) -0.0069(15) -0.0083(16) N16 0.036(2) 0.030(2) 0.0264(17) -0.0005(15) -0.0040(15) -0.0090(17) N108 0.034(2) 0.032(2) 0.042(2) 0.0025(17) -0.0048(17) -0.0102(18) C53 0.025(2) 0.029(2) 0.037(2) -0.0012(18) -0.0003(18) -0.0110(19) C54 0.022(2) 0.029(2) 0.033(2) 0.0013(17) -0.0016(17) -0.0100(18) C55 0.031(2) 0.033(3) 0.036(2) -0.0007(19) -0.0021(19) -0.011(2) C56 0.028(2) 0.040(3) 0.047(3) 0.005(2) -0.002(2) -0.019(2) C57 0.034(3) 0.034(3) 0.051(3) 0.003(2) -0.011(2) -0.019(2) C58 0.040(3) 0.029(2) 0.039(2) -0.0016(19) -0.009(2) -0.014(2) C59 0.025(2) 0.025(2) 0.038(2) 0.0003(18) -0.0069(18) -0.0092(18) C60 0.043(3) 0.032(3) 0.031(2) -0.0035(18) 0.001(2) -0.013(2) C61 0.033(2) 0.030(2) 0.029(2) -0.0087(18) 0.0052(18) -0.009(2) C62 0.034(2) 0.031(2) 0.027(2) -0.0051(18) 0.0045(18) -0.007(2) C63 0.034(3) 0.034(3) 0.036(2) -0.011(2) 0.0033(19) -0.008(2) C64 0.044(3) 0.034(3) 0.033(2) -0.0102(19) 0.010(2) -0.016(2) C65 0.044(3) 0.029(2) 0.031(2) -0.0050(18) 0.003(2) -0.009(2) C66 0.033(2) 0.034(3) 0.030(2) -0.0052(18) 0.0002(18) -0.007(2) C67 0.042(3) 0.037(3) 0.043(3) 0.001(2) -0.006(2) -0.005(2) C68 0.037(3) 0.058(4) 0.068(4) -0.020(3) 0.009(3) -0.007(3) C69 0.062(4) 0.047(3) 0.052(3) -0.004(2) 0.013(3) -0.025(3) C70 0.053(3) 0.039(3) 0.030(2) 0.002(2) 0.003(2) -0.009(2) C71 0.025(2) 0.035(3) 0.029(2) 0.0011(18) -0.0033(17) -0.012(2) C72 0.037(3) 0.038(3) 0.034(2) 0.0037(19) -0.008(2) -0.019(2) C73 0.056(3) 0.052(3) 0.044(3) -0.003(2) -0.015(2) -0.021(3) C74 0.067(4) 0.065(4) 0.048(3) 0.008(3) -0.031(3) -0.022(3) C75 0.037(3) 0.047(3) 0.052(3) 0.005(2) -0.007(2) -0.009(2) C76 0.045(3) 0.051(3) 0.059(3) 0.016(3) -0.023(3) -0.019(3) C77 0.031(2) 0.039(3) 0.046(3) 0.005(2) -0.008(2) -0.011(2) C78 0.028(2) 0.035(3) 0.034(2) 0.0048(19) -0.0065(18) -0.015(2) C79 0.023(2) 0.029(2) 0.037(2) -0.0015(18) -0.0003(18) -0.0087(19) C80 0.022(2) 0.032(2) 0.031(2) -0.0001(17) -0.0022(17) -0.0070(18) C81 0.035(3) 0.035(3) 0.040(2) -0.0029(19) -0.006(2) -0.017(2) C82 0.039(3) 0.027(2) 0.049(3) -0.003(2) -0.010(2) -0.010(2) C83 0.036(3) 0.033(3) 0.053(3) -0.005(2) -0.010(2) -0.003(2) C84 0.024(2) 0.038(3) 0.045(3) 0.001(2) -0.0067(19) -0.006(2) C85 0.032(2) 0.028(2) 0.036(2) -0.0009(18) -0.0048(19) -0.0119(19) C86 0.019(2) 0.030(3) 0.076(3) 0.004(2) -0.009(2) -0.0100(19) C87 0.020(2) 0.035(3) 0.053(3) 0.005(2) -0.010(2) -0.0104(19) C88 0.022(2) 0.036(3) 0.053(3) -0.009(2) -0.009(2) -0.010(2) C89 0.021(2) 0.039(3) 0.043(2) 0.004(2) -0.0111(19) -0.0142(19) C90 0.025(2) 0.036(3) 0.053(3) 0.002(2) -0.012(2) -0.014(2) C91 0.025(2) 0.046(3) 0.042(3) -0.010(2) -0.0072(19) -0.010(2) C92 0.020(2) 0.043(3) 0.047(3) 0.001(2) -0.0072(19) -0.012(2) C93 0.040(3) 0.067(4) 0.050(3) 0.008(3) -0.005(2) -0.022(3) C94 0.054(3) 0.047(3) 0.053(3) -0.009(2) -0.004(2) -0.027(3) C95 0.025(2) 0.049(3) 0.051(3) 0.005(2) -0.009(2) -0.018(2) C96 0.047(3) 0.029(3) 0.079(4) -0.004(2) -0.019(3) -0.009(2) C97 0.056(4) 0.062(4) 0.079(4) -0.031(3) -0.027(3) -0.011(3) C98 0.028(2) 0.031(2) 0.036(2) -0.0002(18) -0.0038(18) -0.0132(19) C99 0.028(2) 0.027(2) 0.042(2) 0.0020(18) 0.0007(19) -0.0065(19) C100 0.030(2) 0.042(3) 0.052(3) -0.001(2) 0.007(2) -0.018(2) C101 0.036(3) 0.040(3) 0.054(3) -0.001(2) 0.018(2) -0.019(2) C102 0.048(3) 0.039(3) 0.038(2) -0.001(2) 0.009(2) -0.014(2) C103 0.037(3) 0.039(3) 0.035(2) 0.000(2) 0.000(2) -0.016(2) C104 0.025(2) 0.030(2) 0.033(2) -0.0015(18) 0.0007(18) -0.0097(18) C105 0.074(5) 0.076(5) 0.088(5) 0.037(4) 0.003(4) -0.021(4) C108 0.033(3) 0.061(4) 0.065(3) 0.004(3) 0.007(3) -0.008(3) P3 0.0467(8) 0.0572(10) 0.0544(8) 0.0019(7) -0.0019(7) -0.0156(7) F7 0.066(2) 0.073(2) 0.064(2) 0.0029(17) 0.0024(17) -0.0032(19) F8 0.102(3) 0.074(3) 0.132(4) -0.015(3) 0.018(3) -0.046(3) F9 0.054(2) 0.139(4) 0.073(2) -0.025(2) -0.0112(18) -0.011(2) F10 0.105(4) 0.118(4) 0.178(5) 0.014(4) 0.030(4) -0.064(3) F11 0.087(3) 0.133(4) 0.059(2) -0.013(2) -0.009(2) 0.018(3) F12 0.068(2) 0.104(3) 0.065(2) 0.001(2) -0.0051(19) 0.017(2) P4 0.0849(15) 0.0827(15) 0.0813(13) 0.0050(11) -0.0042(11) -0.0165(12) F13 0.106(4) 0.136(5) 0.110(4) 0.025(3) -0.021(3) -0.041(3) F14 0.102(4) 0.107(4) 0.113(4) -0.037(3) -0.038(3) 0.016(3) F15 0.135(5) 0.098(4) 0.171(5) 0.044(4) 0.069(4) 0.013(3) F16 0.137(5) 0.113(4) 0.106(4) -0.003(3) -0.025(3) -0.030(3) F17 0.124(4) 0.099(4) 0.153(5) 0.019(3) -0.002(4) -0.033(3) F18 0.081(3) 0.102(3) 0.110(3) -0.011(3) -0.005(2) -0.018(3) N150 0.167(10) 0.097(7) 0.274(15) 0.025(8) -0.095(10) -0.047(7) C151 0.090(6) 0.113(7) 0.116(7) 0.029(6) -0.035(5) -0.055(6) C152 0.223(17) 0.239(18) 0.270(19) 0.153(16) -0.152(16) -0.138(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 N8 2.074(4) . ? Co1 N3 2.075(4) . ? Co1 N1 2.083(4) . ? Co1 N5 2.089(4) . ? Co1 N106 2.137(5) . ? P1 F1 1.259(4) 2_656 ? P1 F1 1.259(4) . ? P1 F3 1.677(5) 2_656 ? P1 F3 1.677(5) . ? P1 F2 1.691(6) . ? P1 F2 1.691(6) 2_656 ? O1 C10 1.380(6) . ? O1 C14 1.441(7) . ? O2 C13 1.357(7) . ? O2 C16 1.460(7) . ? O3 C38 1.400(7) . ? O3 C43 1.426(10) . ? O4 C35 1.364(7) . ? O4 C40 1.420(7) . ? N1 C1 1.310(6) . ? N1 C2 1.416(6) . ? N2 C1 1.344(6) . ? N2 C7 1.380(7) . ? N2 C8 1.462(7) . ? N3 C18 1.317(6) . ? N3 C19 1.397(7) . ? N4 C18 1.363(7) . ? N4 C24 1.388(6) . ? N4 C25 1.444(7) 2_656 ? N5 C26 1.318(7) . ? N5 C27 1.389(6) . ? N6 C26 1.327(7) . ? N6 C32 1.370(7) . ? N6 C33 1.458(8) . ? N7 C45 1.352(7) 2_656 ? N7 C50 1.383(7) . ? N7 C41 1.474(8) . ? N8 C45 1.315(7) . ? N8 C46 1.421(6) . ? N106 C106 1.132(6) . ? C1 H1 0.9500 . ? C2 C7 1.369(7) . ? C2 C3 1.396(7) . ? C3 C4 1.357(8) . ? C3 H3 0.9500 . ? C4 C5 1.394(8) . ? C4 H4 0.9500 . ? C5 C6 1.370(8) . ? C5 H5 0.9500 . ? C6 C7 1.379(8) . ? C6 H6 0.9500 . ? C8 C9 1.507(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C52 1.384(8) . ? C9 C10 1.396(7) . ? C10 C11 1.391(7) . ? C11 C12 1.389(8) . ? C11 C25 1.521(7) . ? C12 C13 1.404(8) . ? C12 C15 1.496(7) . ? C13 C52 1.423(8) . ? 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 . ? C17 C52 1.487(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18 0.9500 . ? C19 C20 1.387(7) . ? C19 C24 1.409(7) . ? C20 C21 1.374(8) . ? C20 H20 0.9500 . ? C21 C22 1.389(9) . ? C21 H21 0.9500 . ? C22 C23 1.379(8) . ? C22 H22 0.9500 . ? C23 C24 1.397(7) . ? C23 H23 0.9500 . ? C25 N4 1.444(7) 2_656 ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26 0.9500 . ? C27 C32 1.393(8) . ? C27 C28 1.420(7) . ? C28 C29 1.366(8) . ? C28 H28 0.9500 . ? C29 C30 1.396(9) . ? C29 H29 0.9500 . ? C30 C31 1.369(8) . ? C30 H30 0.9500 . ? C31 C32 1.414(7) . ? C31 H31 0.9500 . ? C33 C34 1.508(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.371(8) . ? C34 C39 1.381(9) . ? C35 C36 1.384(8) . ? C36 C37 1.403(9) . ? C36 C41 1.508(8) . ? C37 C38 1.391(9) . ? C37 C42 1.499(8) . ? C38 C39 1.390(8) . ? C39 C44 1.495(9) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? 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 N7 1.352(7) 2_656 ? C45 H45 0.9500 . ? C46 C50 1.380(7) 2_656 ? C46 C47 1.390(7) . ? C47 C48 1.363(8) . ? C47 H47 0.9500 . ? C48 C49 1.393(8) . ? C48 H48 0.9500 . ? C49 C51 1.379(8) . ? C49 H49 0.9500 . ? C50 C46 1.380(7) 2_656 ? C50 C51 1.407(7) 2_656 ? C51 C50 1.407(7) 2_656 ? C51 H51 0.9500 . ? C106 C107 1.460(8) . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? Co2 N9 2.098(3) . ? Co2 N11 2.100(3) . ? Co2 N15 2.107(3) . ? Co2 N14 2.123(3) . ? Co2 N108 2.127(4) . ? Co2 F4 2.361(3) . ? P2 F4 1.220(3) 2_765 ? P2 F4 1.220(3) . ? P2 F6 1.713(5) 2_765 ? P2 F6 1.713(5) . ? P2 F5 1.713(5) . ? P2 F5 1.713(5) 2_765 ? O5 C63 1.378(6) . ? O5 C68 1.442(6) . ? O6 C66 1.383(5) . ? O6 C108 1.455(6) . ? O7 C88 1.380(6) . ? O7 C94 1.446(6) . ? O8 C91 1.379(6) . ? O8 C97 1.462(6) . ? N9 C53 1.311(6) . ? N9 C54 1.409(5) . ? N10 C53 1.348(5) . ? N10 C59 1.372(5) . ? N10 C60 1.491(6) . ? N11 C79 1.329(5) . ? N11 C80 1.401(6) . ? N12 C79 1.357(5) . ? N12 C85 1.386(6) . ? N12 C86 1.464(5) . ? N13 C98 1.344(6) 2_765 ? N13 C99 1.384(6) . ? N13 C95 1.476(5) . ? N14 C98 1.313(5) . ? N14 C104 1.402(6) . ? N15 C71 1.296(6) . ? N15 C78 1.404(5) . ? N16 C71 1.341(5) 2_765 ? N16 C72 1.390(6) . ? N16 C70 1.472(6) . ? N108 C75 1.129(6) . ? C53 H53 0.9500 . ? C54 C55 1.388(6) . ? C54 C59 1.395(6) . ? C55 C56 1.380(6) . ? C55 H55 0.9500 . ? C56 C57 1.390(7) . ? C56 H56 0.9500 . ? C57 C58 1.375(7) . ? C57 H57 0.9500 . ? C58 C59 1.406(6) . ? C58 H58 0.9500 . ? C60 C61 1.499(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.383(6) . ? C61 C66 1.400(6) . ? C62 C63 1.411(7) . ? C62 C67 1.512(6) . ? C63 C64 1.385(7) . ? C64 C65 1.401(7) . ? C64 C69 1.515(7) . ? C65 C66 1.396(7) . ? C65 C70 1.502(6) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N16 1.341(5) 2_765 ? C71 H71 0.9500 . ? C72 C78 1.386(7) 2_765 ? C72 C73 1.386(6) . ? C73 C74 1.396(8) . ? C73 H73 0.9500 . ? C74 C76 1.381(8) . ? C74 H74 0.9500 . ? C75 C105 1.457(9) . ? C76 C77 1.388(7) . ? C76 H76 0.9500 . ? C77 C78 1.395(6) 2_765 ? C77 H77 0.9500 . ? C78 C72 1.386(7) 2_765 ? C78 C77 1.395(6) 2_765 ? C79 H79 0.9500 . ? C80 C81 1.390(6) . ? C80 C85 1.396(6) . ? C81 C82 1.367(7) . ? C81 H81 0.9500 . ? C82 C83 1.405(7) . ? C82 H82 0.9500 . ? C83 C84 1.359(7) . ? C83 H83 0.9500 . ? C84 C85 1.395(6) . ? C84 H84 0.9500 . ? C86 C87 1.513(6) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C92 1.386(7) . ? C87 C88 1.390(7) . ? C88 C89 1.387(7) . ? C89 C90 1.392(7) . ? C89 C95 1.497(7) . ? C90 C91 1.390(7) . ? C90 C96 1.523(7) . ? C91 C92 1.400(7) . ? C92 C93 1.502(7) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 N13 1.344(6) 2_765 ? C98 H98 0.9500 . ? C99 C100 1.388(7) . ? C99 C104 1.400(6) 2_765 ? C100 C101 1.361(7) . ? C100 H100 0.9500 . ? C101 C102 1.401(7) . ? C101 H101 0.9500 . ? C102 C103 1.389(7) . ? C102 H102 0.9500 . ? C103 C104 1.396(6) 2_765 ? C103 H103 0.9500 . ? C104 C103 1.396(6) 2_765 ? C104 C99 1.400(6) 2_765 ? C105 H10D 0.9800 . ? C105 H10E 0.9800 . ? C105 H10F 0.9800 . ? C108 H10G 0.9800 . ? C108 H10H 0.9800 . ? C108 H10I 0.9800 . ? P3 F8 1.551(4) . ? P3 F11 1.558(4) . ? P3 F9 1.573(4) . ? P3 F10 1.584(5) . ? P3 F12 1.586(4) . ? P3 F7 1.591(4) . ? P4 F14 1.543(5) . ? P4 F16 1.553(6) . ? P4 F17 1.572(6) . ? P4 F18 1.574(5) . ? P4 F13 1.574(6) . ? P4 F15 1.579(6) . ? N150 C151 1.116(12) . ? C151 C152 1.306(15) . ? C152 H15D 0.9800 . ? C152 H15E 0.9800 . ? C152 H15F 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 N8 Co1 N3 89.69(16) . . ? N8 Co1 N1 89.31(17) . . ? N3 Co1 N1 173.20(15) . . ? N8 Co1 N5 172.96(16) . . ? N3 Co1 N5 90.41(17) . . ? N1 Co1 N5 89.76(17) . . ? N8 Co1 N106 92.41(16) . . ? N3 Co1 N106 94.55(16) . . ? N1 Co1 N106 92.21(16) . . ? N5 Co1 N106 94.60(16) . . ? F1 P1 F1 180.000(2) 2_656 . ? F1 P1 F3 88.7(3) 2_656 2_656 ? F1 P1 F3 91.3(3) . 2_656 ? F1 P1 F3 91.3(3) 2_656 . ? F1 P1 F3 88.7(3) . . ? F3 P1 F3 180.0(4) 2_656 . ? F1 P1 F2 89.2(3) 2_656 . ? F1 P1 F2 90.8(3) . . ? F3 P1 F2 85.5(3) 2_656 . ? F3 P1 F2 94.5(3) . . ? F1 P1 F2 90.8(3) 2_656 2_656 ? F1 P1 F2 89.2(3) . 2_656 ? F3 P1 F2 94.5(3) 2_656 2_656 ? F3 P1 F2 85.5(3) . 2_656 ? F2 P1 F2 180.0(3) . 2_656 ? C10 O1 C14 116.0(4) . . ? C13 O2 C16 111.7(4) . . ? C38 O3 C43 112.2(6) . . ? C35 O4 C40 115.8(5) . . ? C1 N1 C2 104.6(4) . . ? C1 N1 Co1 125.9(3) . . ? C2 N1 Co1 129.2(3) . . ? C1 N2 C7 106.4(4) . . ? C1 N2 C8 128.5(4) . . ? C7 N2 C8 125.1(4) . . ? C18 N3 C19 105.9(4) . . ? C18 N3 Co1 125.2(3) . . ? C19 N3 Co1 128.3(3) . . ? C18 N4 C24 106.9(4) . . ? C18 N4 C25 128.2(4) . 2_656 ? C24 N4 C25 124.5(4) . 2_656 ? C26 N5 C27 105.4(4) . . ? C26 N5 Co1 124.6(3) . . ? C27 N5 Co1 129.7(3) . . ? C26 N6 C32 107.5(4) . . ? C26 N6 C33 129.8(5) . . ? C32 N6 C33 122.7(5) . . ? C45 N7 C50 106.0(4) 2_656 . ? C45 N7 C41 127.4(5) 2_656 . ? C50 N7 C41 126.1(5) . . ? C45 N8 C46 104.5(4) . . ? C45 N8 Co1 124.7(4) . . ? C46 N8 Co1 130.1(3) . . ? C106 N106 Co1 166.4(5) . . ? N1 C1 N2 113.6(4) . . ? N1 C1 H1 123.2 . . ? N2 C1 H1 123.2 . . ? C7 C2 C3 120.5(5) . . ? C7 C2 N1 108.5(4) . . ? C3 C2 N1 131.0(5) . . ? C4 C3 C2 117.6(5) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 121.6(5) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 121.0(5) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 117.3(6) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? C2 C7 C6 122.1(5) . . ? C2 C7 N2 106.9(4) . . ? C6 C7 N2 131.0(5) . . ? N2 C8 C9 114.5(4) . . ? N2 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N2 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C52 C9 C10 119.9(5) . . ? C52 C9 C8 121.3(5) . . ? C10 C9 C8 118.7(5) . . ? O1 C10 C11 118.3(5) . . ? O1 C10 C9 120.3(4) . . ? C11 C10 C9 121.3(5) . . ? C12 C11 C10 120.4(5) . . ? C12 C11 C25 120.1(5) . . ? C10 C11 C25 119.4(5) . . ? C11 C12 C13 118.3(5) . . ? C11 C12 C15 123.8(5) . . ? C13 C12 C15 117.9(5) . . ? O2 C13 C12 119.8(5) . . ? O2 C13 C52 118.4(5) . . ? C12 C13 C52 121.7(5) . . ? O1 C14 H14A 109.5 . . ? O1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C52 C17 H17A 109.5 . . ? C52 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C52 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 N4 112.8(4) . . ? N3 C18 H18 123.6 . . ? N4 C18 H18 123.6 . . ? C20 C19 N3 131.6(5) . . ? C20 C19 C24 119.7(5) . . ? N3 C19 C24 108.7(4) . . ? C21 C20 C19 117.4(5) . . ? C21 C20 H20 121.3 . . ? C19 C20 H20 121.3 . . ? C20 C21 C22 123.0(5) . . ? C20 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C23 C22 C21 120.9(5) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 116.5(5) . . ? C22 C23 H23 121.7 . . ? C24 C23 H23 121.7 . . ? N4 C24 C23 131.8(5) . . ? N4 C24 C19 105.7(4) . . ? C23 C24 C19 122.4(5) . . ? N4 C25 C11 113.6(4) 2_656 . ? N4 C25 H25A 108.9 2_656 . ? C11 C25 H25A 108.9 . . ? N4 C25 H25B 108.9 2_656 . ? C11 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? N5 C26 N6 112.9(4) . . ? N5 C26 H26 123.5 . . ? N6 C26 H26 123.5 . . ? N5 C27 C32 108.3(4) . . ? N5 C27 C28 131.1(5) . . ? C32 C27 C28 120.6(5) . . ? C29 C28 C27 116.1(6) . . ? C29 C28 H28 122.0 . . ? C27 C28 H28 122.0 . . ? C28 C29 C30 123.2(5) . . ? C28 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C31 C30 C29 121.8(5) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 116.1(5) . . ? C30 C31 H31 121.9 . . ? C32 C31 H31 121.9 . . ? N6 C32 C27 105.9(4) . . ? N6 C32 C31 132.0(5) . . ? C27 C32 C31 122.1(5) . . ? N6 C33 C34 114.7(5) . . ? N6 C33 H33A 108.6 . . ? C34 C33 H33A 108.6 . . ? N6 C33 H33B 108.6 . . ? C34 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C35 C34 C39 120.2(5) . . ? C35 C34 C33 118.7(6) . . ? C39 C34 C33 120.8(6) . . ? O4 C35 C34 122.0(5) . . ? O4 C35 C36 116.6(5) . . ? C34 C35 C36 121.3(5) . . ? C35 C36 C37 120.2(5) . . ? C35 C36 C41 118.6(6) . . ? C37 C36 C41 121.1(6) . . ? C38 C37 C36 116.8(5) . . ? C38 C37 C42 119.4(6) . . ? C36 C37 C42 123.8(6) . . ? C39 C38 C37 123.2(5) . . ? C39 C38 O3 117.2(6) . . ? C37 C38 O3 119.6(6) . . ? C34 C39 C38 118.2(5) . . ? C34 C39 C44 122.0(6) . . ? C38 C39 C44 119.7(7) . . ? O4 C40 H40A 109.5 . . ? O4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N7 C41 C36 113.3(5) . . ? N7 C41 H41A 108.9 . . ? C36 C41 H41A 108.9 . . ? N7 C41 H41B 108.9 . . ? C36 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O3 C43 H43A 109.5 . . ? O3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N8 C45 N7 114.0(5) . 2_656 ? N8 C45 H45 123.0 . . ? N7 C45 H45 123.0 2_656 . ? C50 C46 C47 121.3(5) 2_656 . ? C50 C46 N8 108.3(4) 2_656 . ? C47 C46 N8 130.3(5) . . ? C48 C47 C46 116.3(5) . . ? C48 C47 H47 121.9 . . ? C46 C47 H47 121.9 . . ? C47 C48 C49 123.0(5) . . ? C47 C48 H48 118.5 . . ? C49 C48 H48 118.5 . . ? C51 C49 C48 121.5(5) . . ? C51 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C46 C50 N7 107.2(4) 2_656 . ? C46 C50 C51 122.4(5) 2_656 2_656 ? N7 C50 C51 130.4(5) . 2_656 ? C49 C51 C50 115.4(5) . 2_656 ? C49 C51 H51 122.3 . . ? C50 C51 H51 122.3 2_656 . ? C9 C52 C13 118.3(5) . . ? C9 C52 C17 123.5(5) . . ? C13 C52 C17 118.2(5) . . ? N106 C106 C107 177.2(6) . . ? C106 C107 H10A 109.5 . . ? C106 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C106 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? N9 Co2 N11 90.51(13) . . ? N9 Co2 N15 173.89(14) . . ? N11 Co2 N15 90.10(13) . . ? N9 Co2 N14 90.10(13) . . ? N11 Co2 N14 174.29(14) . . ? N15 Co2 N14 88.69(13) . . ? N9 Co2 N108 94.29(14) . . ? N11 Co2 N108 96.47(15) . . ? N15 Co2 N108 91.68(14) . . ? N14 Co2 N108 89.15(14) . . ? N9 Co2 F4 88.07(15) . . ? N11 Co2 F4 87.80(15) . . ? N15 Co2 F4 85.88(15) . . ? N14 Co2 F4 86.55(15) . . ? N108 Co2 F4 175.10(16) . . ? F4 P2 F4 180.0(3) 2_765 . ? F4 P2 F6 90.2(3) 2_765 2_765 ? F4 P2 F6 89.8(3) . 2_765 ? F4 P2 F6 89.8(3) 2_765 . ? F4 P2 F6 90.2(3) . . ? F6 P2 F6 180.0(3) 2_765 . ? F4 P2 F5 89.6(3) 2_765 . ? F4 P2 F5 90.4(3) . . ? F6 P2 F5 90.3(3) 2_765 . ? F6 P2 F5 89.7(3) . . ? F4 P2 F5 90.4(3) 2_765 2_765 ? F4 P2 F5 89.6(3) . 2_765 ? F6 P2 F5 89.7(3) 2_765 2_765 ? F6 P2 F5 90.3(3) . 2_765 ? F5 P2 F5 180.0(5) . 2_765 ? P2 F4 Co2 178.0(4) . . ? C63 O5 C68 112.9(4) . . ? C66 O6 C108 116.3(4) . . ? C88 O7 C94 115.8(4) . . ? C91 O8 C97 113.2(4) . . ? C53 N9 C54 105.1(3) . . ? C53 N9 Co2 124.6(3) . . ? C54 N9 Co2 130.1(3) . . ? C53 N10 C59 107.0(3) . . ? C53 N10 C60 128.9(4) . . ? C59 N10 C60 124.1(3) . . ? C79 N11 C80 105.2(3) . . ? C79 N11 Co2 124.7(3) . . ? C80 N11 Co2 129.7(3) . . ? C79 N12 C85 107.1(3) . . ? C79 N12 C86 128.8(4) . . ? C85 N12 C86 124.1(4) . . ? C98 N13 C99 106.9(3) 2_765 . ? C98 N13 C95 128.2(4) 2_765 . ? C99 N13 C95 124.7(4) . . ? C98 N14 C104 105.1(3) . . ? C98 N14 Co2 122.9(3) . . ? C104 N14 Co2 130.4(3) . . ? C71 N15 C78 105.5(3) . . ? C71 N15 Co2 124.0(3) . . ? C78 N15 Co2 128.4(3) . . ? C71 N16 C72 106.5(4) 2_765 . ? C71 N16 C70 127.4(4) 2_765 . ? C72 N16 C70 125.9(3) . . ? C75 N108 Co2 158.7(4) . . ? N9 C53 N10 113.3(4) . . ? N9 C53 H53 123.3 . . ? N10 C53 H53 123.3 . . ? C55 C54 C59 120.5(4) . . ? C55 C54 N9 131.4(4) . . ? C59 C54 N9 108.1(4) . . ? C56 C55 C54 117.3(4) . . ? C56 C55 H55 121.3 . . ? C54 C55 H55 121.3 . . ? C55 C56 C57 121.7(4) . . ? C55 C56 H56 119.2 . . ? C57 C56 H56 119.2 . . ? C58 C57 C56 122.5(4) . . ? C58 C57 H57 118.7 . . ? C56 C57 H57 118.7 . . ? C57 C58 C59 115.5(4) . . ? C57 C58 H58 122.2 . . ? C59 C58 H58 122.2 . . ? N10 C59 C54 106.5(3) . . ? N10 C59 C58 131.1(4) . . ? C54 C59 C58 122.4(4) . . ? N10 C60 C61 112.9(3) . . ? N10 C60 H60A 109.0 . . ? C61 C60 H60A 109.0 . . ? N10 C60 H60B 109.0 . . ? C61 C60 H60B 109.0 . . ? H60A C60 H60B 107.8 . . ? C62 C61 C66 118.8(4) . . ? C62 C61 C60 122.0(4) . . ? C66 C61 C60 119.1(4) . . ? C61 C62 C63 119.4(4) . . ? C61 C62 C67 121.9(4) . . ? C63 C62 C67 118.7(4) . . ? O5 C63 C64 119.6(4) . . ? O5 C63 C62 118.5(4) . . ? C64 C63 C62 121.8(4) . . ? C63 C64 C65 118.7(4) . . ? C63 C64 C69 119.9(5) . . ? C65 C64 C69 121.3(4) . . ? C66 C65 C64 119.3(4) . . ? C66 C65 C70 117.9(4) . . ? C64 C65 C70 122.6(4) . . ? O6 C66 C65 117.3(4) . . ? O6 C66 C61 120.5(4) . . ? C65 C66 C61 121.9(4) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O5 C68 H68A 109.5 . . ? O5 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O5 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C64 C69 H69A 109.5 . . ? C64 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C64 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N16 C70 C65 112.6(4) . . ? N16 C70 H70A 109.1 . . ? C65 C70 H70A 109.1 . . ? N16 C70 H70B 109.1 . . ? C65 C70 H70B 109.1 . . ? H70A C70 H70B 107.8 . . ? N15 C71 N16 113.8(4) . 2_765 ? N15 C71 H71 123.1 . . ? N16 C71 H71 123.1 2_765 . ? C78 C72 C73 123.8(4) 2_765 . ? C78 C72 N16 105.9(3) 2_765 . ? C73 C72 N16 130.3(5) . . ? C72 C73 C74 114.8(5) . . ? C72 C73 H73 122.6 . . ? C74 C73 H73 122.6 . . ? C76 C74 C73 122.2(5) . . ? C76 C74 H74 118.9 . . ? C73 C74 H74 118.9 . . ? N108 C75 C105 176.5(6) . . ? C74 C76 C77 122.2(5) . . ? C74 C76 H76 118.9 . . ? C77 C76 H76 118.9 . . ? C76 C77 C78 116.3(5) . 2_765 ? C76 C77 H77 121.8 . . ? C78 C77 H77 121.8 2_765 . ? C72 C78 C77 120.6(4) 2_765 2_765 ? C72 C78 N15 108.4(4) 2_765 . ? C77 C78 N15 131.0(4) 2_765 . ? N11 C79 N12 112.6(4) . . ? N11 C79 H79 123.7 . . ? N12 C79 H79 123.7 . . ? C81 C80 C85 119.9(4) . . ? C81 C80 N11 131.1(4) . . ? C85 C80 N11 109.0(4) . . ? C82 C81 C80 117.6(4) . . ? C82 C81 H81 121.2 . . ? C80 C81 H81 121.2 . . ? C81 C82 C83 121.2(4) . . ? C81 C82 H82 119.4 . . ? C83 C82 H82 119.4 . . ? C84 C83 C82 122.9(4) . . ? C84 C83 H83 118.6 . . ? C82 C83 H83 118.6 . . ? C83 C84 C85 115.3(4) . . ? C83 C84 H84 122.3 . . ? C85 C84 H84 122.3 . . ? N12 C85 C84 130.9(4) . . ? N12 C85 C80 106.0(4) . . ? C84 C85 C80 123.1(4) . . ? N12 C86 C87 113.9(4) . . ? N12 C86 H86A 108.8 . . ? C87 C86 H86A 108.8 . . ? N12 C86 H86B 108.8 . . ? C87 C86 H86B 108.8 . . ? H86A C86 H86B 107.7 . . ? C92 C87 C88 119.9(4) . . ? C92 C87 C86 121.6(4) . . ? C88 C87 C86 118.2(4) . . ? O7 C88 C89 117.7(4) . . ? O7 C88 C87 120.6(4) . . ? C89 C88 C87 121.3(4) . . ? C88 C89 C90 119.8(4) . . ? C88 C89 C95 119.2(4) . . ? C90 C89 C95 121.0(4) . . ? C91 C90 C89 118.3(4) . . ? C91 C90 C96 120.1(5) . . ? C89 C90 C96 121.6(4) . . ? O8 C91 C90 119.3(5) . . ? O8 C91 C92 118.2(4) . . ? C90 C91 C92 122.4(4) . . ? C87 C92 C91 118.2(4) . . ? C87 C92 C93 122.3(5) . . ? C91 C92 C93 119.6(5) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O7 C94 H94A 109.5 . . ? O7 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? O7 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? N13 C95 C89 113.2(4) . . ? N13 C95 H95A 108.9 . . ? C89 C95 H95A 108.9 . . ? N13 C95 H95B 108.9 . . ? C89 C95 H95B 108.9 . . ? H95A C95 H95B 107.7 . . ? C90 C96 H96A 109.5 . . ? C90 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C90 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? O8 C97 H97A 109.5 . . ? O8 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? O8 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N14 C98 N13 113.6(4) . 2_765 ? N14 C98 H98 123.2 . . ? N13 C98 H98 123.2 2_765 . ? N13 C99 C100 131.6(4) . . ? N13 C99 C104 105.8(4) . 2_765 ? C100 C99 C104 122.7(4) . 2_765 ? C101 C100 C99 116.9(4) . . ? C101 C100 H100 121.5 . . ? C99 C100 H100 121.5 . . ? C100 C101 C102 122.0(4) . . ? C100 C101 H101 119.0 . . ? C102 C101 H101 119.0 . . ? C103 C102 C101 121.2(4) . . ? C103 C102 H102 119.4 . . ? C101 C102 H102 119.4 . . ? C102 C103 C104 117.5(4) . 2_765 ? C102 C103 H103 121.2 . . ? C104 C103 H103 121.2 2_765 . ? C103 C104 C99 119.7(4) 2_765 2_765 ? C103 C104 N14 131.6(4) 2_765 . ? C99 C104 N14 108.6(3) 2_765 . ? C75 C105 H10D 109.5 . . ? C75 C105 H10E 109.5 . . ? H10D C105 H10E 109.5 . . ? C75 C105 H10F 109.5 . . ? H10D C105 H10F 109.5 . . ? H10E C105 H10F 109.5 . . ? O6 C108 H10G 109.5 . . ? O6 C108 H10H 109.5 . . ? H10G C108 H10H 109.5 . . ? O6 C108 H10I 109.5 . . ? H10G C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? F8 P3 F11 91.3(3) . . ? F8 P3 F9 89.9(3) . . ? F11 P3 F9 178.7(3) . . ? F8 P3 F10 177.0(3) . . ? F11 P3 F10 90.1(3) . . ? F9 P3 F10 88.7(3) . . ? F8 P3 F12 92.9(3) . . ? F11 P3 F12 90.8(2) . . ? F9 P3 F12 89.6(2) . . ? F10 P3 F12 89.7(3) . . ? F8 P3 F7 88.0(2) . . ? F11 P3 F7 90.0(2) . . ? F9 P3 F7 89.5(2) . . ? F10 P3 F7 89.4(3) . . ? F12 P3 F7 178.8(3) . . ? F14 P4 F16 177.2(3) . . ? F14 P4 F17 87.3(4) . . ? F16 P4 F17 90.2(3) . . ? F14 P4 F18 92.9(3) . . ? F16 P4 F18 88.3(3) . . ? F17 P4 F18 88.7(3) . . ? F14 P4 F13 90.4(3) . . ? F16 P4 F13 88.3(3) . . ? F17 P4 F13 90.9(3) . . ? F18 P4 F13 176.6(3) . . ? F14 P4 F15 90.0(4) . . ? F16 P4 F15 92.6(4) . . ? F17 P4 F15 175.4(4) . . ? F18 P4 F15 87.6(3) . . ? F13 P4 F15 92.9(3) . . ? N150 C151 C152 174.6(16) . . ? C151 C152 H15D 109.5 . . ? C151 C152 H15E 109.5 . . ? H15D C152 H15E 109.5 . . ? C151 C152 H15F 109.5 . . ? H15D C152 H15F 109.5 . . ? H15E C152 H15F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.416 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.112 #===END