Supplementary Material (ESI) for Energy & Environmental Science This journal is © The Royal Society of Chemistry 2008 data_global _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Daniel DuBois' _publ_contact_author_email DANIEL.DUBOIS@PNL.GOV _publ_section_title ; Hydrogen Production Using Cobalt-Based Molecular Catalysts Containing a Proton Relay in the Second Coordination Sphere ; loop_ _publ_author_name 'Daniel DuBois' 'R. Morris Bullock' 'M. Rakowski DuBois' 'George M. Jacobsen' 'Brendan Twamley' ; A.D.Wilson ; 'Jenny Y. Yang' # Attachment 'combined.cif' data_bt1161 _database_code_depnum_ccdc_archive 'CCDC 683301' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[RCoCl][BF4]' _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 Cl Co N4 P4, 0.5(B F4), 0.5(B F4)' _chemical_formula_sum 'C56 H56 B Cl Co F4 N4 P4' _chemical_formula_weight 1090.12 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.2939(13) _cell_length_b 12.9425(5) _cell_length_c 28.6361(11) _cell_angle_alpha 90.00 _cell_angle_beta 121.872(1) _cell_angle_gamma 90.00 _cell_volume 10793.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9890 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26.02 _exptl_crystal_description blade _exptl_crystal_colour orange _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4520 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7851 _exptl_absorpt_correction_T_max 0.9529 _exptl_absorpt_process_details 'SADABS-2007/4 (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62971 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.25 _reflns_number_total 9775 _reflns_number_gt 7862 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _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^)+(0.0860P)^2^+14.8951P] 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 9775 _refine_ls_number_parameters 608 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.068 _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 0.115879(13) 0.10100(3) 0.082859(15) 0.02156(12) Uani 1 1 d . . . B1 B 0.0000 0.6557(6) 0.2500 0.0617(16) Uani 1 2 d S . . F1 F 0.03249(8) 0.5898(2) 0.29212(10) 0.0606(6) Uani 1 1 d . . . F2 F 0.02148(12) 0.7157(2) 0.23109(12) 0.0816(9) Uani 1 1 d . . . Cl1 Cl 0.04174(2) 0.13209(6) 0.01371(3) 0.02820(18) Uani 1 1 d . . . P1 P 0.13261(3) 0.04756(6) 0.02202(3) 0.02236(18) Uani 1 1 d . . . P2 P 0.14362(3) -0.05459(6) 0.11936(3) 0.02548(19) Uani 1 1 d . . . P3 P 0.10096(3) 0.14790(6) 0.14575(3) 0.02625(19) Uani 1 1 d . . . P4 P 0.15576(3) 0.24805(6) 0.11003(3) 0.02353(18) Uani 1 1 d . . . C1 C 0.12175(10) 0.1228(2) -0.03732(12) 0.0256(6) Uani 1 1 d . . . C2 C 0.09889(10) 0.2164(2) -0.05150(12) 0.0279(7) Uani 1 1 d . . . H2A H 0.0900 0.2469 -0.0283 0.033 Uiso 1 1 calc R . . C3 C 0.08887(11) 0.2661(3) -0.09990(13) 0.0321(7) Uani 1 1 d . . . H3A H 0.0732 0.3305 -0.1095 0.038 Uiso 1 1 calc R . . C4 C 0.10158(11) 0.2222(3) -0.13406(14) 0.0366(8) Uani 1 1 d . . . H4A H 0.0944 0.2559 -0.1672 0.044 Uiso 1 1 calc R . . C5 C 0.12478(12) 0.1291(3) -0.11980(14) 0.0382(8) Uani 1 1 d . . . H5A H 0.1337 0.0991 -0.1430 0.046 Uiso 1 1 calc R . . C6 C 0.13494(11) 0.0799(3) -0.07203(13) 0.0339(7) Uani 1 1 d . . . H6A H 0.1511 0.0161 -0.0624 0.041 Uiso 1 1 calc R . . C7 C 0.09766(10) -0.0675(2) -0.01320(12) 0.0264(6) Uani 1 1 d . A . H7A H 0.0651 -0.0529 -0.0265 0.032 Uiso 1 1 calc R . . H7B H 0.0998 -0.0834 -0.0456 0.032 Uiso 1 1 calc R . . N8 N 0.11288(9) -0.15693(19) 0.02333(11) 0.0291(6) Uani 1 1 d . . . C9A C 0.10121(16) -0.2568(3) -0.0030(2) 0.0273(16) Uiso 0.647(12) 1 d PG A 1 C10A C 0.12882(15) -0.2946(4) -0.0200(2) 0.046(2) Uiso 0.647(12) 1 d PG A 1 H10A H 0.1555 -0.2571 -0.0121 0.055 Uiso 0.647(12) 1 calc PR A 1 C11A C 0.11880(17) -0.3848(4) -0.0481(2) 0.057(2) Uiso 0.647(12) 1 d PG A 1 H11A H 0.1387 -0.4092 -0.0594 0.068 Uiso 0.647(12) 1 calc PR A 1 C12A C 0.08095(17) -0.4414(3) -0.0606(2) 0.0490(18) Uiso 0.647(12) 1 d PG A 1 H12A H 0.0742 -0.5042 -0.0806 0.059 Uiso 0.647(12) 1 calc PR A 1 C13A C 0.05206(14) -0.4044(4) -0.0431(2) 0.0525(18) Uiso 0.647(12) 1 d PG A 1 H13A H 0.0255 -0.4421 -0.0509 0.063 Uiso 0.647(12) 1 calc PR A 1 C14A C 0.06297(14) -0.3122(4) -0.0143(2) 0.0390(15) Uiso 0.647(12) 1 d PG A 1 H14A H 0.0437 -0.2868 -0.0023 0.047 Uiso 0.647(12) 1 calc PR A 1 C9B C 0.1022(3) -0.2459(6) -0.0117(4) 0.023(3) Uiso 0.353(12) 1 d PG A 2 C10B C 0.1321(2) -0.2821(7) -0.0256(4) 0.043(4) Uiso 0.353(12) 1 d PG A 2 H10B H 0.1595 -0.2450 -0.0144 0.051 Uiso 0.353(12) 1 calc PR A 2 C11B C 0.1231(3) -0.3701(7) -0.0552(4) 0.046(3) Uiso 0.353(12) 1 d PG A 2 H11B H 0.1446 -0.3935 -0.0642 0.056 Uiso 0.353(12) 1 calc PR A 2 C12B C 0.0842(3) -0.4261(6) -0.0724(4) 0.035(3) Uiso 0.353(12) 1 d PG A 2 H12B H 0.0783 -0.4873 -0.0934 0.042 Uiso 0.353(12) 1 calc PR A 2 C13B C 0.0528(2) -0.3907(6) -0.0582(4) 0.052(3) Uiso 0.353(12) 1 d PG A 2 H13B H 0.0254 -0.4280 -0.0693 0.062 Uiso 0.353(12) 1 calc PR A 2 C14B C 0.0627(3) -0.3006(6) -0.0278(4) 0.041(3) Uiso 0.353(12) 1 d PG A 2 H14B H 0.0418 -0.2763 -0.0180 0.050 Uiso 0.353(12) 1 calc PR A 2 C15 C 0.10397(11) -0.1509(2) 0.06739(13) 0.0312(7) Uani 1 1 d . A . H15A H 0.1087 -0.2195 0.0849 0.037 Uiso 1 1 calc R . . H15B H 0.0717 -0.1300 0.0524 0.037 Uiso 1 1 calc R . . C16 C 0.19206(10) 0.0001(2) 0.04933(12) 0.0281(7) Uani 1 1 d . . . H16A H 0.1906 -0.0667 0.0316 0.034 Uiso 1 1 calc R . . H16B H 0.2084 0.0500 0.0395 0.034 Uiso 1 1 calc R . . N17 N 0.21799(8) -0.0138(2) 0.10864(10) 0.0273(6) Uani 1 1 d . . . C18 C 0.26665(10) -0.0077(3) 0.13594(13) 0.0311(7) Uani 1 1 d . . . C19 C 0.28919(11) 0.0043(3) 0.10800(15) 0.0407(8) Uani 1 1 d . . . H19A H 0.2726 -0.0021 0.0691 0.049 Uiso 1 1 calc R . . C20 C 0.33621(12) 0.0259(3) 0.13652(17) 0.0517(10) Uani 1 1 d . . . H20A H 0.3512 0.0353 0.1168 0.062 Uiso 1 1 calc R . . C21 C 0.36080(13) 0.0334(4) 0.19254(18) 0.0617(13) Uani 1 1 d . . . H21A H 0.3926 0.0501 0.2117 0.074 Uiso 1 1 calc R . . C22 C 0.33909(12) 0.0167(4) 0.22108(17) 0.0610(13) Uani 1 1 d . . . H22A H 0.3564 0.0186 0.2601 0.073 Uiso 1 1 calc R . . C23 C 0.29218(11) -0.0030(3) 0.19315(15) 0.0424(9) Uani 1 1 d . . . H23A H 0.2775 -0.0132 0.2131 0.051 Uiso 1 1 calc R . . C24 C 0.19928(10) -0.0928(2) 0.12817(13) 0.0300(7) Uani 1 1 d . . . H24A H 0.2217 -0.1063 0.1676 0.036 Uiso 1 1 calc R . . H24B H 0.1950 -0.1578 0.1078 0.036 Uiso 1 1 calc R . . C25 C 0.14897(11) -0.1019(2) 0.18263(13) 0.0285(7) Uani 1 1 d . . . C26 C 0.11586(11) -0.1665(3) 0.18132(14) 0.0337(7) Uani 1 1 d . . . H26A H 0.0894 -0.1849 0.1470 0.040 Uiso 1 1 calc R . . C27 C 0.12134(12) -0.2040(3) 0.22976(14) 0.0371(8) Uani 1 1 d . . . H27A H 0.0989 -0.2485 0.2287 0.045 Uiso 1 1 calc R . . C28 C 0.15966(11) -0.1764(3) 0.27970(14) 0.0361(8) Uani 1 1 d . . . H28A H 0.1637 -0.2033 0.3129 0.043 Uiso 1 1 calc R . . C29 C 0.19222(11) -0.1098(3) 0.28171(14) 0.0332(7) Uani 1 1 d . . . H29A H 0.2180 -0.0898 0.3162 0.040 Uiso 1 1 calc R . . C30 C 0.18704(11) -0.0725(2) 0.23328(13) 0.0288(7) Uani 1 1 d . . . H30A H 0.2093 -0.0270 0.2346 0.035 Uiso 1 1 calc R . . C31 C 0.06472(11) 0.0665(3) 0.15918(13) 0.0317(7) Uani 1 1 d . . . C32 C 0.06932(14) 0.0663(4) 0.21044(16) 0.0538(11) Uani 1 1 d . . . H32A H 0.0913 0.1099 0.2388 0.065 Uiso 1 1 calc R . . C33 C 0.04166(14) 0.0020(4) 0.22027(16) 0.0595(12) Uani 1 1 d . . . H33A H 0.0450 0.0019 0.2554 0.071 Uiso 1 1 calc R . . C34 C 0.00964(12) -0.0612(3) 0.17917(15) 0.0434(9) Uani 1 1 d . . . H34A H -0.0089 -0.1053 0.1860 0.052 Uiso 1 1 calc R . . C35 C 0.00445(10) -0.0604(3) 0.12778(13) 0.0311(7) Uani 1 1 d . . . H35A H -0.0178 -0.1037 0.0994 0.037 Uiso 1 1 calc R . . C36 C 0.03174(10) 0.0033(2) 0.11756(13) 0.0279(7) Uani 1 1 d . . . H36A H 0.0279 0.0039 0.0822 0.034 Uiso 1 1 calc R . . C37 C 0.15081(10) 0.1761(3) 0.21537(12) 0.0299(7) Uani 1 1 d . . . H37A H 0.1450 0.2417 0.2284 0.036 Uiso 1 1 calc R . . H37B H 0.1534 0.1207 0.2407 0.036 Uiso 1 1 calc R . . N38 N 0.19432(8) 0.1842(2) 0.21809(10) 0.0281(6) Uani 1 1 d . . . C39 C 0.23488(11) 0.1698(2) 0.27151(13) 0.0296(7) Uani 1 1 d . . . C40 C 0.23279(12) 0.1569(3) 0.31854(13) 0.0338(7) Uani 1 1 d . . . H40A H 0.2044 0.1654 0.3164 0.041 Uiso 1 1 calc R . . C41 C 0.27211(12) 0.1315(3) 0.36841(14) 0.0378(8) Uani 1 1 d . . . H41A H 0.2702 0.1217 0.4000 0.045 Uiso 1 1 calc R . . C42 C 0.31388(12) 0.1204(3) 0.37259(14) 0.0386(8) Uani 1 1 d . . . H42A H 0.3405 0.1014 0.4066 0.046 Uiso 1 1 calc R . . C43 C 0.31639(12) 0.1371(3) 0.32674(14) 0.0380(8) Uani 1 1 d . . . H43A H 0.3452 0.1315 0.3296 0.046 Uiso 1 1 calc R . . C44 C 0.27749(11) 0.1621(3) 0.27647(14) 0.0331(7) Uani 1 1 d . . . H44A H 0.2799 0.1739 0.2454 0.040 Uiso 1 1 calc R . . C45 C 0.19575(11) 0.2686(2) 0.18510(12) 0.0278(7) Uani 1 1 d . . . H45A H 0.2274 0.2754 0.1930 0.033 Uiso 1 1 calc R . . H45B H 0.1877 0.3340 0.1959 0.033 Uiso 1 1 calc R . . C46 C 0.06867(11) 0.2693(3) 0.12600(13) 0.0310(7) Uani 1 1 d . A . H46A H 0.0415 0.2619 0.0883 0.037 Uiso 1 1 calc R . . H46B H 0.0574 0.2818 0.1510 0.037 Uiso 1 1 calc R . . N47 N 0.09539(9) 0.3600(2) 0.12758(11) 0.0321(6) Uani 1 1 d . . . C48A C 0.07234(19) 0.4489(5) 0.1278(3) 0.0266(16) Uiso 0.647(12) 1 d P A 1 C49A C 0.0613(2) 0.4640(6) 0.1677(3) 0.0373(16) Uiso 0.647(12) 1 d P A 1 H49A H 0.0696 0.4130 0.1953 0.045 Uiso 0.647(12) 1 calc PR A 1 C50A C 0.0386(2) 0.5516(5) 0.1677(3) 0.0425(18) Uiso 0.647(12) 1 d P A 1 H50A H 0.0316 0.5615 0.1954 0.051 Uiso 0.647(12) 1 calc PR A 1 C51A C 0.0262(2) 0.6241(6) 0.1276(3) 0.0351(16) Uiso 0.647(12) 1 d P A 1 H51A H 0.0106 0.6843 0.1280 0.042 Uiso 0.647(12) 1 calc PR A 1 C52A C 0.0356(2) 0.6131(5) 0.0866(3) 0.0398(16) Uiso 0.647(12) 1 d P A 1 H52A H 0.0262 0.6637 0.0586 0.048 Uiso 0.647(12) 1 calc PR A 1 C53A C 0.0597(2) 0.5242(5) 0.0877(4) 0.0368(17) Uiso 0.647(12) 1 d P A 1 H53A H 0.0674 0.5154 0.0606 0.044 Uiso 0.647(12) 1 calc PR A 1 C48B C 0.0690(3) 0.4665(9) 0.1126(5) 0.024(3) Uiso 0.353(12) 1 d P A 2 C49B C 0.0571(3) 0.4906(9) 0.1515(5) 0.027(3) Uiso 0.353(12) 1 d P A 2 H49B H 0.0661 0.4452 0.1816 0.032 Uiso 0.353(12) 1 calc PR A 2 C50B C 0.0326(3) 0.5790(10) 0.1467(6) 0.028(3) Uiso 0.353(12) 1 d P A 2 H50B H 0.0252 0.5963 0.1734 0.034 Uiso 0.353(12) 1 calc PR A 2 C51B C 0.0194(4) 0.6407(8) 0.1019(6) 0.035(3) Uiso 0.353(12) 1 d P A 2 H51B H 0.0020 0.7012 0.0970 0.042 Uiso 0.353(12) 1 calc PR A 2 C52B C 0.0316(4) 0.6158(9) 0.0620(6) 0.047(3) Uiso 0.353(12) 1 d P A 2 H52B H 0.0233 0.6604 0.0318 0.056 Uiso 0.353(12) 1 calc PR A 2 C53B C 0.0554(4) 0.5258(8) 0.0689(6) 0.031(3) Uiso 0.353(12) 1 d P A 2 H53B H 0.0623 0.5060 0.0420 0.037 Uiso 0.353(12) 1 calc PR A 2 C54 C 0.11394(11) 0.3549(2) 0.09188(13) 0.0284(7) Uani 1 1 d . A . H54A H 0.1292 0.4213 0.0942 0.034 Uiso 1 1 calc R . . H54B H 0.0883 0.3458 0.0534 0.034 Uiso 1 1 calc R . . C55 C 0.18948(10) 0.2948(2) 0.08178(12) 0.0264(7) Uani 1 1 d . . . C56 C 0.17655(12) 0.3786(3) 0.04595(13) 0.0344(7) Uani 1 1 d . . . H56A H 0.1489 0.4147 0.0350 0.041 Uiso 1 1 calc R . . C57 C 0.20406(13) 0.4090(3) 0.02630(15) 0.0448(9) Uani 1 1 d . . . H57A H 0.1952 0.4663 0.0020 0.054 Uiso 1 1 calc R . . C58 C 0.24415(13) 0.3571(3) 0.04156(14) 0.0425(9) Uani 1 1 d . . . H58A H 0.2628 0.3788 0.0280 0.051 Uiso 1 1 calc R . . C59 C 0.25709(12) 0.2732(3) 0.07664(14) 0.0362(8) Uani 1 1 d . . . H59A H 0.2844 0.2365 0.0867 0.043 Uiso 1 1 calc R . . C60 C 0.23016(11) 0.2425(2) 0.09720(13) 0.0289(7) Uani 1 1 d . . . H60A H 0.2395 0.1856 0.1218 0.035 Uiso 1 1 calc R . . B2 B 0.2389(4) 0.2036(8) 0.4794(4) 0.0617(16) Uani 0.50 1 d PD . . F3 F 0.2467(3) 0.2710(9) 0.4470(4) 0.1217(14) Uani 0.50 1 d PD . . F4 F 0.1979(3) 0.1447(7) 0.4462(3) 0.1217(14) Uani 0.50 1 d PD . . F5 F 0.2737(3) 0.1442(7) 0.5029(4) 0.1217(14) Uani 0.50 1 d PD . . F6 F 0.2378(3) 0.2400(9) 0.5230(4) 0.1217(14) Uani 0.50 1 d PD . . 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 0.0198(2) 0.0248(2) 0.0193(2) 0.00042(15) 0.00978(17) -0.00257(15) B1 0.081(4) 0.068(4) 0.045(3) 0.000 0.039(3) 0.000 F1 0.0570(15) 0.0699(16) 0.0536(14) -0.0066(12) 0.0284(12) 0.0049(12) F2 0.122(2) 0.0756(19) 0.0738(18) -0.0202(15) 0.0703(19) -0.0390(18) Cl1 0.0220(4) 0.0365(4) 0.0235(4) 0.0000(3) 0.0103(3) -0.0004(3) P1 0.0209(4) 0.0250(4) 0.0205(4) 0.0003(3) 0.0104(3) -0.0015(3) P2 0.0234(4) 0.0281(4) 0.0219(4) 0.0034(3) 0.0099(3) -0.0018(3) P3 0.0234(4) 0.0346(4) 0.0225(4) -0.0025(3) 0.0133(3) -0.0059(3) P4 0.0231(4) 0.0267(4) 0.0221(4) -0.0020(3) 0.0127(3) -0.0038(3) C1 0.0225(15) 0.0333(17) 0.0210(15) 0.0024(12) 0.0116(12) -0.0050(12) C2 0.0251(15) 0.0344(17) 0.0232(15) -0.0018(13) 0.0121(13) -0.0052(13) C3 0.0312(17) 0.0301(17) 0.0296(17) 0.0059(13) 0.0124(14) -0.0040(13) C4 0.0360(18) 0.046(2) 0.0286(17) 0.0065(15) 0.0180(15) -0.0074(16) C5 0.0368(19) 0.053(2) 0.0328(19) 0.0007(16) 0.0237(16) -0.0017(16) C6 0.0299(17) 0.0433(19) 0.0318(18) 0.0033(15) 0.0187(15) 0.0032(14) C7 0.0266(15) 0.0281(16) 0.0226(15) -0.0011(12) 0.0118(13) -0.0026(12) N8 0.0308(14) 0.0236(13) 0.0302(14) 0.0000(11) 0.0141(12) -0.0008(11) C15 0.0289(17) 0.0272(17) 0.0327(17) 0.0028(13) 0.0129(14) -0.0038(13) C16 0.0240(15) 0.0316(17) 0.0281(16) -0.0010(13) 0.0134(13) -0.0025(13) N17 0.0194(12) 0.0327(14) 0.0257(13) 0.0005(11) 0.0091(11) -0.0023(11) C18 0.0210(15) 0.0324(17) 0.0356(18) -0.0035(14) 0.0120(14) 0.0035(13) C19 0.0258(17) 0.055(2) 0.039(2) -0.0085(17) 0.0153(15) 0.0020(16) C20 0.0312(19) 0.071(3) 0.058(3) -0.016(2) 0.0272(19) -0.0037(19) C21 0.0253(19) 0.096(4) 0.059(3) -0.029(2) 0.0185(19) -0.007(2) C22 0.0245(18) 0.105(4) 0.042(2) -0.021(2) 0.0102(17) 0.003(2) C23 0.0256(17) 0.060(2) 0.037(2) -0.0085(17) 0.0136(15) 0.0020(16) C24 0.0261(16) 0.0318(17) 0.0288(17) 0.0054(13) 0.0122(14) 0.0031(13) C25 0.0295(16) 0.0300(16) 0.0243(16) 0.0085(13) 0.0131(14) 0.0041(13) C26 0.0284(17) 0.0396(19) 0.0294(17) 0.0064(14) 0.0127(14) -0.0004(14) C27 0.0336(18) 0.041(2) 0.039(2) 0.0123(15) 0.0210(16) 0.0020(15) C28 0.0364(18) 0.045(2) 0.0307(18) 0.0111(15) 0.0200(16) 0.0073(15) C29 0.0324(17) 0.0360(18) 0.0282(17) 0.0031(14) 0.0140(15) 0.0051(14) C30 0.0289(16) 0.0296(16) 0.0284(17) 0.0061(13) 0.0153(14) 0.0044(13) C31 0.0283(16) 0.0418(19) 0.0297(17) -0.0018(14) 0.0186(14) -0.0089(14) C32 0.049(2) 0.084(3) 0.036(2) -0.020(2) 0.0282(19) -0.036(2) C33 0.057(2) 0.096(4) 0.037(2) -0.012(2) 0.033(2) -0.034(2) C34 0.0320(18) 0.061(2) 0.039(2) 0.0055(17) 0.0201(16) -0.0144(17) C35 0.0226(15) 0.0360(18) 0.0323(17) 0.0006(14) 0.0128(14) -0.0056(13) C36 0.0232(15) 0.0344(17) 0.0242(15) 0.0017(13) 0.0111(13) 0.0003(13) C37 0.0296(16) 0.0379(18) 0.0234(16) -0.0011(13) 0.0149(14) -0.0071(14) N38 0.0232(13) 0.0380(15) 0.0201(13) -0.0011(11) 0.0093(11) -0.0083(11) C39 0.0295(16) 0.0287(17) 0.0255(16) -0.0040(13) 0.0111(14) -0.0067(13) C40 0.0336(18) 0.0401(19) 0.0265(17) -0.0052(14) 0.0151(15) -0.0075(14) C41 0.042(2) 0.0390(19) 0.0255(17) -0.0004(14) 0.0129(16) -0.0054(15) C42 0.0371(19) 0.0326(18) 0.0314(18) -0.0006(14) 0.0080(16) -0.0028(15) C43 0.0318(18) 0.0333(18) 0.040(2) -0.0022(15) 0.0125(16) -0.0029(14) C44 0.0329(17) 0.0346(18) 0.0319(18) -0.0003(14) 0.0172(15) -0.0035(14) C45 0.0267(16) 0.0341(17) 0.0226(15) -0.0022(13) 0.0129(13) -0.0071(13) C46 0.0249(16) 0.0399(18) 0.0323(17) -0.0070(14) 0.0179(14) -0.0033(14) N47 0.0294(14) 0.0334(15) 0.0375(16) -0.0069(12) 0.0204(13) -0.0012(12) C54 0.0276(16) 0.0275(16) 0.0309(17) -0.0021(13) 0.0159(14) -0.0010(13) C55 0.0253(15) 0.0316(16) 0.0226(15) -0.0074(13) 0.0127(13) -0.0097(13) C56 0.0349(18) 0.0406(19) 0.0284(17) 0.0019(14) 0.0171(15) -0.0029(15) C57 0.046(2) 0.055(2) 0.034(2) 0.0075(17) 0.0217(17) -0.0082(18) C58 0.043(2) 0.063(2) 0.0326(19) -0.0080(17) 0.0275(17) -0.0169(18) C59 0.0309(17) 0.047(2) 0.0338(18) -0.0127(16) 0.0191(15) -0.0093(15) C60 0.0306(16) 0.0318(17) 0.0263(16) -0.0064(13) 0.0165(14) -0.0066(13) B2 0.081(4) 0.068(4) 0.045(3) 0.000 0.039(3) 0.000 F3 0.102(3) 0.145(3) 0.128(4) 0.021(3) 0.067(3) 0.008(3) F4 0.102(3) 0.145(3) 0.128(4) 0.021(3) 0.067(3) 0.008(3) F5 0.102(3) 0.145(3) 0.128(4) 0.021(3) 0.067(3) 0.008(3) F6 0.102(3) 0.145(3) 0.128(4) 0.021(3) 0.067(3) 0.008(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 P3 2.2014(9) . ? Co1 P1 2.2133(8) . ? Co1 P4 2.2303(8) . ? Co1 P2 2.2368(9) . ? Co1 Cl1 2.2870(8) . ? B1 F2 1.364(5) 2 ? B1 F2 1.364(5) . ? B1 F1 1.416(5) 2 ? B1 F1 1.416(5) . ? P1 C1 1.818(3) . ? P1 C7 1.843(3) . ? P1 C16 1.861(3) . ? P2 C25 1.828(3) . ? P2 C24 1.856(3) . ? P2 C15 1.866(3) . ? P3 C31 1.819(3) . ? P3 C46 1.831(3) . ? P3 C37 1.852(3) . ? P4 C55 1.829(3) . ? P4 C54 1.858(3) . ? P4 C45 1.860(3) . ? C1 C2 1.382(4) . ? C1 C6 1.406(4) . ? C2 C3 1.396(4) . ? C2 H2A 0.9500 . ? C3 C4 1.386(5) . ? C3 H3A 0.9500 . ? C4 C5 1.381(5) . ? C4 H4A 0.9500 . ? C5 C6 1.377(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 N8 1.459(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? N8 C9B 1.441(6) . ? N8 C9A 1.443(4) . ? N8 C15 1.448(4) . ? C9A C10A 1.3648 . ? C9A C14A 1.3738 . ? C10A C11A 1.3543 . ? C10A H10A 0.9500 . ? C11A C12A 1.3635 . ? C11A H11A 0.9500 . ? C12A C13A 1.4103 . ? C12A H12A 0.9500 . ? C13A C14A 1.3846 . ? C13A H13A 0.9500 . ? C14A H14A 0.9500 . ? C9B C10B 1.3650 . ? C9B C14B 1.3732 . ? C10B C11B 1.3543 . ? C10B H10B 0.9500 . ? C11B C12B 1.3633 . ? C11B H11B 0.9500 . ? C12B C13B 1.4112 . ? C12B H12B 0.9500 . ? C13B C14B 1.3849 . ? C13B H13B 0.9500 . ? C14B H14B 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N17 1.453(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.423(4) . ? N17 C24 1.465(4) . ? C18 C19 1.384(5) . ? C18 C23 1.393(5) . ? C19 C20 1.398(5) . ? C19 H19A 0.9500 . ? C20 C21 1.366(6) . ? C20 H20A 0.9500 . ? C21 C22 1.382(6) . ? C21 H21A 0.9500 . ? C22 C23 1.391(5) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.394(4) . ? C25 C30 1.398(4) . ? C26 C27 1.385(5) . ? C26 H26A 0.9500 . ? C27 C28 1.384(5) . ? C27 H27A 0.9500 . ? C28 C29 1.387(5) . ? C28 H28A 0.9500 . ? C29 C30 1.389(4) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.391(5) . ? C31 C36 1.394(4) . ? C32 C33 1.398(5) . ? C32 H32A 0.9500 . ? C33 C34 1.376(5) . ? C33 H33A 0.9500 . ? C34 C35 1.386(5) . ? C34 H34A 0.9500 . ? C35 C36 1.390(4) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 N38 1.456(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N38 C39 1.436(4) . ? N38 C45 1.462(4) . ? C39 C44 1.395(5) . ? C39 C40 1.396(5) . ? C40 C41 1.390(5) . ? C40 H40A 0.9500 . ? C41 C42 1.380(5) . ? C41 H41A 0.9500 . ? C42 C43 1.378(5) . ? C42 H42A 0.9500 . ? C43 C44 1.388(5) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N47 1.475(4) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? N47 C48A 1.398(6) . ? N47 C54 1.463(4) . ? N47 C48B 1.579(12) . ? C48A C53A 1.389(9) . ? C48A C49A 1.393(9) . ? C49A C50A 1.375(9) . ? C49A H49A 0.9500 . ? C50A C51A 1.365(9) . ? C50A H50A 0.9500 . ? C51A C52A 1.380(10) . ? C51A H51A 0.9500 . ? C52A C53A 1.406(9) . ? C52A H52A 0.9500 . ? C53A H53A 0.9500 . ? C48B C53B 1.326(18) . ? C48B C49B 1.409(15) . ? C49B C50B 1.383(16) . ? C49B H49B 0.9500 . ? C50B C51B 1.368(17) . ? C50B H50B 0.9500 . ? C51B C52B 1.445(18) . ? C51B H51B 0.9500 . ? C52B C53B 1.376(16) . ? C52B H52B 0.9500 . ? C53B H53B 0.9500 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.395(5) . ? C55 C60 1.396(4) . ? C56 C57 1.387(5) . ? C56 H56A 0.9500 . ? C57 C58 1.378(6) . ? C57 H57A 0.9500 . ? C58 C59 1.383(5) . ? C58 H58A 0.9500 . ? C59 C60 1.390(4) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? B2 F6 1.110(14) 7_556 ? B2 F5 1.271(11) . ? B2 F6 1.355(11) . ? B2 F3 1.397(12) . ? B2 F4 1.432(12) . ? B2 B2 1.57(2) 7_556 ? B2 F3 1.923(14) 7_556 ? F3 F6 0.746(11) 7_556 ? F3 B2 1.923(14) 7_556 ? F5 F6 1.626(13) 7_556 ? F6 F3 0.746(11) 7_556 ? F6 B2 1.110(14) 7_556 ? F6 F5 1.626(13) 7_556 ? 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 P3 Co1 P1 177.34(4) . . ? P3 Co1 P4 81.02(3) . . ? P1 Co1 P4 100.09(3) . . ? P3 Co1 P2 95.23(3) . . ? P1 Co1 P2 82.15(3) . . ? P4 Co1 P2 125.04(3) . . ? P3 Co1 Cl1 91.57(3) . . ? P1 Co1 Cl1 90.30(3) . . ? P4 Co1 Cl1 110.40(3) . . ? P2 Co1 Cl1 124.55(3) . . ? F2 B1 F2 110.6(6) 2 . ? F2 B1 F1 109.53(19) 2 2 ? F2 B1 F1 110.60(15) . 2 ? F2 B1 F1 110.60(15) 2 . ? F2 B1 F1 109.53(18) . . ? F1 B1 F1 105.9(6) 2 . ? C1 P1 C7 99.71(14) . . ? C1 P1 C16 102.01(14) . . ? C7 P1 C16 102.40(14) . . ? C1 P1 Co1 123.91(11) . . ? C7 P1 Co1 108.62(10) . . ? C16 P1 Co1 117.01(10) . . ? C25 P2 C24 102.62(14) . . ? C25 P2 C15 102.48(15) . . ? C24 P2 C15 101.22(15) . . ? C25 P2 Co1 124.08(11) . . ? C24 P2 Co1 117.15(10) . . ? C15 P2 Co1 106.13(11) . . ? C31 P3 C46 101.14(15) . . ? C31 P3 C37 103.39(14) . . ? C46 P3 C37 103.15(15) . . ? C31 P3 Co1 119.55(11) . . ? C46 P3 Co1 110.36(11) . . ? C37 P3 Co1 116.98(10) . . ? C55 P4 C54 101.84(14) . . ? C55 P4 C45 102.21(13) . . ? C54 P4 C45 101.89(15) . . ? C55 P4 Co1 122.84(10) . . ? C54 P4 Co1 107.27(10) . . ? C45 P4 Co1 117.86(10) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 P1 123.3(2) . . ? C6 C1 P1 117.7(2) . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? N8 C7 P1 111.4(2) . . ? N8 C7 H7A 109.3 . . ? P1 C7 H7A 109.3 . . ? N8 C7 H7B 109.3 . . ? P1 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9B N8 C15 123.7(5) . . ? C9A N8 C15 112.0(3) . . ? C9B N8 C7 105.8(5) . . ? C9A N8 C7 116.2(3) . . ? C15 N8 C7 115.0(2) . . ? C10A C9A C14A 119.0 . . ? C10A C9A N8 117.0(3) . . ? C14A C9A N8 123.9(3) . . ? C11A C10A C9A 121.0 . . ? C11A C10A H10A 119.5 . . ? C9A C10A H10A 119.5 . . ? C10A C11A C12A 121.9 . . ? C10A C11A H11A 119.1 . . ? C12A C11A H11A 119.1 . . ? C11A C12A C13A 118.3 . . ? C11A C12A H12A 120.9 . . ? C13A C12A H12A 120.9 . . ? C14A C13A C12A 119.0 . . ? C14A C13A H13A 120.5 . . ? C12A C13A H13A 120.5 . . ? C9A C14A C13A 121.0 . . ? C9A C14A H14A 119.5 . . ? C13A C14A H14A 119.5 . . ? C10B C9B C14B 118.9 . . ? C10B C9B N8 121.5(5) . . ? C14B C9B N8 119.4(5) . . ? C11B C10B C9B 121.0 . . ? C11B C10B H10B 119.5 . . ? C9B C10B H10B 119.5 . . ? C10B C11B C12B 121.9 . . ? C10B C11B H11B 119.1 . . ? C12B C11B H11B 119.1 . . ? C11B C12B C13B 118.2 . . ? C11B C12B H12B 120.9 . . ? C13B C12B H12B 120.9 . . ? C14B C13B C12B 118.9 . . ? C14B C13B H13B 120.5 . . ? C12B C13B H13B 120.5 . . ? C9B C14B C13B 121.0 . . ? C9B C14B H14B 119.5 . . ? C13B C14B H14B 119.5 . . ? N8 C15 P2 109.3(2) . . ? N8 C15 H15A 109.8 . . ? P2 C15 H15A 109.8 . . ? N8 C15 H15B 109.8 . . ? P2 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? N17 C16 P1 113.0(2) . . ? N17 C16 H16A 109.0 . . ? P1 C16 H16A 109.0 . . ? N17 C16 H16B 109.0 . . ? P1 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C18 N17 C16 116.9(3) . . ? C18 N17 C24 116.9(3) . . ? C16 N17 C24 114.3(2) . . ? C19 C18 C23 118.6(3) . . ? C19 C18 N17 122.7(3) . . ? C23 C18 N17 118.4(3) . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 119.5(4) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 120.6(4) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C22 C23 C18 120.2(4) . . ? C22 C23 H23A 119.9 . . ? C18 C23 H23A 119.9 . . ? N17 C24 P2 112.9(2) . . ? N17 C24 H24A 109.0 . . ? P2 C24 H24A 109.0 . . ? N17 C24 H24B 109.0 . . ? P2 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C30 119.5(3) . . ? C26 C25 P2 121.3(2) . . ? C30 C25 P2 119.2(2) . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C28 C29 C30 119.9(3) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 C25 119.9(3) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? C32 C31 C36 119.3(3) . . ? C32 C31 P3 121.0(3) . . ? C36 C31 P3 119.7(2) . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 C31 120.0(3) . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? N38 C37 P3 114.1(2) . . ? N38 C37 H37A 108.7 . . ? P3 C37 H37A 108.7 . . ? N38 C37 H37B 108.7 . . ? P3 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C39 N38 C37 115.9(2) . . ? C39 N38 C45 116.2(2) . . ? C37 N38 C45 113.7(3) . . ? C44 C39 C40 118.5(3) . . ? C44 C39 N38 119.4(3) . . ? C40 C39 N38 121.9(3) . . ? C41 C40 C39 120.2(3) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C42 C41 C40 120.9(3) . . ? C42 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? C43 C42 C41 119.0(3) . . ? C43 C42 H42A 120.5 . . ? C41 C42 H42A 120.5 . . ? C42 C43 C44 121.0(3) . . ? C42 C43 H43A 119.5 . . ? C44 C43 H43A 119.5 . . ? C43 C44 C39 120.2(3) . . ? C43 C44 H44A 119.9 . . ? C39 C44 H44A 119.9 . . ? N38 C45 P4 112.6(2) . . ? N38 C45 H45A 109.1 . . ? P4 C45 H45A 109.1 . . ? N38 C45 H45B 109.1 . . ? P4 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? N47 C46 P3 114.1(2) . . ? N47 C46 H46A 108.7 . . ? P3 C46 H46A 108.7 . . ? N47 C46 H46B 108.7 . . ? P3 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? C48A N47 C54 119.7(4) . . ? C48A N47 C46 108.1(3) . . ? C54 N47 C46 115.8(2) . . ? C54 N47 C48B 104.3(5) . . ? C46 N47 C48B 115.4(4) . . ? C53A C48A C49A 118.5(6) . . ? C53A C48A N47 120.3(6) . . ? C49A C48A N47 121.2(6) . . ? C50A C49A C48A 121.0(7) . . ? C50A C49A H49A 119.5 . . ? C48A C49A H49A 119.5 . . ? C51A C50A C49A 119.4(7) . . ? C51A C50A H50A 120.3 . . ? C49A C50A H50A 120.3 . . ? C50A C51A C52A 122.4(6) . . ? C50A C51A H51A 118.8 . . ? C52A C51A H51A 118.8 . . ? C51A C52A C53A 117.6(7) . . ? C51A C52A H52A 121.2 . . ? C53A C52A H52A 121.2 . . ? C48A C53A C52A 121.1(7) . . ? C48A C53A H53A 119.5 . . ? C52A C53A H53A 119.5 . . ? C53B C48B C49B 121.0(11) . . ? C53B C48B N47 128.8(9) . . ? C49B C48B N47 110.0(10) . . ? C50B C49B C48B 121.2(11) . . ? C50B C49B H49B 119.4 . . ? C48B C49B H49B 119.4 . . ? C51B C50B C49B 117.3(10) . . ? C51B C50B H50B 121.3 . . ? C49B C50B H50B 121.3 . . ? C50B C51B C52B 121.3(11) . . ? C50B C51B H51B 119.3 . . ? C52B C51B H51B 119.3 . . ? C53B C52B C51B 118.4(12) . . ? C53B C52B H52B 120.8 . . ? C51B C52B H52B 120.8 . . ? C48B C53B C52B 120.6(12) . . ? C48B C53B H53B 119.7 . . ? C52B C53B H53B 119.7 . . ? N47 C54 P4 113.2(2) . . ? N47 C54 H54A 108.9 . . ? P4 C54 H54A 108.9 . . ? N47 C54 H54B 108.9 . . ? P4 C54 H54B 108.9 . . ? H54A C54 H54B 107.7 . . ? C56 C55 C60 119.1(3) . . ? C56 C55 P4 123.6(2) . . ? C60 C55 P4 117.4(2) . . ? C57 C56 C55 120.0(3) . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C58 C57 C56 120.8(4) . . ? C58 C57 H57A 119.6 . . ? C56 C57 H57A 119.6 . . ? C57 C58 C59 119.8(3) . . ? C57 C58 H58A 120.1 . . ? C59 C58 H58A 120.1 . . ? C58 C59 C60 120.1(3) . . ? C58 C59 H59A 119.9 . . ? C60 C59 H59A 119.9 . . ? C59 C60 C55 120.3(3) . . ? C59 C60 H60A 119.9 . . ? C55 C60 H60A 119.9 . . ? F6 B2 F5 85.8(10) 7_556 . ? F6 B2 F6 101.5(11) 7_556 . ? F5 B2 F6 101.3(9) . . ? F5 B2 F3 105.9(9) . . ? F6 B2 F3 120.2(12) . . ? F6 B2 F4 142.8(11) 7_556 . ? F5 B2 F4 110.3(9) . . ? F6 B2 F4 107.5(9) . . ? F3 B2 F4 111.0(8) . . ? F6 B2 B2 57.7(9) 7_556 7_556 ? F5 B2 B2 96.7(11) . 7_556 ? F3 B2 B2 80.5(10) . 7_556 ? F4 B2 B2 145.2(12) . 7_556 ? F6 B2 F3 100.3(10) 7_556 7_556 ? F5 B2 F3 84.1(7) . 7_556 ? F3 B2 F3 126.3(8) . 7_556 ? F4 B2 F3 114.2(8) . 7_556 ? B2 B2 F3 45.7(6) 7_556 7_556 ? F6 F3 B2 52.3(13) 7_556 . ? B2 F3 B2 53.7(8) . 7_556 ? F3 F6 B2 95.6(16) 7_556 7_556 ? F3 F6 B2 130.2(19) 7_556 . ? B2 F6 B2 78.5(11) 7_556 . ? F3 F6 F5 123.6(19) 7_556 7_556 ? B2 F6 F5 51.2(7) 7_556 7_556 ? B2 F6 F5 91.0(8) . 7_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.597 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.081 data_bt1194 _database_code_depnum_ccdc_archive 'CCDC 683302' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[C34H37CoN5P2]2[BF4]' _chemical_melting_point ? _chemical_formula_moiety 'C34 H37 Co N5 P2, 2(B F4)' _chemical_formula_sum 'C34 H37 B2 Co F8 N5 P2' _chemical_formula_weight 810.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' B B 0.0013 0.0007 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' 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 10.0584(4) _cell_length_b 20.1715(7) _cell_length_c 17.6050(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.1020(10) _cell_angle_gamma 90.00 _cell_volume 3566.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9863 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.90 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8346 _exptl_absorpt_correction_T_max 0.9381 _exptl_absorpt_process_details 'SADABS-2007/4 (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52775 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8183 _reflns_number_gt 6790 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _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^)+(0.0475P)^2^+1.5921P] 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 8183 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _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 C1 C 0.57877(17) 0.62962(9) 0.13663(10) 0.0194(3) Uani 1 1 d . . . H1A H 0.6103 0.6127 0.1846 0.023 Uiso 1 1 calc R . . C2 C 0.60713(18) 0.59646(9) 0.07031(11) 0.0231(4) Uani 1 1 d . . . H2A H 0.6586 0.5570 0.0730 0.028 Uiso 1 1 calc R . . C3 C 0.56054(17) 0.62086(9) 0.00023(10) 0.0214(4) Uani 1 1 d . . . H3A H 0.5792 0.5977 -0.0450 0.026 Uiso 1 1 calc R . . C4 C 0.48691(18) 0.67887(9) -0.00406(10) 0.0205(4) Uani 1 1 d . . . H4A H 0.4560 0.6957 -0.0522 0.025 Uiso 1 1 calc R . . C5 C 0.45825(18) 0.71235(9) 0.06191(10) 0.0196(4) Uani 1 1 d . . . H5A H 0.4075 0.7521 0.0590 0.024 Uiso 1 1 calc R . . C6 C 0.50399(16) 0.68765(8) 0.13259(10) 0.0159(3) Uani 1 1 d . . . C7 C 0.28099(17) 0.69669(9) 0.22207(10) 0.0183(3) Uani 1 1 d . . . H7A H 0.2237 0.7157 0.1801 0.022 Uiso 1 1 calc R . . H7B H 0.2828 0.6480 0.2151 0.022 Uiso 1 1 calc R . . C9 C 0.14227(17) 0.66347(8) 0.32767(10) 0.0173(3) Uani 1 1 d . . . C10 C 0.19116(18) 0.59897(9) 0.33897(10) 0.0214(4) Uani 1 1 d . . . H10 H 0.2758 0.5873 0.3216 0.026 Uiso 1 1 calc R . . C11 C 0.1163(2) 0.55206(9) 0.37553(11) 0.0267(4) Uani 1 1 d . . . H11 H 0.1502 0.5084 0.3829 0.032 Uiso 1 1 calc R . . C12 C -0.0076(2) 0.56814(10) 0.40149(11) 0.0293(4) Uani 1 1 d . . . H12 H -0.0579 0.5361 0.4271 0.035 Uiso 1 1 calc R . . C13 C -0.0567(2) 0.63168(10) 0.38943(11) 0.0277(4) Uani 1 1 d . . . H13 H -0.1417 0.6430 0.4067 0.033 Uiso 1 1 calc R . . C14 C 0.01661(18) 0.67916(9) 0.35240(10) 0.0205(4) Uani 1 1 d . . . H14 H -0.0190 0.7223 0.3440 0.025 Uiso 1 1 calc R . . C15 C 0.19600(17) 0.78145(8) 0.30661(10) 0.0188(3) Uani 1 1 d . . . H15A H 0.1424 0.7867 0.3518 0.023 Uiso 1 1 calc R . . H15B H 0.1443 0.7997 0.2619 0.023 Uiso 1 1 calc R . . C16 C 0.30752(17) 0.90568(8) 0.36084(10) 0.0167(3) Uani 1 1 d . . . C17 C 0.21514(17) 0.94344(9) 0.31691(10) 0.0188(3) Uani 1 1 d . . . H17 H 0.1774 0.9263 0.2703 0.023 Uiso 1 1 calc R . . C18 C 0.17884(18) 1.00605(9) 0.34161(11) 0.0222(4) Uani 1 1 d . . . H18 H 0.1144 1.0312 0.3126 0.027 Uiso 1 1 calc R . . C19 C 0.23667(18) 1.03190(9) 0.40873(11) 0.0225(4) Uani 1 1 d . . . H19 H 0.2130 1.0750 0.4251 0.027 Uiso 1 1 calc R . . C20 C 0.32877(18) 0.99476(9) 0.45166(11) 0.0223(4) Uani 1 1 d . . . H20 H 0.3687 1.0128 0.4973 0.027 Uiso 1 1 calc R . . C21 C 0.36368(17) 0.93120(9) 0.42877(10) 0.0191(3) Uani 1 1 d . . . H21 H 0.4252 0.9055 0.4592 0.023 Uiso 1 1 calc R . . C22 C 0.44945(17) 0.77393(8) 0.39299(10) 0.0172(3) Uani 1 1 d . . . H22A H 0.4618 0.7965 0.4395 0.021 Uiso 1 1 d . . . H22B H 0.3891 0.7377 0.4042 0.021 Uiso 1 1 d . . . C24 C 0.66631(17) 0.79688(8) 0.34527(10) 0.0169(3) Uani 1 1 d . . . C25 C 0.68631(17) 0.85147(9) 0.39435(10) 0.0197(4) Uani 1 1 d . . . H25 H 0.6370 0.8547 0.4387 0.024 Uiso 1 1 calc R . . C26 C 0.77686(18) 0.90041(9) 0.37868(11) 0.0224(4) Uani 1 1 d . . . H26 H 0.7885 0.9371 0.4122 0.027 Uiso 1 1 calc R . . C27 C 0.85149(18) 0.89671(9) 0.31424(11) 0.0233(4) Uani 1 1 d . . . H27 H 0.9115 0.9312 0.3028 0.028 Uiso 1 1 calc R . . C28 C 0.83673(18) 0.84211(10) 0.26739(11) 0.0230(4) Uani 1 1 d . . . H28 H 0.8896 0.8384 0.2245 0.028 Uiso 1 1 calc R . . C29 C 0.74533(17) 0.79226(9) 0.28207(10) 0.0200(4) Uani 1 1 d . . . H29 H 0.7365 0.7550 0.2492 0.024 Uiso 1 1 calc R . . C30 C 0.54373(18) 0.69645(8) 0.30446(10) 0.0180(3) Uani 1 1 d . . . H30A H 0.4902 0.6608 0.3265 0.022 Uiso 1 1 calc R . . H30B H 0.6290 0.6768 0.2901 0.022 Uiso 1 1 calc R . . C32 C 0.66228(18) 0.84998(9) 0.08965(10) 0.0192(4) Uani 1 1 d . . . C33 C 0.7597(2) 0.85832(10) 0.03244(11) 0.0276(4) Uani 1 1 d . . . H33A H 0.8393 0.8322 0.0466 0.041 Uiso 1 1 calc R . . H33B H 0.7839 0.9052 0.0290 0.041 Uiso 1 1 calc R . . H33C H 0.7216 0.8432 -0.0170 0.041 Uiso 1 1 calc R . . C35 C 0.23341(17) 0.87208(9) 0.09408(10) 0.0196(4) Uani 1 1 d . . . C36 C 0.14436(19) 0.88868(10) 0.02884(11) 0.0272(4) Uani 1 1 d . . . H36A H 0.0611 0.9067 0.0466 0.041 Uiso 1 1 calc R . . H36B H 0.1252 0.8487 -0.0014 0.041 Uiso 1 1 calc R . . H36C H 0.1869 0.9218 -0.0026 0.041 Uiso 1 1 calc R . . C38 C 0.55067(17) 0.97987(9) 0.26377(10) 0.0195(4) Uani 1 1 d . . . C39 C 0.5965(2) 1.04450(9) 0.29069(12) 0.0302(4) Uani 1 1 d . . . H39A H 0.5951 1.0461 0.3463 0.045 Uiso 1 1 calc R . . H39B H 0.5377 1.0790 0.2685 0.045 Uiso 1 1 calc R . . H39C H 0.6875 1.0520 0.2754 0.045 Uiso 1 1 calc R . . Co1 Co 0.46769(2) 0.838071(11) 0.218297(13) 0.01432(7) Uani 1 1 d . . . N8 N 0.22352(15) 0.71200(7) 0.29446(9) 0.0183(3) Uani 1 1 d . . . N23 N 0.57097(14) 0.74777(7) 0.36202(8) 0.0174(3) Uani 1 1 d . . . N31 N 0.58666(15) 0.84297(7) 0.13451(8) 0.0173(3) Uani 1 1 d . . . N34 N 0.30625(15) 0.85976(7) 0.14384(9) 0.0192(3) Uani 1 1 d . . . N37 N 0.51369(14) 0.92926(7) 0.24361(8) 0.0172(3) Uani 1 1 d . . . P1 P 0.45198(4) 0.72970(2) 0.21684(2) 0.01461(10) Uani 1 1 d . . . P2 P 0.35558(4) 0.82702(2) 0.32129(2) 0.01494(10) Uani 1 1 d . . . B1 B 0.9571(2) 0.70469(11) 0.10214(13) 0.0266(5) Uani 1 1 d . . . F1 F 1.02842(14) 0.65121(7) 0.07536(7) 0.0416(3) Uani 1 1 d . . . F2 F 1.03055(15) 0.76227(7) 0.09474(11) 0.0626(5) Uani 1 1 d . . . F3 F 0.83913(12) 0.71106(6) 0.05897(8) 0.0376(3) Uani 1 1 d . . . F4 F 0.9340(2) 0.69479(7) 0.17728(7) 0.0609(5) Uani 1 1 d . . . B2 B -0.0666(2) 1.00999(11) 0.14787(12) 0.0244(4) Uani 1 1 d . . . F5 F -0.00561(14) 0.94938(6) 0.16385(7) 0.0404(3) Uani 1 1 d . . . F6 F 0.01425(12) 1.04975(7) 0.10561(7) 0.0390(3) Uani 1 1 d . . . F7 F -0.18623(13) 1.00000(7) 0.10785(8) 0.0472(4) Uani 1 1 d . . . F8 F -0.08924(19) 1.04164(7) 0.21618(7) 0.0554(4) 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 C1 0.0208(9) 0.0183(8) 0.0190(9) 0.0009(7) 0.0015(7) 0.0011(7) C2 0.0233(9) 0.0219(9) 0.0243(9) -0.0030(7) 0.0042(7) 0.0048(7) C3 0.0205(9) 0.0254(9) 0.0186(9) -0.0053(7) 0.0051(7) -0.0026(7) C4 0.0235(9) 0.0213(9) 0.0165(8) 0.0010(7) 0.0000(7) -0.0048(7) C5 0.0221(9) 0.0161(8) 0.0206(9) -0.0004(7) 0.0000(7) 0.0000(7) C6 0.0174(8) 0.0138(8) 0.0166(8) -0.0026(6) 0.0021(6) -0.0022(6) C7 0.0184(8) 0.0166(8) 0.0200(9) -0.0041(7) 0.0036(7) -0.0028(6) C9 0.0188(8) 0.0176(8) 0.0155(8) -0.0023(6) 0.0000(6) -0.0042(6) C10 0.0213(9) 0.0204(9) 0.0220(9) -0.0020(7) -0.0019(7) -0.0014(7) C11 0.0363(11) 0.0172(9) 0.0257(10) 0.0015(7) -0.0066(8) -0.0049(8) C12 0.0380(11) 0.0253(10) 0.0248(10) 0.0025(8) 0.0043(8) -0.0124(8) C13 0.0256(10) 0.0293(10) 0.0288(10) -0.0025(8) 0.0080(8) -0.0070(8) C14 0.0222(9) 0.0187(9) 0.0207(9) -0.0023(7) 0.0018(7) -0.0029(7) C15 0.0185(8) 0.0145(8) 0.0238(9) -0.0025(7) 0.0046(7) -0.0017(6) C16 0.0178(8) 0.0124(8) 0.0203(8) -0.0010(6) 0.0061(7) -0.0012(6) C17 0.0201(8) 0.0168(8) 0.0198(8) 0.0003(7) 0.0035(7) -0.0011(7) C18 0.0222(9) 0.0182(9) 0.0265(10) 0.0024(7) 0.0056(7) 0.0027(7) C19 0.0235(9) 0.0150(8) 0.0297(10) -0.0038(7) 0.0074(8) 0.0008(7) C20 0.0218(9) 0.0206(9) 0.0247(9) -0.0070(7) 0.0036(7) -0.0038(7) C21 0.0182(8) 0.0179(8) 0.0214(9) -0.0015(7) 0.0016(7) 0.0008(7) C22 0.0208(8) 0.0160(8) 0.0149(8) 0.0008(6) 0.0021(6) 0.0001(6) C24 0.0163(8) 0.0169(8) 0.0171(8) 0.0020(6) -0.0018(6) 0.0038(6) C25 0.0186(8) 0.0207(9) 0.0197(9) -0.0008(7) -0.0008(7) 0.0038(7) C26 0.0209(9) 0.0187(9) 0.0270(10) -0.0021(7) -0.0059(7) 0.0000(7) C27 0.0180(9) 0.0243(9) 0.0271(10) 0.0045(8) -0.0035(7) -0.0020(7) C28 0.0178(9) 0.0305(10) 0.0205(9) 0.0031(7) -0.0005(7) 0.0023(7) C29 0.0189(8) 0.0212(9) 0.0194(9) -0.0017(7) -0.0025(7) 0.0035(7) C30 0.0229(9) 0.0135(8) 0.0173(8) -0.0009(6) -0.0006(7) 0.0018(7) C32 0.0215(9) 0.0159(8) 0.0197(9) -0.0011(7) -0.0022(7) 0.0012(7) C33 0.0270(10) 0.0327(11) 0.0238(10) 0.0046(8) 0.0081(8) 0.0045(8) C35 0.0198(9) 0.0179(9) 0.0215(9) 0.0011(7) 0.0034(7) 0.0004(7) C36 0.0256(10) 0.0344(11) 0.0211(9) 0.0045(8) -0.0029(8) 0.0038(8) C38 0.0189(8) 0.0186(9) 0.0208(9) 0.0027(7) -0.0007(7) 0.0007(7) C39 0.0387(11) 0.0170(9) 0.0336(11) -0.0026(8) -0.0101(9) -0.0036(8) Co1 0.01584(12) 0.01222(12) 0.01487(12) -0.00028(8) 0.00066(8) 0.00004(8) N8 0.0195(7) 0.0132(7) 0.0227(8) -0.0045(6) 0.0068(6) -0.0019(6) N23 0.0201(7) 0.0150(7) 0.0167(7) -0.0013(6) -0.0006(6) 0.0006(6) N31 0.0187(7) 0.0147(7) 0.0182(7) 0.0001(6) -0.0012(6) 0.0006(5) N34 0.0206(7) 0.0155(7) 0.0215(8) 0.0000(6) 0.0011(6) -0.0001(6) N37 0.0166(7) 0.0167(7) 0.0182(7) 0.0014(6) 0.0018(6) 0.0005(6) P1 0.0163(2) 0.0128(2) 0.0147(2) -0.00115(15) 0.00076(16) 0.00056(16) P2 0.0165(2) 0.0123(2) 0.0161(2) -0.00097(16) 0.00171(16) 0.00006(16) B1 0.0353(12) 0.0211(10) 0.0229(11) 0.0008(8) -0.0045(9) -0.0030(9) F1 0.0453(8) 0.0448(8) 0.0350(7) -0.0064(6) 0.0040(6) 0.0112(6) F2 0.0485(9) 0.0354(8) 0.0999(13) 0.0238(8) -0.0316(9) -0.0194(7) F3 0.0278(6) 0.0412(7) 0.0434(8) 0.0028(6) -0.0030(5) -0.0055(5) F4 0.1217(15) 0.0415(8) 0.0205(7) 0.0038(6) 0.0121(8) 0.0298(9) B2 0.0304(11) 0.0220(10) 0.0206(10) -0.0012(8) -0.0010(8) 0.0008(9) F5 0.0528(8) 0.0345(7) 0.0347(7) 0.0066(5) 0.0100(6) 0.0187(6) F6 0.0326(7) 0.0450(8) 0.0388(7) 0.0120(6) -0.0025(5) -0.0114(6) F7 0.0333(7) 0.0494(8) 0.0577(9) 0.0109(7) -0.0104(6) -0.0130(6) F8 0.1119(13) 0.0280(7) 0.0273(7) -0.0059(5) 0.0128(8) 0.0111(8) _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 C1 C2 1.389(2) . ? C1 C6 1.391(2) . ? C1 H1A 0.9500 . ? C2 C3 1.386(3) . ? C2 H2A 0.9500 . ? C3 C4 1.385(3) . ? C3 H3A 0.9500 . ? C4 C5 1.387(2) . ? C4 H4A 0.9500 . ? C5 C6 1.395(2) . ? C5 H5A 0.9500 . ? C6 P1 1.8103(17) . ? C7 N8 1.461(2) . ? C7 P1 1.8512(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C14 1.395(2) . ? C9 C10 1.401(2) . ? C9 N8 1.421(2) . ? C10 C11 1.389(3) . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.392(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 N8 1.446(2) . ? C15 P2 1.8555(18) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.393(2) . ? C16 C17 1.401(2) . ? C16 P2 1.8090(17) . ? C17 C18 1.391(2) . ? C17 H17 0.9500 . ? C18 C19 1.390(3) . ? C18 H18 0.9500 . ? C19 C20 1.384(3) . ? C19 H19 0.9500 . ? C20 C21 1.395(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 N23 1.463(2) . ? C22 P2 1.8716(18) . ? C22 H22A 0.9392 . ? C22 H22B 0.9769 . ? C24 C29 1.405(2) . ? C24 C25 1.407(2) . ? C24 N23 1.421(2) . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.396(3) . ? C26 H26 0.9500 . ? C27 C28 1.379(3) . ? C27 H27 0.9500 . ? C28 C29 1.396(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 N23 1.464(2) . ? C30 P1 1.8780(18) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C32 N31 1.134(2) . ? C32 C33 1.453(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 N34 1.139(2) . ? C35 C36 1.457(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C38 N37 1.137(2) . ? C38 C39 1.454(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? Co1 N37 1.9427(15) . ? Co1 N31 1.9516(15) . ? Co1 N34 2.0776(15) . ? Co1 P1 2.1918(5) . ? Co1 P2 2.1978(5) . ? B1 F4 1.370(3) . ? B1 F3 1.380(3) . ? B1 F2 1.386(3) . ? B1 F1 1.392(3) . ? B2 F7 1.376(3) . ? B2 F6 1.387(3) . ? B2 F5 1.390(2) . ? B2 F8 1.391(2) . ? 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 C2 C1 C6 119.83(16) . . ? C2 C1 H1A 120.1 . . ? C6 C1 H1A 120.1 . . ? C3 C2 C1 120.16(17) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C4 C3 C2 120.18(17) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 120.03(17) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 119.96(16) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C1 C6 C5 119.83(16) . . ? C1 C6 P1 122.13(13) . . ? C5 C6 P1 117.87(13) . . ? N8 C7 P1 112.33(12) . . ? N8 C7 H7A 109.1 . . ? P1 C7 H7A 109.1 . . ? N8 C7 H7B 109.1 . . ? P1 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C14 C9 C10 118.89(16) . . ? C14 C9 N8 121.53(16) . . ? C10 C9 N8 119.52(16) . . ? C11 C10 C9 120.22(17) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.81(18) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 118.97(18) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 120.97(18) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C9 120.12(17) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? N8 C15 P2 109.23(12) . . ? N8 C15 H15A 109.8 . . ? P2 C15 H15A 109.8 . . ? N8 C15 H15B 109.8 . . ? P2 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? C21 C16 C17 119.92(16) . . ? C21 C16 P2 123.38(13) . . ? C17 C16 P2 116.56(13) . . ? C18 C17 C16 119.89(17) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 120.11(17) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 119.88(17) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.76(17) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C16 C21 C20 119.41(17) . . ? C16 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N23 C22 P2 110.86(11) . . ? N23 C22 H22A 115.2 . . ? P2 C22 H22A 110.4 . . ? N23 C22 H22B 110.3 . . ? P2 C22 H22B 105.5 . . ? H22A C22 H22B 103.9 . . ? C29 C24 C25 118.02(16) . . ? C29 C24 N23 122.36(15) . . ? C25 C24 N23 119.59(15) . . ? C26 C25 C24 120.71(17) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.90(17) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 118.92(17) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 121.01(18) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C24 120.35(17) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? N23 C30 P1 112.41(11) . . ? N23 C30 H30A 109.1 . . ? P1 C30 H30A 109.1 . . ? N23 C30 H30B 109.1 . . ? P1 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? N31 C32 C33 179.4(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N34 C35 C36 177.9(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N37 C38 C39 179.0(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N37 Co1 N31 88.69(6) . . ? N37 Co1 N34 96.53(6) . . ? N31 Co1 N34 90.15(6) . . ? N37 Co1 P1 164.41(5) . . ? N31 Co1 P1 95.08(4) . . ? N34 Co1 P1 98.58(4) . . ? N37 Co1 P2 91.91(4) . . ? N31 Co1 P2 172.61(4) . . ? N34 Co1 P2 97.09(4) . . ? P1 Co1 P2 82.450(17) . . ? C9 N8 C15 119.18(14) . . ? C9 N8 C7 118.48(13) . . ? C15 N8 C7 114.95(14) . . ? C24 N23 C22 114.37(13) . . ? C24 N23 C30 116.90(14) . . ? C22 N23 C30 112.58(14) . . ? C32 N31 Co1 173.73(15) . . ? C35 N34 Co1 168.47(14) . . ? C38 N37 Co1 172.65(15) . . ? C6 P1 C7 100.53(8) . . ? C6 P1 C30 110.77(8) . . ? C7 P1 C30 104.31(8) . . ? C6 P1 Co1 116.94(6) . . ? C7 P1 Co1 115.14(6) . . ? C30 P1 Co1 108.34(6) . . ? C16 P2 C15 103.94(8) . . ? C16 P2 C22 112.20(8) . . ? C15 P2 C22 102.21(8) . . ? C16 P2 Co1 112.85(6) . . ? C15 P2 Co1 114.45(6) . . ? C22 P2 Co1 110.60(6) . . ? F4 B1 F3 111.1(2) . . ? F4 B1 F2 109.39(19) . . ? F3 B1 F2 108.47(17) . . ? F4 B1 F1 109.38(17) . . ? F3 B1 F1 109.21(17) . . ? F2 B1 F1 109.3(2) . . ? F7 B2 F6 109.39(17) . . ? F7 B2 F5 109.81(17) . . ? F6 B2 F5 110.63(17) . . ? F7 B2 F8 109.27(19) . . ? F6 B2 F8 109.06(17) . . ? F5 B2 F8 108.65(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.466 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.065