Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Simon A. Llewellyn' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Rd Oxford OX1 3QR ; _publ_contact_author_email simon.llewellyn@chem.ox.ac.uk loop_ _publ_author_name _publ_author_address 'Llewellyn, Simon A.' ;Inorganic Chemistry Laboratory South Parks Rd Oxford OX1 3QR ; 'Green, Malcolm L. H.' ;Inorganic Chemistry Laboratory South Parks Rd Oxford OX1 3QR ; 'Cowley, Andrew R.' ;Central Chemical Laboratory South Parks Rd Oxford ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; B(C6F5)3-Adducts of Transition Metal Acyl Compounds ; data_ARC487 _database_code_depnum_ccdc_archive 'CCDC 287089' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #============================================================= _cell_length_a 20.2640(2) _cell_angle_alpha 90 _cell_length_b 13.0854(2) _cell_angle_beta 93.9521(5) _cell_length_c 25.3366(2) _cell_angle_gamma 90 _cell_volume 6702.34(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Co ' 0.2990 0.9730 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C72 H26 B2 Co1 F36 O4 P2 ' _chemical_formula_moiety ' C72 H26 B2 Co1 F36 O4 P2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 1781.43 _cell_measurement_reflns_used 87004 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' dark blue ' _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_meas ? _exptl_crystal_F_000 3524 _exptl_absorpt_coefficient_mu 0.458 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 87004 _reflns_number_total 15169 #15818 unique reflections includin absences _diffrn_reflns_av_R_equivalents 0.042 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -26 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _refine_diff_density_min -0.77 _refine_diff_density_max 1.14 _refine_ls_number_reflns 10011 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1062 #_refine_ls_R_factor_ref 0.0502 _refine_ls_wR_factor_ref 0.0597 _refine_ls_goodness_of_fit_ref 1.0690 #_reflns_number_all 15169 _refine_ls_R_factor_all 0.0800 _refine_ls_wR_factor_all 0.0702 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 10011 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_gt 0.0597 _refine_ls_shift/su_max 0.023388 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.43 1.08 0.980 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type Co1 Co 0.248014(19) 0.30475(3) 0.361538(14) 0.0276 1.0000 Uani O1 O 0.26509(12) 0.36162(17) 0.29397(8) 0.0393 1.0000 Uani P1 P 0.26969(4) 0.39127(6) 0.23721(3) 0.0290 1.0000 Uani C1 C 0.26747(14) 0.5270(2) 0.23003(12) 0.0340 1.0000 Uani C2 C 0.29125(17) 0.5879(3) 0.27260(14) 0.0439 1.0000 Uani C3 C 0.2897(2) 0.6941(3) 0.26810(19) 0.0584 1.0000 Uani C4 C 0.2643(2) 0.7359(3) 0.2204(2) 0.0586 1.0000 Uani C5 C 0.2410(2) 0.6783(3) 0.17844(18) 0.0561 1.0000 Uani C6 C 0.24224(18) 0.5729(3) 0.18325(14) 0.0445 1.0000 Uani F1 F 0.26205(16) 0.83844(18) 0.21631(15) 0.0902 1.0000 Uani C7 C 0.20090(15) 0.3399(2) 0.19787(12) 0.0327 1.0000 Uani C8 C 0.13960(18) 0.3373(3) 0.21968(15) 0.0508 1.0000 Uani C9 C 0.08463(18) 0.2967(4) 0.19190(17) 0.0576 1.0000 Uani C10 C 0.09293(19) 0.2575(4) 0.14257(16) 0.0606 1.0000 Uani C11 C 0.1525(2) 0.2557(4) 0.12005(15) 0.0653 1.0000 Uani C12 C 0.20690(16) 0.2987(3) 0.14807(13) 0.0467 1.0000 Uani F2 F 0.03994(13) 0.2121(3) 0.11625(12) 0.0976 1.0000 Uani C13 C 0.34386(14) 0.3428(2) 0.21203(11) 0.0314 1.0000 Uani C14 C 0.36667(16) 0.2473(2) 0.23001(12) 0.0373 1.0000 Uani C15 C 0.42188(16) 0.2038(3) 0.20980(15) 0.0436 1.0000 Uani C16 C 0.45255(17) 0.2568(3) 0.17179(16) 0.0509 1.0000 Uani C17 C 0.43256(19) 0.3519(4) 0.15366(16) 0.0570 1.0000 Uani C18 C 0.37753(18) 0.3957(3) 0.17455(14) 0.0479 1.0000 Uani F3 F 0.50564(12) 0.2133(2) 0.15109(12) 0.0709 1.0000 Uani O2 O 0.22158(11) 0.42599(16) 0.39882(9) 0.0385 1.0000 Uani P2 P 0.18089(4) 0.50607(6) 0.42318(3) 0.0307 1.0000 Uani C19 C 0.15368(13) 0.5989(2) 0.37558(11) 0.0309 1.0000 Uani C20 C 0.14404(18) 0.5681(3) 0.32329(13) 0.0443 1.0000 Uani C21 C 0.11681(19) 0.6336(3) 0.28476(13) 0.0518 1.0000 Uani C22 C 0.09977(16) 0.7292(3) 0.29951(14) 0.0442 1.0000 Uani C23 C 0.10807(17) 0.7636(3) 0.35083(15) 0.0450 1.0000 Uani C24 C 0.13506(16) 0.6979(2) 0.38898(13) 0.0385 1.0000 Uani F4 F 0.07319(12) 0.79384(19) 0.26196(9) 0.0624 1.0000 Uani C25 C 0.22915(13) 0.5622(2) 0.47691(11) 0.0289 1.0000 Uani C26 C 0.29473(15) 0.5856(2) 0.46920(13) 0.0370 1.0000 Uani C27 C 0.33600(16) 0.6263(3) 0.51040(15) 0.0447 1.0000 Uani C28 C 0.30952(18) 0.6415(3) 0.55843(15) 0.0458 1.0000 Uani C29 C 0.2462(2) 0.6176(3) 0.56768(15) 0.0516 1.0000 Uani C30 C 0.20544(17) 0.5780(3) 0.52664(13) 0.0427 1.0000 Uani F5 F 0.34872(12) 0.6814(2) 0.59861(10) 0.0666 1.0000 Uani C31 C 0.10730(13) 0.4511(2) 0.44640(11) 0.0276 1.0000 Uani C32 C 0.11322(14) 0.3670(2) 0.48031(12) 0.0334 1.0000 Uani C33 C 0.05758(15) 0.3155(2) 0.49509(12) 0.0353 1.0000 Uani C34 C -0.00336(14) 0.3508(2) 0.47588(11) 0.0328 1.0000 Uani C35 C -0.01141(14) 0.4325(2) 0.44262(12) 0.0347 1.0000 Uani C36 C 0.04430(14) 0.4832(2) 0.42768(11) 0.0320 1.0000 Uani F6 F -0.05781(9) 0.30114(16) 0.49090(8) 0.0446 1.0000 Uani O3 O 0.31344(10) 0.21548(17) 0.39628(9) 0.0354 1.0000 Uani B1 B 0.38280(16) 0.2155(2) 0.41928(12) 0.0283 1.0000 Uani C37 C 0.40027(14) 0.0903(2) 0.42750(12) 0.0331 1.0000 Uani C38 C 0.39343(14) 0.0257(2) 0.38310(12) 0.0357 1.0000 Uani C39 C 0.40099(16) -0.0792(3) 0.38624(14) 0.0406 1.0000 Uani C40 C 0.41626(16) -0.1240(3) 0.43444(14) 0.0428 1.0000 Uani C41 C 0.42310(16) -0.0647(3) 0.47924(13) 0.0394 1.0000 Uani C42 C 0.41468(15) 0.0402(3) 0.47508(12) 0.0364 1.0000 Uani F7 F 0.37968(10) 0.06445(15) 0.33518(8) 0.0469 1.0000 Uani F8 F 0.39294(12) -0.13679(16) 0.34239(9) 0.0592 1.0000 Uani F9 F 0.42314(12) -0.22628(16) 0.43834(9) 0.0565 1.0000 Uani F10 F 0.43691(12) -0.10892(17) 0.52651(9) 0.0568 1.0000 Uani F11 F 0.42212(11) 0.09167(17) 0.52090(8) 0.0506 1.0000 Uani C43 C 0.39162(14) 0.2809(2) 0.47464(12) 0.0333 1.0000 Uani C44 C 0.33996(16) 0.2944(3) 0.50717(13) 0.0402 1.0000 Uani C45 C 0.34389(18) 0.3536(3) 0.55232(14) 0.0454 1.0000 Uani C46 C 0.40216(19) 0.4033(2) 0.56752(13) 0.0428 1.0000 Uani C47 C 0.45533(17) 0.3915(2) 0.53756(13) 0.0397 1.0000 Uani C48 C 0.44944(15) 0.3317(2) 0.49248(12) 0.0350 1.0000 Uani F12 F 0.28185(11) 0.2465(2) 0.49624(10) 0.0621 1.0000 Uani F13 F 0.29176(13) 0.3637(2) 0.58114(10) 0.0681 1.0000 Uani F14 F 0.40640(13) 0.46171(17) 0.61131(9) 0.0580 1.0000 Uani F15 F 0.51351(11) 0.43793(17) 0.55171(9) 0.0537 1.0000 Uani F16 F 0.50500(9) 0.32199(17) 0.46587(8) 0.0471 1.0000 Uani C49 C 0.43140(14) 0.2673(2) 0.37566(12) 0.0341 1.0000 Uani C50 C 0.41691(14) 0.3659(3) 0.35899(12) 0.0373 1.0000 Uani C51 C 0.45298(17) 0.4218(3) 0.32481(14) 0.0452 1.0000 Uani C52 C 0.50770(18) 0.3771(3) 0.30569(14) 0.0500 1.0000 Uani C53 C 0.52538(16) 0.2804(3) 0.32022(14) 0.0486 1.0000 Uani C54 C 0.48764(16) 0.2267(3) 0.35505(13) 0.0398 1.0000 Uani F17 F 0.36391(9) 0.41304(15) 0.37791(8) 0.0457 1.0000 Uani F18 F 0.43550(13) 0.51556(19) 0.31054(11) 0.0688 1.0000 Uani F19 F 0.54370(13) 0.4289(2) 0.27164(10) 0.0713 1.0000 Uani F20 F 0.57827(11) 0.2350(2) 0.30062(10) 0.0701 1.0000 Uani F21 F 0.50996(10) 0.13232(18) 0.36778(9) 0.0554 1.0000 Uani O4 O 0.16291(10) 0.22634(16) 0.36745(8) 0.0303 1.0000 Uani B2 B 0.13550(15) 0.1173(2) 0.36301(12) 0.0266 1.0000 Uani C55 C 0.18382(14) 0.0462(2) 0.40323(11) 0.0299 1.0000 Uani C56 C 0.19009(14) 0.0707(2) 0.45705(12) 0.0318 1.0000 Uani C57 C 0.22437(15) 0.0134(3) 0.49548(12) 0.0371 1.0000 Uani C58 C 0.25376(16) -0.0759(3) 0.48093(15) 0.0437 1.0000 Uani C59 C 0.24958(16) -0.1049(2) 0.42854(15) 0.0412 1.0000 Uani C60 C 0.21621(15) -0.0432(2) 0.39130(12) 0.0342 1.0000 Uani F22 F 0.15828(9) 0.15361(14) 0.47429(7) 0.0373 1.0000 Uani F23 F 0.22819(11) 0.04279(17) 0.54638(8) 0.0505 1.0000 Uani F24 F 0.28633(11) -0.13426(17) 0.51790(10) 0.0592 1.0000 Uani F25 F 0.27790(10) -0.19244(14) 0.41412(10) 0.0530 1.0000 Uani F26 F 0.21597(10) -0.07743(14) 0.34085(8) 0.0436 1.0000 Uani C61 C 0.13494(15) 0.0824(2) 0.30047(11) 0.0306 1.0000 Uani C62 C 0.19175(14) 0.0934(2) 0.27359(12) 0.0323 1.0000 Uani C63 C 0.19754(16) 0.0666(2) 0.22168(12) 0.0375 1.0000 Uani C64 C 0.14343(18) 0.0269(3) 0.19313(12) 0.0415 1.0000 Uani C65 C 0.08554(17) 0.0139(3) 0.21717(13) 0.0402 1.0000 Uani C66 C 0.08237(15) 0.0400(2) 0.26991(12) 0.0348 1.0000 Uani F27 F 0.24707(8) 0.13086(14) 0.30040(7) 0.0371 1.0000 Uani F28 F 0.25471(10) 0.07860(17) 0.19872(8) 0.0490 1.0000 Uani F29 F 0.14707(12) 0.00212(19) 0.14183(8) 0.0588 1.0000 Uani F30 F 0.03176(10) -0.02446(18) 0.18971(8) 0.0543 1.0000 Uani F31 F 0.02348(9) 0.02048(16) 0.29011(8) 0.0452 1.0000 Uani C67 C 0.05879(14) 0.1184(2) 0.38253(11) 0.0288 1.0000 Uani C68 C 0.01460(15) 0.1944(2) 0.36658(11) 0.0326 1.0000 Uani C69 C -0.05051(15) 0.1988(3) 0.37937(12) 0.0371 1.0000 Uani C70 C -0.07461(14) 0.1223(3) 0.41032(13) 0.0396 1.0000 Uani C71 C -0.03363(15) 0.0435(3) 0.42659(12) 0.0374 1.0000 Uani C72 C 0.03109(14) 0.0426(2) 0.41266(11) 0.0316 1.0000 Uani F32 F 0.03461(9) 0.27182(15) 0.33563(8) 0.0440 1.0000 Uani F33 F -0.09011(9) 0.27621(17) 0.36316(9) 0.0513 1.0000 Uani F34 F -0.13721(9) 0.12578(19) 0.42445(9) 0.0544 1.0000 Uani F35 F -0.05667(10) -0.03292(17) 0.45593(9) 0.0523 1.0000 Uani F36 F 0.06664(9) -0.04043(14) 0.42916(8) 0.0446 1.0000 Uani H1 H 0.292(4) 0.163(7) 0.401(3) 0.14(3) 1.0000 Uiso H2 H 0.144(4) 0.264(7) 0.381(3) 0.14(3) 1.0000 Uiso H21 H 0.3094 0.5552 0.3062 0.0526 1.0000 Uiso H31 H 0.3063 0.7388 0.2982 0.0700 1.0000 Uiso H51 H 0.2234 0.7114 0.1448 0.0670 1.0000 Uiso H61 H 0.2249 0.5294 0.1529 0.0533 1.0000 Uiso H81 H 0.1353 0.3652 0.2560 0.0618 1.0000 Uiso H91 H 0.0404 0.2959 0.2072 0.0698 1.0000 Uiso H111 H 0.1567 0.2243 0.0845 0.0785 1.0000 Uiso H121 H 0.2507 0.3000 0.1322 0.0562 1.0000 Uiso H141 H 0.3430 0.2102 0.2576 0.0448 1.0000 Uiso H151 H 0.4389 0.1358 0.2225 0.0527 1.0000 Uiso H171 H 0.4569 0.3883 0.1263 0.0694 1.0000 Uiso H181 H 0.3622 0.4651 0.1627 0.0581 1.0000 Uiso H201 H 0.1570 0.4973 0.3132 0.0533 1.0000 Uiso H211 H 0.1099 0.6110 0.2471 0.0624 1.0000 Uiso H231 H 0.0948 0.8346 0.3602 0.0539 1.0000 Uiso H241 H 0.1414 0.7213 0.4266 0.0462 1.0000 Uiso H261 H 0.3125 0.5732 0.4339 0.0446 1.0000 Uiso H271 H 0.3831 0.6438 0.5052 0.0534 1.0000 Uiso H291 H 0.2293 0.6284 0.6034 0.0620 1.0000 Uiso H301 H 0.1585 0.5606 0.5327 0.0517 1.0000 Uiso H321 H 0.1581 0.3436 0.4941 0.0400 1.0000 Uiso H331 H 0.0616 0.2546 0.5190 0.0425 1.0000 Uiso H351 H -0.0566 0.4553 0.4293 0.0416 1.0000 Uiso H361 H 0.0394 0.5433 0.4033 0.0385 1.0000 Uiso 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 0.03269(19) 0.02535(18) 0.02548(17) 0.00031(14) 0.00720(14) -0.00015(15) O1 0.0491(13) 0.0428(12) 0.0270(10) 0.0024(9) 0.0108(9) -0.0048(10) P1 0.0313(4) 0.0307(4) 0.0259(3) 0.0014(3) 0.0069(3) -0.0031(3) C1 0.0318(14) 0.0318(14) 0.0392(16) 0.0009(12) 0.0072(12) -0.0011(12) C2 0.0445(18) 0.0379(17) 0.0491(18) -0.0044(14) 0.0017(15) -0.0059(14) C3 0.053(2) 0.0425(19) 0.079(3) -0.0137(19) 0.003(2) -0.0073(17) C4 0.051(2) 0.0326(17) 0.092(3) 0.0074(19) 0.006(2) -0.0009(16) C5 0.056(2) 0.0406(19) 0.071(2) 0.0157(18) -0.0030(19) -0.0038(16) C6 0.0456(18) 0.0404(17) 0.0473(18) 0.0120(14) 0.0012(15) -0.0034(14) F1 0.095(2) 0.0298(11) 0.144(3) 0.0103(14) -0.0022(19) -0.0034(12) C7 0.0318(14) 0.0321(14) 0.0349(14) -0.0016(11) 0.0070(11) -0.0013(11) C8 0.0410(18) 0.063(2) 0.0502(19) -0.0191(17) 0.0182(15) -0.0122(16) C9 0.0340(17) 0.075(3) 0.065(2) -0.015(2) 0.0149(16) -0.0132(17) C10 0.0355(18) 0.094(3) 0.052(2) -0.008(2) 0.0005(16) -0.020(2) C11 0.044(2) 0.110(4) 0.0416(19) -0.021(2) 0.0040(16) -0.018(2) C12 0.0317(15) 0.075(2) 0.0336(15) -0.0057(16) 0.0052(12) -0.0093(16) F2 0.0465(13) 0.173(3) 0.0731(17) -0.0367(19) 0.0008(12) -0.0425(17) C13 0.0283(13) 0.0364(15) 0.0297(13) -0.0018(11) 0.0030(11) -0.0038(11) C14 0.0392(16) 0.0348(16) 0.0380(15) -0.0017(12) 0.0036(13) -0.0047(13) C15 0.0366(16) 0.0344(16) 0.061(2) -0.0096(15) 0.0089(15) 0.0002(13) C16 0.0346(16) 0.063(2) 0.056(2) -0.0173(18) 0.0141(15) -0.0006(16) C17 0.0406(19) 0.076(3) 0.057(2) 0.012(2) 0.0218(16) 0.0027(18) C18 0.0403(17) 0.057(2) 0.0484(19) 0.0145(16) 0.0140(14) 0.0028(15) F3 0.0443(12) 0.0776(17) 0.0942(18) -0.0183(14) 0.0285(12) 0.0063(11) O2 0.0342(11) 0.0318(10) 0.0506(13) -0.0116(9) 0.0094(9) 0.0019(8) P2 0.0274(3) 0.0291(3) 0.0358(4) -0.0037(3) 0.0050(3) -0.0010(3) C19 0.0248(13) 0.0331(14) 0.0355(14) -0.0018(11) 0.0072(11) -0.0039(11) C20 0.0471(19) 0.0498(19) 0.0363(16) -0.0065(14) 0.0050(14) 0.0108(15) C21 0.0459(19) 0.077(3) 0.0335(16) 0.0002(17) 0.0067(14) 0.0113(18) C22 0.0307(15) 0.0502(19) 0.0523(19) 0.0197(16) 0.0063(14) 0.0001(14) C23 0.0422(18) 0.0336(16) 0.059(2) 0.0074(15) 0.0014(15) -0.0071(14) C24 0.0416(16) 0.0301(14) 0.0437(16) -0.0006(13) 0.0030(13) -0.0086(13) F4 0.0535(13) 0.0720(15) 0.0611(13) 0.0294(12) 0.0001(10) 0.0036(11) C25 0.0254(13) 0.0249(13) 0.0366(14) -0.0029(11) 0.0023(11) -0.0012(10) C26 0.0298(14) 0.0400(16) 0.0416(16) 0.0005(13) 0.0058(12) -0.0051(12) C27 0.0277(14) 0.0417(17) 0.064(2) -0.0002(15) -0.0017(14) -0.0067(13) C28 0.0478(19) 0.0354(16) 0.0521(19) -0.0098(14) -0.0121(15) -0.0031(14) C29 0.055(2) 0.054(2) 0.0457(19) -0.0184(16) 0.0049(16) -0.0121(17) C30 0.0373(16) 0.0480(18) 0.0439(17) -0.0147(14) 0.0113(13) -0.0091(14) F5 0.0632(14) 0.0684(15) 0.0646(14) -0.0170(12) -0.0212(11) -0.0163(12) C31 0.0280(13) 0.0256(13) 0.0296(13) -0.0036(10) 0.0046(10) -0.0012(10) C32 0.0291(14) 0.0348(15) 0.0362(15) 0.0036(12) 0.0014(11) 0.0014(12) C33 0.0372(15) 0.0320(14) 0.0371(15) 0.0037(12) 0.0065(12) -0.0038(12) C34 0.0260(13) 0.0407(15) 0.0328(14) -0.0066(12) 0.0108(11) -0.0073(12) C35 0.0256(13) 0.0442(17) 0.0342(14) -0.0012(12) 0.0023(11) 0.0014(12) C36 0.0278(13) 0.0349(15) 0.0335(14) -0.0015(12) 0.0022(11) 0.0011(11) F6 0.0334(9) 0.0527(11) 0.0494(10) -0.0002(9) 0.0141(8) -0.0114(8) O3 0.0272(10) 0.0327(11) 0.0455(12) 0.0021(9) -0.0026(9) -0.0079(8) B1 0.0305(15) 0.0281(15) 0.0261(14) 0.0021(11) -0.0002(12) -0.0131(12) C37 0.0236(13) 0.0341(15) 0.0416(15) 0.0011(12) 0.0026(11) 0.0024(11) C38 0.0287(14) 0.0385(16) 0.0398(16) -0.0007(12) 0.0004(12) 0.0032(12) C39 0.0383(16) 0.0361(16) 0.0473(18) -0.0065(13) 0.0025(14) 0.0042(13) C40 0.0367(16) 0.0376(17) 0.0545(19) 0.0038(14) 0.0050(14) 0.0055(13) C41 0.0315(15) 0.0411(17) 0.0452(17) 0.0104(14) -0.0006(13) 0.0040(13) C42 0.0290(14) 0.0440(17) 0.0359(15) -0.0017(13) -0.0009(12) 0.0010(12) F7 0.0527(11) 0.0439(11) 0.0432(10) -0.0032(8) -0.0026(9) 0.0058(9) F8 0.0738(15) 0.0439(11) 0.0594(13) -0.0129(10) 0.0000(11) 0.0083(11) F9 0.0663(14) 0.0360(10) 0.0674(14) 0.0050(9) 0.0057(11) 0.0149(10) F10 0.0632(13) 0.0510(12) 0.0556(12) 0.0136(10) -0.0007(10) 0.0084(10) F11 0.0563(12) 0.0522(12) 0.0425(10) 0.0003(9) -0.0037(9) 0.0071(10) C43 0.0299(14) 0.0314(14) 0.0384(15) 0.0033(12) 0.0007(12) -0.0020(11) C44 0.0354(16) 0.0405(17) 0.0445(17) 0.0031(13) 0.0017(13) -0.0057(13) C45 0.0495(19) 0.0429(18) 0.0451(18) 0.0056(15) 0.0136(15) 0.0102(15) C46 0.061(2) 0.0309(15) 0.0360(16) -0.0028(12) -0.0009(15) 0.0037(14) C47 0.0448(18) 0.0328(15) 0.0408(16) 0.0029(13) -0.0025(13) -0.0052(13) C48 0.0314(14) 0.0340(15) 0.0394(15) 0.0038(12) 0.0019(12) -0.0032(11) F12 0.0394(11) 0.0817(16) 0.0668(14) -0.0096(12) 0.0164(10) -0.0186(11) F13 0.0626(14) 0.0813(17) 0.0640(14) -0.0059(12) 0.0313(12) 0.0005(13) F14 0.0814(16) 0.0468(12) 0.0457(11) -0.0110(9) 0.0032(10) 0.0076(11) F15 0.0534(12) 0.0530(12) 0.0536(12) -0.0071(10) -0.0045(9) -0.0145(10) F16 0.0283(9) 0.0640(13) 0.0490(11) -0.0090(9) 0.0022(8) -0.0053(8) C49 0.0263(13) 0.0417(16) 0.0339(14) -0.0054(12) -0.0012(11) -0.0053(12) C50 0.0272(14) 0.0455(17) 0.0390(16) -0.0025(13) 0.0005(12) -0.0064(12) C51 0.0394(17) 0.0472(19) 0.0485(18) 0.0046(15) -0.0001(14) -0.0136(14) C52 0.0421(18) 0.066(2) 0.0425(18) 0.0017(16) 0.0050(14) -0.0253(17) C53 0.0293(15) 0.071(2) 0.0465(18) -0.0112(17) 0.0098(14) -0.0104(16) C54 0.0321(15) 0.0449(17) 0.0420(16) -0.0046(14) 0.0004(13) -0.0007(13) F17 0.0395(10) 0.0373(10) 0.0603(12) 0.0022(9) 0.0038(9) -0.0001(8) F18 0.0681(15) 0.0568(14) 0.0822(17) 0.0214(12) 0.0096(13) -0.0133(12) F19 0.0618(14) 0.0906(18) 0.0644(14) 0.0075(13) 0.0249(12) -0.0305(13) F20 0.0436(12) 0.100(2) 0.0689(15) -0.0158(14) 0.0225(11) -0.0052(12) F21 0.0366(10) 0.0608(13) 0.0700(14) 0.0011(11) 0.0126(9) 0.0091(9) O4 0.0319(10) 0.0242(9) 0.0359(10) -0.0030(8) 0.0099(8) -0.0018(8) B2 0.0274(14) 0.0230(14) 0.0298(14) -0.0015(11) 0.0045(11) -0.0022(11) C55 0.0263(13) 0.0277(13) 0.0362(14) -0.0001(11) 0.0064(11) -0.0054(11) C56 0.0274(13) 0.0294(13) 0.0388(15) -0.0011(11) 0.0041(11) -0.0043(11) C57 0.0331(15) 0.0427(17) 0.0353(15) 0.0044(13) 0.0007(12) -0.0058(13) C58 0.0327(16) 0.0422(17) 0.056(2) 0.0176(15) 0.0007(14) -0.0021(13) C59 0.0354(16) 0.0287(15) 0.060(2) 0.0064(14) 0.0095(14) 0.0026(12) C60 0.0332(14) 0.0288(14) 0.0411(16) -0.0002(12) 0.0079(12) -0.0021(12) F22 0.0380(9) 0.0379(9) 0.0364(9) -0.0073(7) 0.0048(7) 0.0015(7) F23 0.0554(12) 0.0596(13) 0.0357(10) 0.0053(9) -0.0040(8) -0.0037(10) F24 0.0540(12) 0.0527(12) 0.0690(14) 0.0236(11) -0.0091(10) 0.0068(10) F25 0.0482(11) 0.0309(9) 0.0803(15) 0.0072(10) 0.0078(10) 0.0104(8) F26 0.0515(11) 0.0335(9) 0.0472(10) -0.0037(8) 0.0126(8) 0.0054(8) C61 0.0334(14) 0.0264(13) 0.0325(14) -0.0012(11) 0.0062(11) -0.0031(11) C62 0.0314(14) 0.0306(14) 0.0354(14) -0.0028(11) 0.0047(11) -0.0009(11) C63 0.0408(16) 0.0380(16) 0.0348(15) -0.0052(12) 0.0104(13) -0.0018(13) C64 0.0535(19) 0.0455(18) 0.0261(14) -0.0081(13) 0.0071(13) -0.0047(15) C65 0.0434(17) 0.0396(16) 0.0371(16) -0.0089(13) -0.0002(13) -0.0066(14) C66 0.0348(15) 0.0338(15) 0.0364(15) -0.0029(12) 0.0061(12) -0.0040(12) F27 0.0313(8) 0.0435(10) 0.0372(9) -0.0061(7) 0.0082(7) -0.0067(7) F28 0.0449(11) 0.0614(12) 0.0429(10) -0.0104(9) 0.0194(9) -0.0056(9) F29 0.0668(14) 0.0764(15) 0.0343(10) -0.0192(10) 0.0119(9) -0.0101(12) F30 0.0487(11) 0.0692(14) 0.0441(11) -0.0168(10) -0.0024(9) -0.0145(10) F31 0.0356(9) 0.0554(11) 0.0456(10) -0.0115(9) 0.0106(8) -0.0145(8) C67 0.0287(13) 0.0310(13) 0.0273(13) -0.0041(10) 0.0057(10) -0.0050(11) C68 0.0315(14) 0.0332(14) 0.0331(14) 0.0010(12) 0.0021(11) -0.0036(12) C69 0.0282(14) 0.0427(16) 0.0400(15) -0.0047(13) -0.0003(12) 0.0027(12) C70 0.0237(13) 0.0550(19) 0.0404(16) -0.0080(14) 0.0046(12) -0.0037(13) C71 0.0331(15) 0.0453(17) 0.0344(15) 0.0015(13) 0.0058(12) -0.0116(13) C72 0.0329(14) 0.0309(14) 0.0312(14) 0.0000(11) 0.0043(11) -0.0028(11) F32 0.0350(9) 0.0417(10) 0.0553(11) 0.0166(9) 0.0043(8) 0.0007(8) F33 0.0317(9) 0.0526(12) 0.0690(13) 0.0038(10) -0.0011(9) 0.0085(8) F34 0.0243(9) 0.0778(15) 0.0621(12) -0.0013(11) 0.0119(8) -0.0051(9) F35 0.0406(10) 0.0618(13) 0.0560(12) 0.0155(10) 0.0152(9) -0.0134(9) F36 0.0395(10) 0.0362(9) 0.0595(12) 0.0130(8) 0.0129(9) -0.0011(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . O1 . 1.920(2) yes Co1 . O2 . 1.941(2) yes Co1 . O3 . 1.933(2) yes Co1 . O4 . 2.021(2) yes O1 . P1 . 1.499(2) yes P1 . C1 . 1.786(3) yes P1 . C7 . 1.788(3) yes P1 . C13 . 1.789(3) yes C1 . C2 . 1.399(5) yes C1 . C6 . 1.394(5) yes C2 . C3 . 1.395(5) yes C2 . H21 . 1.000 no C3 . C4 . 1.392(6) yes C3 . H31 . 1.000 no C4 . C5 . 1.361(6) yes C4 . F1 . 1.347(5) yes C5 . C6 . 1.384(5) yes C5 . H51 . 1.000 no C6 . H61 . 1.000 no C7 . C8 . 1.394(4) yes C7 . C12 . 1.385(4) yes C8 . C9 . 1.382(5) yes C8 . H81 . 1.000 no C9 . C10 . 1.372(6) yes C9 . H91 . 1.000 no C10 . C11 . 1.371(6) yes C10 . F2 . 1.361(4) yes C11 . C12 . 1.388(5) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C13 . C14 . 1.398(4) yes C13 . C18 . 1.392(4) yes C14 . C15 . 1.384(5) yes C14 . H141 . 1.000 no C15 . C16 . 1.370(5) yes C15 . H151 . 1.000 no C16 . C17 . 1.377(6) yes C16 . F3 . 1.354(4) yes C17 . C18 . 1.391(5) yes C17 . H171 . 1.000 no C18 . H181 . 1.000 no O2 . P2 . 1.493(2) yes P2 . C19 . 1.773(3) yes P2 . C25 . 1.779(3) yes P2 . C31 . 1.791(3) yes C19 . C20 . 1.386(4) yes C19 . C24 . 1.398(4) yes C20 . C21 . 1.385(5) yes C20 . H201 . 1.000 no C21 . C22 . 1.358(6) yes C21 . H211 . 1.000 no C22 . C23 . 1.375(5) yes C22 . F4 . 1.356(4) yes C23 . C24 . 1.378(5) yes C23 . H231 . 1.000 no C24 . H241 . 1.000 no C25 . C26 . 1.391(4) yes C25 . C30 . 1.395(4) yes C26 . C27 . 1.397(5) yes C26 . H261 . 1.000 no C27 . C28 . 1.378(5) yes C27 . H271 . 1.000 no C28 . C29 . 1.357(5) yes C28 . F5 . 1.352(4) yes C29 . C30 . 1.383(5) yes C29 . H291 . 1.000 no C30 . H301 . 1.000 no C31 . C32 . 1.396(4) yes C31 . C36 . 1.396(4) yes C32 . C33 . 1.387(4) yes C32 . H321 . 1.000 no C33 . C34 . 1.376(4) yes C33 . H331 . 1.000 no C34 . C35 . 1.364(5) yes C34 . F6 . 1.357(3) yes C35 . C36 . 1.384(4) yes C35 . H351 . 1.000 no C36 . H361 . 1.000 no O3 . B1 . 1.484(4) yes O3 . H1 . 0.82(8) no B1 . C37 . 1.687(4) yes B1 . C43 . 1.642(4) yes B1 . C49 . 1.674(4) yes C37 . C38 . 1.406(4) yes C37 . C42 . 1.385(4) yes C38 . C39 . 1.383(5) yes C38 . F7 . 1.328(4) yes C39 . C40 . 1.371(5) yes C39 . F8 . 1.343(4) yes C40 . C41 . 1.374(5) yes C40 . F9 . 1.348(4) yes C41 . C42 . 1.387(5) yes C41 . F10 . 1.342(4) yes C42 . F11 . 1.342(4) yes C43 . C44 . 1.387(4) yes C43 . C48 . 1.395(4) yes C44 . C45 . 1.380(5) yes C44 . F12 . 1.346(4) yes C45 . C46 . 1.380(5) yes C45 . F13 . 1.331(4) yes C46 . C47 . 1.369(5) yes C46 . F14 . 1.345(4) yes C47 . C48 . 1.383(5) yes C47 . F15 . 1.352(4) yes C48 . F16 . 1.358(4) yes C49 . C50 . 1.383(5) yes C49 . C54 . 1.391(4) yes C50 . C51 . 1.381(5) yes C50 . F17 . 1.354(4) yes C51 . C52 . 1.372(6) yes C51 . F18 . 1.320(4) yes C52 . C53 . 1.359(6) yes C52 . F19 . 1.350(4) yes C53 . C54 . 1.396(5) yes C53 . F20 . 1.349(4) yes C54 . F21 . 1.347(4) yes O4 . B2 . 1.532(3) yes O4 . H2 . 0.72(8) no B2 . C55 . 1.651(4) yes B2 . C61 . 1.648(4) yes B2 . C67 . 1.663(4) yes C55 . C56 . 1.398(4) yes C55 . C60 . 1.386(4) yes C56 . C57 . 1.378(4) yes C56 . F22 . 1.350(3) yes C57 . C58 . 1.373(5) yes C57 . F23 . 1.343(4) yes C58 . C59 . 1.377(5) yes C58 . F24 . 1.346(4) yes C59 . C60 . 1.382(5) yes C59 . F25 . 1.343(4) yes C60 . F26 . 1.354(4) yes C61 . C62 . 1.385(4) yes C61 . C66 . 1.389(4) yes C62 . C63 . 1.374(4) yes C62 . F27 . 1.361(3) yes C63 . C64 . 1.373(5) yes C63 . F28 . 1.341(4) yes C64 . C65 . 1.369(5) yes C64 . F29 . 1.346(3) yes C65 . C66 . 1.385(4) yes C65 . F30 . 1.349(4) yes C66 . F31 . 1.355(3) yes C67 . C68 . 1.380(4) yes C67 . C72 . 1.393(4) yes C68 . C69 . 1.381(4) yes C68 . F32 . 1.360(3) yes C69 . C70 . 1.381(5) yes C69 . F33 . 1.339(4) yes C70 . C71 . 1.369(5) yes C70 . F34 . 1.342(3) yes C71 . C72 . 1.382(4) yes C71 . F35 . 1.349(4) yes C72 . F36 . 1.354(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Co1 . O2 . 100.94(10) yes O1 . Co1 . O3 . 118.70(10) yes O2 . Co1 . O3 . 118.43(10) yes O1 . Co1 . O4 . 118.03(9) yes O2 . Co1 . O4 . 96.51(9) yes O3 . Co1 . O4 . 102.79(9) yes Co1 . O1 . P1 . 169.42(16) yes O1 . P1 . C1 . 110.63(14) yes O1 . P1 . C7 . 109.87(13) yes C1 . P1 . C7 . 107.71(14) yes O1 . P1 . C13 . 111.08(14) yes C1 . P1 . C13 . 109.42(14) yes C7 . P1 . C13 . 108.03(13) yes P1 . C1 . C2 . 118.9(2) yes P1 . C1 . C6 . 121.4(2) yes C2 . C1 . C6 . 119.8(3) yes C1 . C2 . C3 . 120.0(3) yes C1 . C2 . H21 . 120.015 no C3 . C2 . H21 . 120.015 no C2 . C3 . C4 . 117.9(4) yes C2 . C3 . H31 . 121.068 no C4 . C3 . H31 . 121.068 no C3 . C4 . C5 . 123.2(3) yes C3 . C4 . F1 . 117.8(4) yes C5 . C4 . F1 . 118.9(4) yes C4 . C5 . C6 . 118.7(4) yes C4 . C5 . H51 . 120.663 no C6 . C5 . H51 . 120.663 no C1 . C6 . C5 . 120.5(3) yes C1 . C6 . H61 . 119.757 no C5 . C6 . H61 . 119.757 no P1 . C7 . C8 . 118.0(2) yes P1 . C7 . C12 . 122.7(2) yes C8 . C7 . C12 . 119.2(3) yes C7 . C8 . C9 . 121.1(3) yes C7 . C8 . H81 . 119.456 no C9 . C8 . H81 . 119.457 no C8 . C9 . C10 . 117.5(3) yes C8 . C9 . H91 . 121.225 no C10 . C9 . H91 . 121.225 no C9 . C10 . C11 . 123.5(3) yes C9 . C10 . F2 . 117.9(3) yes C11 . C10 . F2 . 118.4(4) yes C10 . C11 . C12 . 118.1(3) yes C10 . C11 . H111 . 120.949 no C12 . C11 . H111 . 120.950 no C7 . C12 . C11 . 120.5(3) yes C7 . C12 . H121 . 119.763 no C11 . C12 . H121 . 119.763 no P1 . C13 . C14 . 117.9(2) yes P1 . C13 . C18 . 122.0(2) yes C14 . C13 . C18 . 120.0(3) yes C13 . C14 . C15 . 120.3(3) yes C13 . C14 . H141 . 119.858 no C15 . C14 . H141 . 119.858 no C14 . C15 . C16 . 118.0(3) yes C14 . C15 . H151 . 121.005 no C16 . C15 . H151 . 121.005 no C15 . C16 . C17 . 123.7(3) yes C15 . C16 . F3 . 118.0(4) yes C17 . C16 . F3 . 118.3(3) yes C16 . C17 . C18 . 118.1(3) yes C16 . C17 . H171 . 120.953 no C18 . C17 . H171 . 120.953 no C13 . C18 . C17 . 119.9(3) yes C13 . C18 . H181 . 120.068 no C17 . C18 . H181 . 120.068 no Co1 . O2 . P2 . 162.53(15) yes O2 . P2 . C19 . 110.76(14) yes O2 . P2 . C25 . 108.41(13) yes C19 . P2 . C25 . 111.51(13) yes O2 . P2 . C31 . 110.46(13) yes C19 . P2 . C31 . 105.78(13) yes C25 . P2 . C31 . 109.91(13) yes P2 . C19 . C20 . 117.9(2) yes P2 . C19 . C24 . 123.1(2) yes C20 . C19 . C24 . 118.7(3) yes C19 . C20 . C21 . 121.1(3) yes C19 . C20 . H201 . 119.440 no C21 . C20 . H201 . 119.440 no C20 . C21 . C22 . 118.2(3) yes C20 . C21 . H211 . 120.881 no C22 . C21 . H211 . 120.881 no C21 . C22 . C23 . 123.0(3) yes C21 . C22 . F4 . 118.6(3) yes C23 . C22 . F4 . 118.4(3) yes C22 . C23 . C24 . 118.4(3) yes C22 . C23 . H231 . 120.796 no C24 . C23 . H231 . 120.796 no C19 . C24 . C23 . 120.6(3) yes C19 . C24 . H241 . 119.720 no C23 . C24 . H241 . 119.720 no P2 . C25 . C26 . 117.6(2) yes P2 . C25 . C30 . 123.2(2) yes C26 . C25 . C30 . 119.1(3) yes C25 . C26 . C27 . 120.5(3) yes C25 . C26 . H261 . 119.747 no C27 . C26 . H261 . 119.747 no C26 . C27 . C28 . 117.7(3) yes C26 . C27 . H271 . 121.137 no C28 . C27 . H271 . 121.137 no C27 . C28 . C29 . 123.4(3) yes C27 . C28 . F5 . 118.4(3) yes C29 . C28 . F5 . 118.2(3) yes C28 . C29 . C30 . 118.6(3) yes C28 . C29 . H291 . 120.693 no C30 . C29 . H291 . 120.693 no C25 . C30 . C29 . 120.7(3) yes C25 . C30 . H301 . 119.657 no C29 . C30 . H301 . 119.657 no P2 . C31 . C32 . 118.7(2) yes P2 . C31 . C36 . 122.0(2) yes C32 . C31 . C36 . 119.0(3) yes C31 . C32 . C33 . 120.8(3) yes C31 . C32 . H321 . 119.598 no C33 . C32 . H321 . 119.598 no C32 . C33 . C34 . 117.9(3) yes C32 . C33 . H331 . 121.047 no C34 . C33 . H331 . 121.047 no C33 . C34 . C35 . 123.2(3) yes C33 . C34 . F6 . 117.9(3) yes C35 . C34 . F6 . 118.9(3) yes C34 . C35 . C36 . 118.7(3) yes C34 . C35 . H351 . 120.673 no C36 . C35 . H351 . 120.673 no C31 . C36 . C35 . 120.4(3) yes C31 . C36 . H361 . 119.788 no C35 . C36 . H361 . 119.788 no Co1 . O3 . B1 . 141.25(18) yes Co1 . O3 . H1 . 103(6) no B1 . O3 . H1 . 116(6) no O3 . B1 . C37 . 103.5(2) yes O3 . B1 . C43 . 112.3(2) yes C37 . B1 . C43 . 113.0(2) yes O3 . B1 . C49 . 109.0(2) yes C37 . B1 . C49 . 110.3(2) yes C43 . B1 . C49 . 108.6(2) yes B1 . C37 . C38 . 118.5(3) yes B1 . C37 . C42 . 126.6(3) yes C38 . C37 . C42 . 114.5(3) yes C37 . C38 . C39 . 123.1(3) yes C37 . C38 . F7 . 120.3(3) yes C39 . C38 . F7 . 116.6(3) yes C38 . C39 . C40 . 119.6(3) yes C38 . C39 . F8 . 120.2(3) yes C40 . C39 . F8 . 120.2(3) yes C39 . C40 . C41 . 119.8(3) yes C39 . C40 . F9 . 120.4(3) yes C41 . C40 . F9 . 119.7(3) yes C40 . C41 . C42 . 119.4(3) yes C40 . C41 . F10 . 119.8(3) yes C42 . C41 . F10 . 120.8(3) yes C37 . C42 . C41 . 123.5(3) yes C37 . C42 . F11 . 121.3(3) yes C41 . C42 . F11 . 115.2(3) yes B1 . C43 . C44 . 122.1(3) yes B1 . C43 . C48 . 124.4(3) yes C44 . C43 . C48 . 113.5(3) yes C43 . C44 . C45 . 124.1(3) yes C43 . C44 . F12 . 120.3(3) yes C45 . C44 . F12 . 115.6(3) yes C44 . C45 . C46 . 119.7(3) yes C44 . C45 . F13 . 120.5(3) yes C46 . C45 . F13 . 119.8(3) yes C45 . C46 . C47 . 118.9(3) yes C45 . C46 . F14 . 120.2(3) yes C47 . C46 . F14 . 120.9(3) yes C46 . C47 . C48 . 119.7(3) yes C46 . C47 . F15 . 120.5(3) yes C48 . C47 . F15 . 119.8(3) yes C43 . C48 . C47 . 124.1(3) yes C43 . C48 . F16 . 120.1(3) yes C47 . C48 . F16 . 115.8(3) yes B1 . C49 . C50 . 117.2(3) yes B1 . C49 . C54 . 128.9(3) yes C50 . C49 . C54 . 113.8(3) yes C49 . C50 . C51 . 125.1(3) yes C49 . C50 . F17 . 118.3(3) yes C51 . C50 . F17 . 116.6(3) yes C50 . C51 . C52 . 118.1(3) yes C50 . C51 . F18 . 121.3(3) yes C52 . C51 . F18 . 120.5(3) yes C51 . C52 . C53 . 120.4(3) yes C51 . C52 . F19 . 119.8(4) yes C53 . C52 . F19 . 119.8(4) yes C52 . C53 . C54 . 119.6(3) yes C52 . C53 . F20 . 120.7(3) yes C54 . C53 . F20 . 119.7(4) yes C49 . C54 . C53 . 123.0(3) yes C49 . C54 . F21 . 122.0(3) yes C53 . C54 . F21 . 115.0(3) yes Co1 . O4 . B2 . 140.72(17) yes Co1 . O4 . H2 . 100(7) no B2 . O4 . H2 . 118(7) no O4 . B2 . C55 . 106.4(2) yes O4 . B2 . C61 . 107.9(2) yes C55 . B2 . C61 . 113.7(2) yes O4 . B2 . C67 . 108.2(2) yes C55 . B2 . C67 . 110.4(2) yes C61 . B2 . C67 . 110.1(2) yes B2 . C55 . C56 . 118.9(2) yes B2 . C55 . C60 . 127.7(3) yes C56 . C55 . C60 . 113.2(3) yes C55 . C56 . C57 . 124.9(3) yes C55 . C56 . F22 . 119.1(3) yes C57 . C56 . F22 . 115.9(3) yes C56 . C57 . C58 . 118.7(3) yes C56 . C57 . F23 . 121.0(3) yes C58 . C57 . F23 . 120.3(3) yes C57 . C58 . C59 . 119.6(3) yes C57 . C58 . F24 . 119.8(3) yes C59 . C58 . F24 . 120.6(3) yes C58 . C59 . C60 . 119.4(3) yes C58 . C59 . F25 . 119.9(3) yes C60 . C59 . F25 . 120.7(3) yes C55 . C60 . C59 . 124.1(3) yes C55 . C60 . F26 . 120.9(3) yes C59 . C60 . F26 . 114.9(3) yes B2 . C61 . C62 . 119.5(2) yes B2 . C61 . C66 . 126.9(3) yes C62 . C61 . C66 . 113.5(3) yes C61 . C62 . C63 . 125.0(3) yes C61 . C62 . F27 . 118.4(2) yes C63 . C62 . F27 . 116.6(3) yes C62 . C63 . C64 . 118.9(3) yes C62 . C63 . F28 . 121.2(3) yes C64 . C63 . F28 . 119.9(3) yes C63 . C64 . C65 . 119.3(3) yes C63 . C64 . F29 . 120.3(3) yes C65 . C64 . F29 . 120.4(3) yes C64 . C65 . C66 . 119.8(3) yes C64 . C65 . F30 . 120.2(3) yes C66 . C65 . F30 . 120.0(3) yes C61 . C66 . C65 . 123.5(3) yes C61 . C66 . F31 . 121.8(3) yes C65 . C66 . F31 . 114.8(3) yes B2 . C67 . C68 . 121.3(2) yes B2 . C67 . C72 . 125.2(3) yes C68 . C67 . C72 . 113.3(3) yes C67 . C68 . C69 . 124.9(3) yes C67 . C68 . F32 . 119.5(2) yes C69 . C68 . F32 . 115.6(3) yes C68 . C69 . C70 . 118.9(3) yes C68 . C69 . F33 . 121.4(3) yes C70 . C69 . F33 . 119.6(3) yes C69 . C70 . C71 . 119.1(3) yes C69 . C70 . F34 . 120.3(3) yes C71 . C70 . F34 . 120.6(3) yes C70 . C71 . C72 . 119.8(3) yes C70 . C71 . F35 . 119.9(3) yes C72 . C71 . F35 . 120.3(3) yes C67 . C72 . C71 . 124.0(3) yes C67 . C72 . F36 . 121.0(3) yes C71 . C72 . F36 . 115.0(3) yes #===END data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 287090' #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 12.5164(3) _cell_angle_alpha 90 _cell_length_b 17.0794(5) _cell_angle_beta 99.4628(11) _cell_length_c 18.0656(4) _cell_angle_gamma 90 _cell_volume 3809.4 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'Co ' 0.2990 0.9730 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C41 H18 B1 Co1 F15 O4 P1 ' _chemical_formula_moiety ' C41 H18 B1 Co1 F15 O4 P1 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 960.28 _cell_measurement_reflns_used 37239 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' pale yellow ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1914.620 _exptl_absorpt_coefficient_mu 0.610 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.96 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 37239 _reflns_number_total 8941 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_gt 5530 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _refine_diff_density_min -0.32 _refine_diff_density_max 0.69 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 5530 _refine_ls_number_parameters 568 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0480 _refine_ls_goodness_of_fit_ref 1.0261 _refine_ls_shift/su_max 0.000343 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 4.56 0.438E-01 4.12 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Co1 0.31559(2) 0.108884(19) 0.246507(18) 0.0217 1.0000 Uani C1 0.3371(2) 0.08677(16) 0.15336(15) 0.0300 1.0000 Uani C143 0.2495(2) -0.19161(16) 0.42963(14) 0.0301 1.0000 Uani O1 0.35243(18) 0.07165(13) 0.09515(11) 0.0419 1.0000 Uani C2 0.4120(2) 0.07294(16) 0.32401(16) 0.0299 1.0000 Uani O2 0.47109(18) 0.04933(14) 0.37357(13) 0.0462 1.0000 Uani C3 0.2025(2) 0.16173(16) 0.27330(16) 0.0320 1.0000 Uani O3 0.13115(18) 0.19211(13) 0.29339(15) 0.0493 1.0000 Uani P1 0.41123(5) 0.22035(4) 0.23930(3) 0.0209 1.0000 Uani C4 0.37494(19) 0.27509(14) 0.15207(13) 0.0228 1.0000 Uani C5 0.26727(19) 0.27708(15) 0.11708(14) 0.0256 1.0000 Uani C6 0.2366(2) 0.32441(17) 0.05435(15) 0.0316 1.0000 Uani C7 0.3128(2) 0.36900(16) 0.02614(14) 0.0307 1.0000 Uani C8 0.4205(2) 0.36669(16) 0.05961(14) 0.0292 1.0000 Uani C9 0.4525(2) 0.31994(15) 0.12304(14) 0.0260 1.0000 Uani C10 0.55494(19) 0.20115(14) 0.24558(14) 0.0244 1.0000 Uani C11 0.5934(2) 0.16381(16) 0.18607(15) 0.0297 1.0000 Uani C12 0.7036(2) 0.14666(16) 0.19106(17) 0.0334 1.0000 Uani C13 0.7754(2) 0.16711(17) 0.25475(18) 0.0361 1.0000 Uani C14 0.7381(2) 0.20350(17) 0.31390(16) 0.0346 1.0000 Uani C15 0.6286(2) 0.22043(16) 0.30990(15) 0.0296 1.0000 Uani C16 0.4036(2) 0.29267(15) 0.31247(13) 0.0248 1.0000 Uani C17 0.3836(3) 0.26959(18) 0.38286(17) 0.0405 1.0000 Uani C18 0.3818(4) 0.3244(2) 0.43921(17) 0.0531 1.0000 Uani C19 0.3996(3) 0.4026(2) 0.42562(18) 0.0482 1.0000 Uani C20 0.4195(3) 0.42639(17) 0.35637(17) 0.0368 1.0000 Uani C21 0.4211(2) 0.37133(16) 0.29961(14) 0.0279 1.0000 Uani C22 0.23417(19) 0.01287(15) 0.24678(14) 0.0256 1.0000 Uani C23 0.2655(2) -0.05980(16) 0.20926(17) 0.0318 1.0000 Uani O4 0.15073(13) 0.0121(1) 0.27817(9) 0.0238 1.0000 Uani B1 0.0650(2) -0.05347(17) 0.28179(15) 0.0231 1.0000 Uani C24 0.1161(2) -0.12550(14) 0.33580(14) 0.0249 1.0000 Uani C25 0.2175(2) -0.13114(15) 0.37924(14) 0.0269 1.0000 Uani C27 0.1774(2) -0.24939(16) 0.43913(15) 0.0322 1.0000 Uani C28 0.0748(2) -0.24729(15) 0.39751(15) 0.0308 1.0000 Uani C29 0.0466(2) -0.18622(15) 0.34816(14) 0.0275 1.0000 Uani C30 0.01477(19) -0.07381(15) 0.19446(14) 0.0240 1.0000 Uani C31 0.0140(2) -0.14565(15) 0.15925(14) 0.0264 1.0000 Uani C32 -0.0344(2) -0.15953(17) 0.08590(16) 0.0344 1.0000 Uani C33 -0.0847(2) -0.0994(2) 0.04429(16) 0.0408 1.0000 Uani C34 -0.0853(3) -0.02584(19) 0.07533(16) 0.0399 1.0000 Uani C35 -0.0359(2) -0.01429(16) 0.14829(15) 0.0319 1.0000 Uani C36 -0.02643(19) -0.01271(14) 0.32547(13) 0.0231 1.0000 Uani C37 -0.1375(2) -0.02361(15) 0.30771(13) 0.0250 1.0000 Uani C38 -0.21122(19) 0.00521(15) 0.34946(14) 0.0251 1.0000 Uani C39 -0.1756(2) 0.04791(15) 0.41323(14) 0.0267 1.0000 Uani C40 -0.0668(2) 0.06208(15) 0.43321(14) 0.0264 1.0000 Uani C41 0.00522(18) 0.03137(15) 0.39032(13) 0.0232 1.0000 Uani F1 0.29434(12) -0.07542(9) 0.37578(9) 0.0340 1.0000 Uani F2 0.34941(13) -0.19283(11) 0.47006(9) 0.0390 1.0000 Uani F3 0.20637(17) -0.30720(11) 0.48869(11) 0.0480 1.0000 Uani F4 0.00207(15) -0.3035(1) 0.40525(11) 0.0449 1.0000 Uani F5 -0.05575(12) -0.18612(9) 0.31071(9) 0.0337 1.0000 Uani F6 0.06355(13) -0.20785(9) 0.19640(9) 0.0330 1.0000 Uani F7 -0.03145(17) -0.23178(11) 0.0568(1) 0.0497 1.0000 Uani F8 -0.13400(18) -0.11149(14) -0.02691(11) 0.0641 1.0000 Uani F9 -0.13533(19) 0.03356(13) 0.0346(1) 0.0590 1.0000 Uani F10 -0.04142(15) 0.0585(1) 0.17634(9) 0.0400 1.0000 Uani F11 -0.18071(12) -0.0646(1) 0.24574(9) 0.0358 1.0000 Uani F12 -0.31781(12) -0.0063(1) 0.32749(9) 0.0364 1.0000 Uani F13 -0.24703(13) 0.07668(11) 0.45354(9) 0.0377 1.0000 Uani F14 -0.03063(13) 0.1051(1) 0.49503(8) 0.0349 1.0000 Uani F15 0.11163(12) 0.0431(1) 0.41651(8) 0.0312 1.0000 Uani H51 0.2119 0.2445 0.1370 0.0311 1.0000 Uiso H61 0.1590 0.3261 0.0296 0.0374 1.0000 Uiso H71 0.2900 0.4031 -0.0187 0.0368 1.0000 Uiso H81 0.4754 0.3984 0.0385 0.0358 1.0000 Uiso H91 0.5301 0.3185 0.1475 0.0317 1.0000 Uiso H111 0.5417 0.1493 0.1398 0.0363 1.0000 Uiso H121 0.7304 0.1196 0.1486 0.0417 1.0000 Uiso H131 0.8543 0.1555 0.2580 0.0436 1.0000 Uiso H141 0.7903 0.2178 0.3600 0.0409 1.0000 Uiso H151 0.6025 0.2465 0.3532 0.0357 1.0000 Uiso H171 0.3704 0.2131 0.3928 0.0503 1.0000 Uiso H181 0.3678 0.3074 0.4897 0.0664 1.0000 Uiso H191 0.3980 0.4421 0.4663 0.0595 1.0000 Uiso H201 0.4327 0.4829 0.3468 0.0448 1.0000 Uiso H211 0.4350 0.3887 0.2492 0.0338 1.0000 Uiso H231 0.2337 -0.0583 0.1547 0.0397 1.0000 Uiso H232 0.3462 -0.0629 0.2149 0.0397 1.0000 Uiso H233 0.2374 -0.1067 0.2330 0.0397 1.0000 Uiso 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 0.02007(16) 0.02013(17) 0.02667(17) 0.00302(13) 0.00921(12) -0.00108(13) C1 0.0312(13) 0.0269(13) 0.0324(13) 0.004(1) 0.007(1) -0.0042(11) C143 0.0333(13) 0.0302(13) 0.0285(12) 0.000(1) 0.011(1) 0.0056(11) O1 0.0544(13) 0.0456(13) 0.029(1) -0.0021(9) 0.0167(9) -0.006(1) C2 0.0267(12) 0.0261(13) 0.0385(14) 0.0015(11) 0.0099(11) -0.0051(11) O2 0.0384(11) 0.0471(13) 0.0497(13) 0.016(1) -0.003(1) 0.001(1) C3 0.0314(13) 0.0255(13) 0.0411(14) 0.0077(11) 0.0117(11) -0.0017(11) O3 0.0419(12) 0.0379(12) 0.0755(16) 0.0132(11) 0.0310(12) 0.014(1) P1 0.0205(3) 0.0202(3) 0.0232(3) 0.0027(2) 0.0073(2) -0.0007(2) C4 0.0252(11) 0.0203(11) 0.0244(11) 0.0009(9) 0.0088(9) 0.0019(9) C5 0.0232(11) 0.0252(12) 0.0294(12) -0.001(1) 0.007(1) 0.001(1) C6 0.0282(12) 0.0314(14) 0.0340(13) 0.0019(11) 0.002(1) 0.0074(11) C7 0.0417(15) 0.0267(13) 0.0236(12) 0.003(1) 0.005(1) 0.0087(11) C8 0.0327(13) 0.0273(12) 0.0295(13) 0.006(1) 0.011(1) 0.0016(11) C9 0.0270(12) 0.0257(12) 0.0266(11) 0.002(1) 0.0082(9) -0.001(1) C10 0.0218(11) 0.0214(12) 0.0311(12) 0.008(1) 0.0074(9) -0.0012(9) C11 0.0252(12) 0.0301(13) 0.0355(13) -0.0009(11) 0.009(1) -0.001(1) C12 0.0290(13) 0.0258(13) 0.0493(16) 0.0030(12) 0.0179(12) 0.0024(11) C13 0.0215(12) 0.0288(14) 0.0587(18) 0.0091(13) 0.0091(12) 0.0025(11) C14 0.0272(13) 0.0322(15) 0.0430(15) 0.0068(12) 0.0012(11) -0.0019(11) C15 0.0272(12) 0.0256(12) 0.0365(14) 0.003(1) 0.007(1) 0.000(1) C16 0.0239(11) 0.0240(12) 0.0272(12) 0.002(1) 0.0067(9) 0.0007(9) C17 0.0602(19) 0.0324(15) 0.0332(14) -0.0019(12) 0.0202(13) -0.0085(14) C18 0.092(3) 0.0432(18) 0.0304(15) -0.0058(13) 0.0296(16) -0.0115(18) C19 0.073(2) 0.0371(17) 0.0385(16) -0.0090(13) 0.0214(16) -0.0037(16) C20 0.0475(16) 0.0260(14) 0.0384(15) -0.0013(11) 0.0120(12) -0.0030(12) C21 0.0283(12) 0.0279(13) 0.0283(12) 0.002(1) 0.007(1) 0.001(1) C22 0.0218(11) 0.0281(13) 0.0277(12) 0.003(1) 0.0062(9) -0.000(1) C23 0.0293(12) 0.0241(13) 0.0459(15) -0.0036(11) 0.0177(11) -0.002(1) O4 0.0226(8) 0.0211(8) 0.0295(8) -0.0007(7) 0.0096(7) -0.0041(7) B1 0.0199(12) 0.0256(13) 0.0254(12) -0.0036(11) 0.008(1) -0.0041(11) C24 0.0262(11) 0.0236(12) 0.0275(12) -0.0035(9) 0.0119(9) -0.0005(9) C25 0.0286(12) 0.0240(12) 0.0314(12) -0.003(1) 0.014(1) -0.005(1) C27 0.0427(15) 0.0249(13) 0.0324(13) 0.0025(11) 0.0164(12) 0.0050(11) C28 0.0403(14) 0.0216(12) 0.0355(13) -0.005(1) 0.0213(11) -0.0072(11) C29 0.0257(12) 0.0285(13) 0.0301(12) -0.008(1) 0.010(1) -0.005(1) C30 0.0204(11) 0.0266(13) 0.0265(11) -0.004(1) 0.0083(9) -0.0015(9) C31 0.0228(11) 0.0275(13) 0.0307(12) -0.004(1) 0.010(1) 0.002(1) C32 0.0351(14) 0.0342(15) 0.0340(14) -0.0171(12) 0.0058(11) 0.0016(12) C33 0.0390(15) 0.0542(19) 0.0268(13) -0.0123(13) -0.0017(11) 0.0148(14) C34 0.0455(16) 0.0427(17) 0.0318(13) 0.0022(12) 0.0070(12) 0.0199(14) C35 0.0366(14) 0.0302(14) 0.0309(13) -0.0042(11) 0.0113(11) 0.0033(11) C36 0.0236(11) 0.0242(12) 0.0229(11) -0.0026(9) 0.0080(9) -0.0026(9) C37 0.0229(11) 0.0258(12) 0.0263(11) -0.0049(9) 0.0042(9) -0.0040(9) C38 0.0179(11) 0.0269(12) 0.0314(12) -0.001(1) 0.0067(9) -0.0038(9) C39 0.0292(12) 0.0255(13) 0.0280(12) -0.001(1) 0.013(1) 0.004(1) C40 0.0325(13) 0.0244(12) 0.0221(11) -0.0031(9) 0.0040(9) -0.002(1) C41 0.0203(11) 0.0245(12) 0.0252(11) 0.0014(9) 0.0050(9) -0.0006(9) F1 0.0233(7) 0.0347(9) 0.0427(9) 0.0071(7) 0.0018(6) -0.0097(6) F2 0.0323(8) 0.044(1) 0.0393(9) 0.0079(7) 0.0028(7) 0.0072(7) F3 0.0613(12) 0.0351(9) 0.049(1) 0.0155(8) 0.0131(9) 0.0066(8) F4 0.051(1) 0.0284(9) 0.0599(11) 0.0012(8) 0.0234(9) -0.0149(8) F5 0.0265(7) 0.0324(8) 0.0440(9) -0.0049(7) 0.0116(6) -0.0100(6) F6 0.0375(8) 0.0285(8) 0.0335(8) -0.0060(6) 0.0071(6) 0.0063(7) F7 0.0585(11) 0.0441(11) 0.043(1) -0.0229(8) -0.0010(8) 0.0087(9) F8 0.0680(13) 0.0818(16) 0.035(1) -0.021(1) -0.0145(9) 0.0335(12) F9 0.0776(14) 0.0575(13) 0.039(1) 0.0052(9) -0.0002(9) 0.0353(11) F10 0.0587(11) 0.0277(8) 0.0350(8) 0.0001(7) 0.0120(8) 0.0073(8) F11 0.0249(7) 0.047(1) 0.0368(8) -0.0180(7) 0.0079(6) -0.0084(7) F12 0.0192(7) 0.047(1) 0.0445(9) -0.0085(8) 0.0092(6) -0.0027(7) F13 0.0314(8) 0.048(1) 0.0377(8) -0.0099(7) 0.0168(7) 0.0063(7) F14 0.0401(8) 0.0379(9) 0.0278(7) -0.0117(7) 0.0085(6) -0.0030(7) F15 0.0220(7) 0.0389(9) 0.0324(8) -0.0091(7) 0.0037(6) -0.0065(6) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . C1 . 1.788(3) yes Co1 . C2 . 1.799(3) yes Co1 . C3 . 1.811(3) yes Co1 . P1 . 2.2640(7) yes Co1 . C22 . 1.931(3) yes C1 . O1 . 1.129(3) yes C143 . C25 . 1.391(4) yes C143 . C27 . 1.367(4) yes C143 . F2 . 1.341(3) yes C2 . O2 . 1.137(3) yes C3 . O3 . 1.142(3) yes P1 . C4 . 1.824(2) yes P1 . C10 . 1.814(2) yes P1 . C16 . 1.823(3) yes C4 . C5 . 1.392(3) yes C4 . C9 . 1.404(3) yes C5 . C6 . 1.394(4) yes C5 . H51 . 1.000 no C6 . C7 . 1.382(4) yes C6 . H61 . 1.000 no C7 . C8 . 1.384(4) yes C7 . H71 . 1.000 no C8 . C9 . 1.400(4) yes C8 . H81 . 1.000 no C9 . H91 . 1.000 no C10 . C11 . 1.401(4) yes C10 . C15 . 1.399(4) yes C11 . C12 . 1.398(4) yes C11 . H111 . 1.000 no C12 . C13 . 1.383(4) yes C12 . H121 . 1.000 no C13 . C14 . 1.382(4) yes C13 . H131 . 1.000 no C14 . C15 . 1.391(4) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C16 . C17 . 1.393(4) yes C16 . C21 . 1.387(4) yes C17 . C18 . 1.386(4) yes C17 . H171 . 1.000 no C18 . C19 . 1.382(5) yes C18 . H181 . 1.000 no C19 . C20 . 1.376(4) yes C19 . H191 . 1.000 no C20 . C21 . 1.394(4) yes C20 . H201 . 1.000 no C21 . H211 . 1.000 no C22 . C23 . 1.497(4) yes C22 . O4 . 1.268(3) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no O4 . B1 . 1.561(3) yes B1 . C24 . 1.634(4) yes B1 . C30 . 1.637(4) yes B1 . C36 . 1.647(3) yes C24 . C25 . 1.382(4) yes C24 . C29 . 1.394(4) yes C25 . F1 . 1.361(3) yes C27 . C28 . 1.378(4) yes C27 . F3 . 1.342(3) yes C28 . C29 . 1.380(4) yes C28 . F4 . 1.346(3) yes C29 . F5 . 1.347(3) yes C30 . C31 . 1.381(4) yes C30 . C35 . 1.399(4) yes C31 . C32 . 1.384(4) yes C31 . F6 . 1.352(3) yes C32 . C33 . 1.364(4) yes C32 . F7 . 1.344(3) yes C33 . C34 . 1.377(4) yes C33 . F8 . 1.348(3) yes C34 . C35 . 1.375(4) yes C34 . F9 . 1.346(3) yes C35 . F10 . 1.348(3) yes C36 . C37 . 1.387(3) yes C36 . C41 . 1.394(3) yes C37 . C38 . 1.375(3) yes C37 . F11 . 1.355(3) yes C38 . C39 . 1.374(4) yes C38 . F12 . 1.342(3) yes C39 . C40 . 1.372(4) yes C39 . F13 . 1.336(3) yes C40 . C41 . 1.385(3) yes C40 . F14 . 1.352(3) yes C41 . F15 . 1.353(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . Co1 . C2 . 118.34(12) yes C1 . Co1 . C3 . 127.04(13) yes C2 . Co1 . C3 . 114.57(13) yes C1 . Co1 . P1 . 87.74(9) yes C2 . Co1 . P1 . 92.20(8) yes C3 . Co1 . P1 . 92.31(9) yes C1 . Co1 . C22 . 89.10(11) yes C2 . Co1 . C22 . 89.71(11) yes C3 . Co1 . C22 . 89.22(11) yes P1 . Co1 . C22 . 176.81(8) yes Co1 . C1 . O1 . 178.5(3) yes C25 . C143 . C27 . 119.6(3) yes C25 . C143 . F2 . 120.7(2) yes C27 . C143 . F2 . 119.8(2) yes Co1 . C2 . O2 . 178.4(2) yes Co1 . C3 . O3 . 176.2(2) yes Co1 . P1 . C4 . 114.95(8) yes Co1 . P1 . C10 . 111.88(8) yes C4 . P1 . C10 . 104.49(11) yes Co1 . P1 . C16 . 115.90(8) yes C4 . P1 . C16 . 104.12(11) yes C10 . P1 . C16 . 104.28(12) yes P1 . C4 . C5 . 119.32(18) yes P1 . C4 . C9 . 120.87(19) yes C5 . C4 . C9 . 119.6(2) yes C4 . C5 . C6 . 120.0(2) yes C4 . C5 . H51 . 120.0 no C6 . C5 . H51 . 120.0 no C5 . C6 . C7 . 120.3(2) yes C5 . C6 . H61 . 119.8 no C7 . C6 . H61 . 119.8 no C6 . C7 . C8 . 120.3(2) yes C6 . C7 . H71 . 119.8 no C8 . C7 . H71 . 119.8 no C7 . C8 . C9 . 120.0(2) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 120.0 no C4 . C9 . C8 . 119.6(2) yes C4 . C9 . H91 . 120.2 no C8 . C9 . H91 . 120.2 no P1 . C10 . C11 . 119.7(2) yes P1 . C10 . C15 . 121.41(19) yes C11 . C10 . C15 . 118.8(2) yes C10 . C11 . C12 . 120.3(2) yes C10 . C11 . H111 . 119.8 no C12 . C11 . H111 . 119.8 no C11 . C12 . C13 . 120.0(3) yes C11 . C12 . H121 . 120.0 no C13 . C12 . H121 . 120.0 no C12 . C13 . C14 . 120.1(2) yes C12 . C13 . H131 . 120.0 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 120.5(3) yes C13 . C14 . H141 . 119.7 no C15 . C14 . H141 . 119.7 no C10 . C15 . C14 . 120.2(2) yes C10 . C15 . H151 . 119.9 no C14 . C15 . H151 . 119.9 no P1 . C16 . C17 . 120.6(2) yes P1 . C16 . C21 . 120.41(19) yes C17 . C16 . C21 . 119.0(2) yes C16 . C17 . C18 . 120.4(3) yes C16 . C17 . H171 . 119.8 no C18 . C17 . H171 . 119.8 no C17 . C18 . C19 . 120.0(3) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 120.3(3) yes C18 . C19 . H191 . 119.8 no C20 . C19 . H191 . 119.8 no C19 . C20 . C21 . 119.8(3) yes C19 . C20 . H201 . 120.1 no C21 . C20 . H201 . 120.1 no C16 . C21 . C20 . 120.6(2) yes C16 . C21 . H211 . 119.7 no C20 . C21 . H211 . 119.7 no Co1 . C22 . C23 . 121.69(17) yes Co1 . C22 . O4 . 118.91(19) yes C23 . C22 . O4 . 119.4(2) yes C22 . C23 . H231 . 109.5 no C22 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . O4 . B1 . 130.5(2) yes O4 . B1 . C24 . 111.17(19) yes O4 . B1 . C30 . 105.65(19) yes C24 . B1 . C30 . 117.8(2) yes O4 . B1 . C36 . 104.67(19) yes C24 . B1 . C36 . 105.46(19) yes C30 . B1 . C36 . 111.4(2) yes B1 . C24 . C25 . 128.6(2) yes B1 . C24 . C29 . 117.5(2) yes C25 . C24 . C29 . 113.3(2) yes C143 . C25 . C24 . 124.2(2) yes C143 . C25 . F1 . 114.8(2) yes C24 . C25 . F1 . 121.0(2) yes C143 . C27 . C28 . 119.2(3) yes C143 . C27 . F3 . 120.2(3) yes C28 . C27 . F3 . 120.6(3) yes C27 . C28 . C29 . 119.2(2) yes C27 . C28 . F4 . 120.7(3) yes C29 . C28 . F4 . 120.1(3) yes C24 . C29 . C28 . 124.5(2) yes C24 . C29 . F5 . 119.0(2) yes C28 . C29 . F5 . 116.5(2) yes B1 . C30 . C31 . 127.2(2) yes B1 . C30 . C35 . 119.0(2) yes C31 . C30 . C35 . 113.7(2) yes C30 . C31 . C32 . 124.2(3) yes C30 . C31 . F6 . 120.1(2) yes C32 . C31 . F6 . 115.7(2) yes C31 . C32 . C33 . 119.2(3) yes C31 . C32 . F7 . 119.7(3) yes C33 . C32 . F7 . 121.0(2) yes C32 . C33 . C34 . 119.7(3) yes C32 . C33 . F8 . 120.5(3) yes C34 . C33 . F8 . 119.8(3) yes C33 . C34 . C35 . 119.3(3) yes C33 . C34 . F9 . 119.9(3) yes C35 . C34 . F9 . 120.7(3) yes C30 . C35 . C34 . 123.8(3) yes C30 . C35 . F10 . 119.5(2) yes C34 . C35 . F10 . 116.7(2) yes B1 . C36 . C37 . 125.5(2) yes B1 . C36 . C41 . 120.5(2) yes C37 . C36 . C41 . 113.7(2) yes C36 . C37 . C38 . 124.2(2) yes C36 . C37 . F11 . 120.6(2) yes C38 . C37 . F11 . 115.2(2) yes C37 . C38 . C39 . 119.7(2) yes C37 . C38 . F12 . 120.6(2) yes C39 . C38 . F12 . 119.7(2) yes C38 . C39 . C40 . 119.0(2) yes C38 . C39 . F13 . 119.9(2) yes C40 . C39 . F13 . 121.1(2) yes C39 . C40 . C41 . 119.7(2) yes C39 . C40 . F14 . 119.8(2) yes C41 . C40 . F14 . 120.5(2) yes C36 . C41 . C40 . 123.6(2) yes C36 . C41 . F15 . 120.1(2) yes C40 . C41 . F15 . 116.3(2) yes