# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M Bruce' _publ_contact_author_email MICHAEL.BRUCE@ADELAIDE.EDU.AU _publ_section_title ; Conversion of C C to CO in alkynyl-metal complexes: oxidation of carbon chains capped by carbon-tricobalt clusters ; loop_ _publ_author_name 'M Bruce' 'Paul A. Humphrey' 'B Nicholson' 'Brian W Skelton' 'Allan H White' ; N.N.Zaitseva ; # Attachment '10.br1078.cif' data_br1078 _database_code_depnum_ccdc_archive 'CCDC 754937' #TrackingRef '10.br1078.cif' _audit_creation_date 2009-04-28T15:14:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C46 H25 Co3 O17 P2 Ru3' _chemical_formula_sum 'C46 H25 Co3 O17 P2 Ru3' _chemical_formula_weight 1391.6 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _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 42.394(4) _cell_length_b 11.2403(10) _cell_length_c 21.920(2) _cell_angle_alpha 90 _cell_angle_beta 109.043(2) _cell_angle_gamma 90 _cell_volume 9873.7(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7607 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 34.25 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5440 _exptl_special_details ; Bruker SMART CCD diffractometer ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.87 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_unetI/netI 0.0443 _diffrn_reflns_number 81132 _diffrn_reflns_limit_h_min -68 _diffrn_reflns_limit_h_max 64 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 35.14 _diffrn_reflns_theta_full 35.14 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 21780 _reflns_number_gt 15239 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0380P)^2^+34.4174P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 21780 _refine_ls_number_parameters 677 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.221 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.142 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ru1 Ru 0.242601(6) 1.08232(2) 0.368210(11) 0.02504(5) Uani 1 1 d . . . Ru2 Ru 0.190480(6) 1.241394(19) 0.301964(11) 0.02274(5) Uani 1 1 d . . . Ru3 Ru 0.202840(6) 1.03357(2) 0.238556(11) 0.02561(5) Uani 1 1 d . . . Co4 Co 0.128118(10) 0.67288(3) 0.425080(18) 0.02340(7) Uani 1 1 d . A . Co5 Co 0.092082(10) 0.79663(4) 0.469804(18) 0.02591(8) Uani 1 1 d . A . Co6 Co 0.152525(10) 0.83643(4) 0.501130(18) 0.02686(8) Uani 1 1 d . . . C11 C 0.28863(9) 1.1431(3) 0.38606(18) 0.0383(7) Uani 1 1 d . . . O11 O 0.31403(7) 1.1828(3) 0.39518(16) 0.0574(8) Uani 1 1 d . . . C12 C 0.25476(9) 0.9198(3) 0.38770(17) 0.0364(7) Uani 1 1 d . . . O12 O 0.26210(8) 0.8236(3) 0.39721(15) 0.0534(7) Uani 1 1 d . . . C13 C 0.23900(8) 1.1067(3) 0.45203(15) 0.0316(6) Uani 1 1 d . . . O13 O 0.23625(8) 1.1191(3) 0.50126(12) 0.0455(6) Uani 1 1 d . . . C21 C 0.19847(8) 1.3979(3) 0.26973(16) 0.0310(6) Uani 1 1 d . . . O21 O 0.20220(7) 1.4859(2) 0.24815(14) 0.0459(6) Uani 1 1 d . . . C22 C 0.14350(8) 1.2377(3) 0.25640(15) 0.0314(6) Uani 1 1 d . . . O22 O 0.11578(6) 1.2303(3) 0.23036(14) 0.0470(6) Uani 1 1 d . . . C23 C 0.18445(8) 1.2985(3) 0.37908(16) 0.0317(6) Uani 1 1 d . . . O23 O 0.18171(7) 1.3300(3) 0.42628(13) 0.0493(7) Uani 1 1 d . . . C31 C 0.22308(9) 1.0452(3) 0.16911(15) 0.0335(6) Uani 1 1 d . . . O31 O 0.23476(7) 1.0491(3) 0.12987(12) 0.0484(7) Uani 1 1 d . . . C32 C 0.20706(11) 0.8639(3) 0.24788(17) 0.0414(8) Uani 1 1 d . . . O32 O 0.20957(11) 0.7647(3) 0.25429(16) 0.0677(10) Uani 1 1 d . . . C33 C 0.15763(9) 1.0200(3) 0.18317(15) 0.0327(6) Uani 1 1 d . . . O33 O 0.13079(7) 1.0151(3) 0.15095(14) 0.0489(7) Uani 1 1 d . . . C41 C 0.13184(9) 0.5584(3) 0.48333(16) 0.0342(6) Uani 1 1 d . . . O41 O 0.13523(8) 0.4900(3) 0.52395(13) 0.0510(7) Uani 1 1 d . . . C42 C 0.16181(9) 0.6443(3) 0.39502(18) 0.0382(7) Uani 1 1 d . . . O42 O 0.18291(8) 0.6243(3) 0.37541(17) 0.0629(9) Uani 1 1 d . . . C51 C 0.08881(9) 0.7327(4) 0.54256(15) 0.0392(8) Uani 1 1 d . . . O51 O 0.08665(8) 0.6975(4) 0.58988(13) 0.0656(10) Uani 1 1 d . . . C52 C 0.07857(10) 0.9458(3) 0.47228(19) 0.0402(8) Uani 1 1 d . . . O52 O 0.07111(9) 1.0427(3) 0.47299(18) 0.0608(9) Uani 1 1 d . . . C61 C 0.16236(9) 0.7523(3) 0.57558(15) 0.0351(7) Uani 1 1 d . . . O61 O 0.16732(7) 0.6955(3) 0.62058(12) 0.0482(7) Uani 1 1 d . . . C62 C 0.19146(8) 0.8374(3) 0.48577(15) 0.0335(6) Uani 1 1 d . . . O62 O 0.21639(6) 0.8408(3) 0.47664(13) 0.0447(6) Uani 1 1 d . . . C63 C 0.15216(10) 0.9912(3) 0.51986(18) 0.0415(8) Uani 1 1 d . . . O63 O 0.15191(9) 1.0898(3) 0.53009(18) 0.0656(9) Uani 1 1 d . . . C1 C 0.19177(7) 1.0597(2) 0.32354(13) 0.0231(5) Uani 1 1 d . . . C2 C 0.16643(7) 1.0027(2) 0.34048(13) 0.0238(5) Uani 1 1 d . . . C3 C 0.14277(8) 0.9592(3) 0.35156(14) 0.0265(5) Uani 1 1 d . . . C4 C 0.11338(7) 0.9174(2) 0.36388(13) 0.0228(5) Uani 1 1 d . . . O4 O 0.08547(5) 0.95007(19) 0.32921(11) 0.0298(4) Uani 1 1 d . . . C5 C 0.11871(7) 0.8361(2) 0.41827(12) 0.0225(5) Uani 1 1 d . . . P4 P 0.089259(19) 0.61403(6) 0.33642(3) 0.02394(13) Uani 1 1 d . . . C411 C 0.09786(8) 0.6333(3) 0.26031(14) 0.0305(6) Uani 1 1 d . A . C412 C 0.09039(10) 0.7387(3) 0.22445(18) 0.0395(8) Uani 1 1 d . . . H412 H 0.0801 0.8027 0.239 0.047 Uiso 1 1 calc R A . C413 C 0.09803(12) 0.7503(4) 0.16733(19) 0.0488(10) Uani 1 1 d . A . H413 H 0.0928 0.8217 0.1429 0.059 Uiso 1 1 calc R . . C414 C 0.11335(10) 0.6559(4) 0.14653(18) 0.0483(10) Uani 1 1 d . . . H414 H 0.1185 0.6627 0.1076 0.058 Uiso 1 1 calc R A . C415 C 0.12083(13) 0.5557(5) 0.1814(2) 0.0673(15) Uani 1 1 d . A . H415 H 0.1316 0.4924 0.1674 0.081 Uiso 1 1 calc R . . C416 C 0.11303(13) 0.5432(5) 0.2378(2) 0.0629(14) Uani 1 1 d . . . H416 H 0.1183 0.4709 0.2614 0.076 Uiso 1 1 calc R A . C421 C 0.0771(4) 0.4586(11) 0.3322(9) 0.033(4) Uani 0.716(10) 1 d P A 1 C422 C 0.05065(17) 0.4206(5) 0.2785(4) 0.067(3) Uani 0.716(10) 1 d P A 1 H422 H 0.0377 0.477 0.2484 0.08 Uiso 0.716(10) 1 calc PR A 1 C423 C 0.04357(18) 0.3010(6) 0.2695(5) 0.095(4) Uani 0.716(10) 1 d P A 1 H423 H 0.0254 0.2751 0.2336 0.114 Uiso 0.716(10) 1 calc PR A 1 C424 C 0.06280(17) 0.2186(5) 0.3123(5) 0.066(3) Uani 0.716(10) 1 d P A 1 H424 H 0.0574 0.1365 0.3058 0.08 Uiso 0.716(10) 1 calc PR A 1 C425 C 0.0897(5) 0.2533(14) 0.3644(9) 0.054(5) Uani 0.716(10) 1 d P A 1 H425 H 0.1028 0.1968 0.3942 0.065 Uiso 0.716(10) 1 calc PR A 1 C426 C 0.0968(3) 0.3735(10) 0.3714(5) 0.0345(18) Uani 0.716(10) 1 d P A 1 H426 H 0.1163 0.3983 0.4048 0.041 Uiso 0.716(10) 1 calc PR A 1 C431 C 0.0782(14) 0.457(4) 0.333(3) 0.045(14) Uiso 0.284(10) 1 d P A 2 C432 C 0.0436(3) 0.4149(11) 0.3146(6) 0.030(2) Uiso 0.284(10) 1 d P A 2 H432 H 0.0258 0.4699 0.2987 0.036 Uiso 0.284(10) 1 calc PR A 2 C433 C 0.0366(3) 0.2940(12) 0.3199(7) 0.038(3) Uiso 0.284(10) 1 d P A 2 H433 H 0.0141 0.2676 0.3034 0.046 Uiso 0.284(10) 1 calc PR A 2 C434 C 0.0610(4) 0.2139(14) 0.3479(7) 0.038(3) Uiso 0.284(10) 1 d P A 2 H434 H 0.0564 0.1332 0.3548 0.046 Uiso 0.284(10) 1 calc PR A 2 C435 C 0.0924(12) 0.258(4) 0.3652(15) 0.035(6) Uiso 0.284(10) 1 d P A 2 H435 H 0.1101 0.2013 0.3778 0.042 Uiso 0.284(10) 1 calc PR A 2 C436 C 0.1016(6) 0.376(2) 0.3663(11) 0.021(3) Uiso 0.284(10) 1 d P A 2 H436 H 0.1237 0.4008 0.3897 0.025 Uiso 0.284(10) 1 calc PR A 2 C0 C 0.05092(7) 0.6999(2) 0.32269(13) 0.0236(5) Uani 1 1 d . A . H0A H 0.0316 0.6541 0.295 0.028 Uiso 1 1 calc R . . H0B H 0.0523 0.7753 0.3004 0.028 Uiso 1 1 calc R . . P5 P 0.045537(19) 0.73118(7) 0.40070(4) 0.02585(14) Uani 1 1 d . . . C511 C 0.01204(8) 0.8402(3) 0.38294(15) 0.0344(7) Uani 1 1 d D A . C512 C -0.00571(15) 0.8554(6) 0.4251(2) 0.0776(18) Uani 1 1 d D . . H512 H -0.0019 0.8028 0.4607 0.093 Uiso 1 1 calc R A . C513 C -0.02907(17) 0.9462(6) 0.4166(3) 0.091(2) Uani 1 1 d D A . H513 H -0.0405 0.9557 0.447 0.109 Uiso 1 1 calc R . . C514 C -0.03581(12) 1.0220(4) 0.3652(2) 0.0595(12) Uani 1 1 d D . . H514 H -0.0521 1.0828 0.3585 0.071 Uiso 1 1 calc R A . C515 C -0.01816(12) 1.0067(4) 0.3239(2) 0.0582(11) Uani 1 1 d D A . H515 H -0.0224 1.0576 0.2875 0.07 Uiso 1 1 calc R . . C516 C 0.00586(10) 0.9189(3) 0.3335(2) 0.0467(9) Uani 1 1 d D . . H516 H 0.0184 0.9135 0.3046 0.056 Uiso 1 1 calc R A . C521 C 0.02587(8) 0.5958(3) 0.41580(15) 0.0336(7) Uani 1 1 d . A . C522 C 0.04460(9) 0.5089(3) 0.45732(18) 0.0408(8) Uani 1 1 d . . . H522 H 0.0673 0.5241 0.4817 0.049 Uiso 1 1 calc R A . C523 C 0.03028(12) 0.3999(4) 0.4632(2) 0.0551(11) Uani 1 1 d . A . H523 H 0.0433 0.3403 0.4909 0.066 Uiso 1 1 calc R . . C524 C -0.00275(12) 0.3786(4) 0.4289(2) 0.0586(12) Uani 1 1 d . . . H524 H -0.0123 0.3036 0.4323 0.07 Uiso 1 1 calc R A . C525 C -0.02198(11) 0.4653(5) 0.3897(2) 0.0616(13) Uani 1 1 d . A . H525 H -0.045 0.4509 0.3674 0.074 Uiso 1 1 calc R . . C526 C -0.00781(9) 0.5740(4) 0.3825(2) 0.0501(10) Uani 1 1 d . . . H526 H -0.0211 0.6333 0.3549 0.06 Uiso 1 1 calc R A . H1 H 0.2001(10) 1.188(4) 0.234(2) 0.044(11) Uiso 1 1 d . . . H2 H 0.2441(11) 1.059(4) 0.288(2) 0.045(12) Uiso 1 1 d . . . H3 H 0.2315(16) 1.236(5) 0.338(3) 0.09(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02294(10) 0.02780(11) 0.02529(10) 0.00516(8) 0.00914(8) 0.00193(8) Ru2 0.02203(9) 0.02202(10) 0.02498(10) 0.00267(7) 0.00878(8) -0.00026(8) Ru3 0.03118(11) 0.02512(10) 0.02371(10) 0.00189(8) 0.01334(8) 0.00031(8) Co4 0.02455(17) 0.02375(17) 0.02127(16) 0.00180(13) 0.00663(13) -0.00207(14) Co5 0.02864(19) 0.03106(19) 0.02107(16) -0.00175(14) 0.01227(14) -0.00716(15) Co6 0.02833(19) 0.0316(2) 0.02003(16) -0.00056(14) 0.00704(14) -0.00852(15) C11 0.0293(15) 0.0435(19) 0.0413(18) 0.0099(14) 0.0103(13) 0.0031(14) O11 0.0290(13) 0.071(2) 0.069(2) 0.0144(16) 0.0117(13) -0.0064(13) C12 0.0411(17) 0.0360(16) 0.0354(16) 0.0095(13) 0.0168(14) 0.0102(14) O12 0.070(2) 0.0396(14) 0.0559(17) 0.0156(13) 0.0272(15) 0.0231(14) C13 0.0336(15) 0.0305(14) 0.0298(14) 0.0025(11) 0.0091(12) -0.0012(12) O13 0.0608(17) 0.0465(15) 0.0309(12) -0.0014(11) 0.0173(12) -0.0066(13) C21 0.0294(14) 0.0276(14) 0.0355(15) 0.0036(11) 0.0101(12) -0.0006(11) O21 0.0448(14) 0.0353(13) 0.0607(17) 0.0170(12) 0.0216(13) -0.0025(11) C22 0.0321(15) 0.0313(15) 0.0297(14) 0.0004(11) 0.0086(12) 0.0028(12) O22 0.0278(12) 0.0579(17) 0.0488(15) -0.0053(13) 0.0037(11) 0.0024(11) C23 0.0259(13) 0.0329(15) 0.0349(15) 0.0001(12) 0.0081(12) 0.0034(11) O23 0.0465(15) 0.0633(18) 0.0398(14) -0.0115(13) 0.0166(12) 0.0090(13) C31 0.0366(16) 0.0380(16) 0.0296(14) 0.0042(12) 0.0158(13) 0.0053(13) O31 0.0486(15) 0.0702(19) 0.0325(12) 0.0108(12) 0.0216(12) 0.0131(14) C32 0.065(2) 0.0291(15) 0.0330(16) -0.0014(12) 0.0196(16) 0.0019(15) O32 0.118(3) 0.0288(14) 0.0573(19) -0.0007(13) 0.029(2) 0.0068(16) C33 0.0400(17) 0.0319(15) 0.0292(14) -0.0014(11) 0.0152(13) -0.0067(13) O33 0.0405(14) 0.0578(17) 0.0446(15) -0.0047(13) 0.0086(12) -0.0148(13) C41 0.0358(16) 0.0333(15) 0.0320(15) 0.0022(12) 0.0089(13) -0.0020(13) O41 0.0686(19) 0.0431(15) 0.0381(14) 0.0168(11) 0.0128(13) 0.0036(14) C42 0.0350(16) 0.0393(18) 0.0413(18) -0.0066(14) 0.0138(14) -0.0034(14) O42 0.0424(16) 0.081(2) 0.075(2) -0.0188(18) 0.0323(16) -0.0024(16) C51 0.0338(16) 0.059(2) 0.0241(13) -0.0039(14) 0.0085(12) -0.0192(15) O51 0.0586(19) 0.112(3) 0.0273(12) 0.0081(15) 0.0154(13) -0.0343(19) C52 0.0435(19) 0.0415(19) 0.0446(19) -0.0101(15) 0.0265(16) -0.0083(15) O52 0.073(2) 0.0394(15) 0.088(2) -0.0159(15) 0.051(2) -0.0056(14) C61 0.0354(16) 0.0445(18) 0.0226(13) -0.0020(12) 0.0059(11) -0.0145(14) O61 0.0563(17) 0.0575(17) 0.0254(11) 0.0065(11) 0.0060(11) -0.0179(13) C62 0.0328(15) 0.0384(16) 0.0258(13) 0.0049(12) 0.0047(11) -0.0053(13) O62 0.0324(12) 0.0574(17) 0.0455(14) 0.0105(12) 0.0144(11) -0.0048(11) C63 0.0442(19) 0.0399(18) 0.0380(17) -0.0058(14) 0.0100(15) -0.0107(15) O63 0.080(2) 0.0384(16) 0.075(2) -0.0142(15) 0.0204(19) -0.0161(16) C1 0.0246(12) 0.0249(12) 0.0199(11) 0.0009(9) 0.0077(9) 0.0015(9) C2 0.0274(12) 0.0228(11) 0.0222(11) 0.0020(9) 0.0097(10) 0.0001(10) C3 0.0318(14) 0.0243(12) 0.0243(12) 0.0024(10) 0.0101(11) -0.0027(11) C4 0.0274(12) 0.0198(11) 0.0238(11) -0.0022(9) 0.0120(10) -0.0034(9) O4 0.0259(10) 0.0275(10) 0.0354(11) 0.0073(8) 0.0092(9) 0.0004(8) C5 0.0239(12) 0.0244(12) 0.0206(11) -0.0009(9) 0.0092(9) -0.0049(9) P4 0.0270(3) 0.0211(3) 0.0226(3) -0.0005(2) 0.0065(3) 0.0004(3) C411 0.0285(14) 0.0418(17) 0.0211(12) -0.0040(11) 0.0079(10) 0.0038(12) C412 0.051(2) 0.0379(17) 0.0398(17) -0.0037(14) 0.0284(16) -0.0040(15) C413 0.069(3) 0.049(2) 0.0405(19) -0.0029(16) 0.0339(19) -0.0100(19) C414 0.0374(18) 0.082(3) 0.0307(16) -0.0122(18) 0.0187(14) -0.0028(19) C415 0.076(3) 0.091(4) 0.040(2) -0.002(2) 0.026(2) 0.045(3) C416 0.080(3) 0.070(3) 0.041(2) 0.008(2) 0.023(2) 0.046(3) C421 0.028(4) 0.015(3) 0.046(6) -0.0044(16) -0.0025(19) 0.0004(15) C422 0.049(3) 0.028(2) 0.087(6) -0.010(3) -0.027(4) 0.002(2) C423 0.052(4) 0.029(3) 0.152(10) -0.021(4) -0.035(5) -0.003(3) C424 0.051(4) 0.021(2) 0.114(7) -0.010(3) 0.010(4) -0.006(2) C425 0.062(8) 0.019(3) 0.087(8) 0.006(3) 0.031(5) 0.004(3) C426 0.037(4) 0.026(2) 0.044(4) 0.005(2) 0.018(3) 0.000(3) C0 0.0255(12) 0.0238(12) 0.0215(11) 0.0036(9) 0.0077(9) 0.0023(10) P5 0.0247(3) 0.0330(4) 0.0212(3) 0.0032(3) 0.0093(3) -0.0015(3) C511 0.0288(14) 0.0456(18) 0.0318(15) -0.0012(13) 0.0139(12) 0.0037(13) C512 0.086(4) 0.108(5) 0.059(3) 0.027(3) 0.052(3) 0.045(3) C513 0.096(5) 0.111(5) 0.092(4) 0.009(4) 0.067(4) 0.044(4) C514 0.052(2) 0.056(3) 0.072(3) -0.008(2) 0.022(2) 0.019(2) C515 0.058(3) 0.052(2) 0.066(3) 0.006(2) 0.024(2) 0.023(2) C516 0.049(2) 0.045(2) 0.053(2) 0.0057(17) 0.0273(18) 0.0155(17) C521 0.0292(14) 0.0442(18) 0.0264(13) 0.0059(12) 0.0078(11) -0.0118(13) C522 0.0367(17) 0.0431(19) 0.0401(18) 0.0092(14) 0.0092(14) -0.0125(15) C523 0.057(3) 0.054(2) 0.053(2) 0.0196(19) 0.015(2) -0.012(2) C524 0.059(3) 0.062(3) 0.051(2) 0.013(2) 0.014(2) -0.029(2) C525 0.046(2) 0.078(3) 0.052(2) 0.018(2) 0.0044(19) -0.032(2) C526 0.0321(17) 0.068(3) 0.045(2) 0.0201(19) 0.0049(15) -0.0145(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ru1 C12 1.909(3) . ? Ru1 C13 1.912(3) . ? Ru1 C11 1.982(4) . ? Ru1 C1 2.071(3) . ? Ru1 Ru3 2.8448(4) . ? Ru1 Ru2 2.8451(4) . ? Ru1 H2 1.79(4) . ? Ru1 H3 1.86(6) . ? Ru2 C23 1.902(3) . ? Ru2 C22 1.915(3) . ? Ru2 C21 1.966(3) . ? Ru2 C1 2.093(3) . ? Ru2 Ru3 2.8529(4) . ? Ru2 H1 1.77(4) . ? Ru2 H3 1.66(6) . ? Ru3 C33 1.911(3) . ? Ru3 C32 1.920(4) . ? Ru3 C31 1.981(3) . ? Ru3 C1 2.085(3) . ? Ru3 H1 1.74(4) . ? Ru3 H2 1.76(4) . ? Co4 C41 1.783(3) . ? Co4 C42 1.787(4) . ? Co4 C5 1.873(3) . ? Co4 P4 2.1999(8) . ? Co4 Co6 2.4705(6) . ? Co4 Co5 2.4914(6) . ? Co5 C52 1.778(4) . ? Co5 C51 1.796(3) . ? Co5 C5 1.892(3) . ? Co5 P5 2.1861(9) . ? Co5 Co6 2.4677(6) . ? Co6 C63 1.789(4) . ? Co6 C62 1.789(4) . ? Co6 C61 1.813(3) . ? Co6 C5 1.912(3) . ? C11 O11 1.122(4) . ? C12 O12 1.125(4) . ? C13 O13 1.131(4) . ? C21 O21 1.130(4) . ? C22 O22 1.130(4) . ? C23 O23 1.135(4) . ? C31 O31 1.125(4) . ? C32 O32 1.125(4) . ? C33 O33 1.128(4) . ? C41 O41 1.150(4) . ? C42 O42 1.134(4) . ? C51 O51 1.141(4) . ? C52 O52 1.136(5) . ? C61 O61 1.136(4) . ? C62 O62 1.139(4) . ? C63 O63 1.132(5) . ? C1 C2 1.401(4) . ? C2 C3 1.210(4) . ? C3 C4 1.437(4) . ? C4 O4 1.235(3) . ? C4 C5 1.460(4) . ? P4 C421 1.816(13) . ? P4 C431 1.82(5) . ? P4 C0 1.828(3) . ? P4 C411 1.833(3) . ? C411 C416 1.374(5) . ? C411 C412 1.400(5) . ? C412 C413 1.398(5) . ? C412 H412 0.95 . ? C413 C414 1.396(6) . ? C413 H413 0.95 . ? C414 C415 1.341(7) . ? C414 H414 0.95 . ? C415 C416 1.386(6) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C426 1.37(2) . ? C421 C422 1.401(17) . ? C422 C423 1.377(8) . ? C422 H422 0.95 . ? C423 C424 1.380(11) . ? C423 H423 0.95 . ? C424 C425 1.38(2) . ? C424 H424 0.95 . ? C425 C426 1.38(2) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C431 C436 1.37(6) . ? C431 C432 1.46(6) . ? C432 C433 1.404(18) . ? C432 H432 0.95 . ? C433 C434 1.36(2) . ? C433 H433 0.95 . ? C434 C435 1.35(5) . ? C434 H434 0.95 . ? C435 C436 1.38(5) . ? C435 H435 0.95 . ? C436 H436 0.95 . ? C0 P5 1.832(3) . ? C0 H0A 0.99 . ? C0 H0B 0.99 . ? P5 C521 1.816(3) . ? P5 C511 1.819(3) . ? C511 C516 1.357(5) . ? C511 C512 1.380(5) . ? C512 C513 1.392(6) . ? C512 H512 0.95 . ? C513 C514 1.366(6) . ? C513 H513 0.95 . ? C514 C515 1.361(6) . ? C514 H514 0.95 . ? C515 C516 1.384(5) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C522 1.393(5) . ? C521 C526 1.397(5) . ? C522 C523 1.392(5) . ? C522 H522 0.95 . ? C523 C524 1.377(6) . ? C523 H523 0.95 . ? C524 C525 1.377(7) . ? C524 H524 0.95 . ? C525 C526 1.393(6) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? 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 C12 Ru1 C13 91.28(14) . . ? C12 Ru1 C11 96.27(16) . . ? C13 Ru1 C11 98.23(15) . . ? C12 Ru1 C1 98.73(14) . . ? C13 Ru1 C1 94.29(12) . . ? C11 Ru1 C1 160.20(13) . . ? C12 Ru1 Ru3 93.89(11) . . ? C13 Ru1 Ru3 141.29(10) . . ? C11 Ru1 Ru3 119.20(11) . . ? C1 Ru1 Ru3 47.01(7) . . ? C12 Ru1 Ru2 145.48(12) . . ? C13 Ru1 Ru2 96.22(10) . . ? C11 Ru1 Ru2 115.77(10) . . ? C1 Ru1 Ru2 47.22(8) . . ? Ru3 Ru1 Ru2 60.185(9) . . ? C12 Ru1 H2 89.2(14) . . ? C13 Ru1 H2 177.6(14) . . ? C11 Ru1 H2 84.0(14) . . ? C1 Ru1 H2 83.3(14) . . ? Ru3 Ru1 H2 36.3(14) . . ? Ru2 Ru1 H2 82.1(14) . . ? C12 Ru1 H3 171.7(19) . . ? C13 Ru1 H3 97.0(19) . . ? C11 Ru1 H3 82.5(19) . . ? C1 Ru1 H3 80.8(19) . . ? Ru3 Ru1 H3 79.7(19) . . ? Ru2 Ru1 H3 33.7(19) . . ? H2 Ru1 H3 82(2) . . ? C23 Ru2 C22 93.00(14) . . ? C23 Ru2 C21 96.09(14) . . ? C22 Ru2 C21 95.96(13) . . ? C23 Ru2 C1 97.46(12) . . ? C22 Ru2 C1 92.44(12) . . ? C21 Ru2 C1 163.64(12) . . ? C23 Ru2 Ru1 93.78(9) . . ? C22 Ru2 Ru1 139.01(10) . . ? C21 Ru2 Ru1 123.34(9) . . ? C1 Ru2 Ru1 46.59(8) . . ? C23 Ru2 Ru3 143.99(10) . . ? C22 Ru2 Ru3 93.05(10) . . ? C21 Ru2 Ru3 118.49(10) . . ? C1 Ru2 Ru3 46.82(7) . . ? Ru1 Ru2 Ru3 59.902(9) . . ? C23 Ru2 H1 174.7(13) . . ? C22 Ru2 H1 92.3(13) . . ? C21 Ru2 H1 83.6(14) . . ? C1 Ru2 H1 82.0(14) . . ? Ru1 Ru2 H1 82.1(14) . . ? Ru3 Ru2 H1 35.2(14) . . ? C23 Ru2 H3 91(2) . . ? C22 Ru2 H3 176(2) . . ? C21 Ru2 H3 86(2) . . ? C1 Ru2 H3 85(2) . . ? Ru1 Ru2 H3 38(2) . . ? Ru3 Ru2 H3 83(2) . . ? H1 Ru2 H3 84(3) . . ? C33 Ru3 C32 91.59(16) . . ? C33 Ru3 C31 96.50(14) . . ? C32 Ru3 C31 95.66(15) . . ? C33 Ru3 C1 96.16(12) . . ? C32 Ru3 C1 94.90(13) . . ? C31 Ru3 C1 163.25(13) . . ? C33 Ru3 Ru1 142.61(10) . . ? C32 Ru3 Ru1 94.63(11) . . ? C31 Ru3 Ru1 119.41(10) . . ? C1 Ru3 Ru1 46.61(8) . . ? C33 Ru3 Ru2 93.97(10) . . ? C32 Ru3 Ru2 141.90(11) . . ? C31 Ru3 Ru2 120.99(10) . . ? C1 Ru3 Ru2 47.04(8) . . ? Ru1 Ru3 Ru2 59.913(9) . . ? C33 Ru3 H1 90.5(14) . . ? C32 Ru3 H1 177.3(14) . . ? C31 Ru3 H1 85.9(14) . . ? C1 Ru3 H1 83.1(14) . . ? Ru1 Ru3 H1 82.6(14) . . ? Ru2 Ru3 H1 36.1(14) . . ? C33 Ru3 H2 175.1(14) . . ? C32 Ru3 H2 93.3(14) . . ? C31 Ru3 H2 82.6(14) . . ? C1 Ru3 H2 83.8(14) . . ? Ru1 Ru3 H2 37.2(14) . . ? Ru2 Ru3 H2 82.4(14) . . ? H1 Ru3 H2 84.7(19) . . ? C41 Co4 C42 103.87(17) . . ? C41 Co4 C5 136.94(14) . . ? C42 Co4 C5 108.78(15) . . ? C41 Co4 P4 106.35(11) . . ? C42 Co4 P4 94.50(12) . . ? C5 Co4 P4 98.36(8) . . ? C41 Co4 Co6 97.70(11) . . ? C42 Co4 Co6 99.99(12) . . ? C5 Co4 Co6 49.94(8) . . ? P4 Co4 Co6 147.99(3) . . ? C41 Co4 Co5 92.49(12) . . ? C42 Co4 Co5 155.81(12) . . ? C5 Co4 Co5 48.89(8) . . ? P4 Co4 Co5 97.87(3) . . ? Co6 Co4 Co5 59.644(17) . . ? C52 Co5 C51 103.37(18) . . ? C52 Co5 C5 93.34(14) . . ? C51 Co5 C5 149.13(15) . . ? C52 Co5 P5 96.41(13) . . ? C51 Co5 P5 99.60(11) . . ? C5 Co5 P5 104.16(8) . . ? C52 Co5 Co6 97.83(12) . . ? C51 Co5 Co6 101.52(11) . . ? C5 Co5 Co6 49.91(8) . . ? P5 Co5 Co6 150.97(3) . . ? C52 Co5 Co4 141.57(11) . . ? C51 Co5 Co4 111.16(14) . . ? C5 Co5 Co4 48.23(9) . . ? P5 Co5 Co4 94.02(3) . . ? Co6 Co5 Co4 59.757(17) . . ? C63 Co6 C62 96.59(17) . . ? C63 Co6 C61 108.51(17) . . ? C62 Co6 C61 102.55(15) . . ? C63 Co6 C5 99.22(15) . . ? C62 Co6 C5 105.85(13) . . ? C61 Co6 C5 137.30(13) . . ? C63 Co6 Co5 98.87(13) . . ? C62 Co6 Co5 152.47(10) . . ? C61 Co6 Co5 93.95(11) . . ? C5 Co6 Co5 49.20(8) . . ? C63 Co6 Co4 147.73(12) . . ? C62 Co6 Co4 94.97(11) . . ? C61 Co6 Co4 98.16(11) . . ? C5 Co6 Co4 48.56(8) . . ? Co5 Co6 Co4 60.600(16) . . ? O11 C11 Ru1 176.6(3) . . ? O12 C12 Ru1 177.6(3) . . ? O13 C13 Ru1 178.3(3) . . ? O21 C21 Ru2 176.5(3) . . ? O22 C22 Ru2 176.9(3) . . ? O23 C23 Ru2 177.6(3) . . ? O31 C31 Ru3 178.4(3) . . ? O32 C32 Ru3 179.0(3) . . ? O33 C33 Ru3 178.1(3) . . ? O41 C41 Co4 175.5(3) . . ? O42 C42 Co4 178.7(4) . . ? O51 C51 Co5 176.7(4) . . ? O52 C52 Co5 176.9(3) . . ? O61 C61 Co6 176.5(3) . . ? O62 C62 Co6 178.3(3) . . ? O63 C63 Co6 178.2(4) . . ? C2 C1 Ru1 134.4(2) . . ? C2 C1 Ru3 126.0(2) . . ? Ru1 C1 Ru3 86.38(11) . . ? C2 C1 Ru2 122.7(2) . . ? Ru1 C1 Ru2 86.20(11) . . ? Ru3 C1 Ru2 86.14(10) . . ? C3 C2 C1 174.8(3) . . ? C2 C3 C4 175.1(3) . . ? O4 C4 C3 120.2(3) . . ? O4 C4 C5 123.4(3) . . ? C3 C4 C5 116.5(2) . . ? C4 C5 Co4 130.6(2) . . ? C4 C5 Co5 132.1(2) . . ? Co4 C5 Co5 82.88(11) . . ? C4 C5 Co6 130.0(2) . . ? Co4 C5 Co6 81.50(11) . . ? Co5 C5 Co6 80.90(10) . . ? C421 P4 C0 106.0(6) . . ? C431 P4 C0 107.5(18) . . ? C421 P4 C411 101.9(7) . . ? C431 P4 C411 101.8(18) . . ? C0 P4 C411 102.61(13) . . ? C421 P4 Co4 116.9(6) . . ? C431 P4 Co4 115.8(18) . . ? C0 P4 Co4 110.85(9) . . ? C411 P4 Co4 117.04(11) . . ? C416 C411 C412 117.9(3) . . ? C416 C411 P4 119.7(3) . . ? C412 C411 P4 122.3(2) . . ? C413 C412 C411 120.4(3) . . ? C413 C412 H412 119.8 . . ? C411 C412 H412 119.8 . . ? C414 C413 C412 119.4(4) . . ? C414 C413 H413 120.3 . . ? C412 C413 H413 120.3 . . ? C415 C414 C413 120.0(4) . . ? C415 C414 H414 120 . . ? C413 C414 H414 120 . . ? C414 C415 C416 120.9(4) . . ? C414 C415 H415 119.6 . . ? C416 C415 H415 119.6 . . ? C411 C416 C415 121.4(4) . . ? C411 C416 H416 119.3 . . ? C415 C416 H416 119.3 . . ? C426 C421 C422 118.0(10) . . ? C426 C421 P4 122.2(11) . . ? C422 C421 P4 118.2(11) . . ? C423 C422 C421 119.7(8) . . ? C423 C422 H422 120.1 . . ? C421 C422 H422 120.1 . . ? C422 C423 C424 120.3(6) . . ? C422 C423 H423 119.8 . . ? C424 C423 H423 119.8 . . ? C423 C424 C425 121.2(8) . . ? C423 C424 H424 119.4 . . ? C425 C424 H424 119.4 . . ? C424 C425 C426 117.4(14) . . ? C424 C425 H425 121.3 . . ? C426 C425 H425 121.3 . . ? C421 C426 C425 123.0(13) . . ? C421 C426 H426 118.5 . . ? C425 C426 H426 118.5 . . ? C436 C431 C432 115(4) . . ? C436 C431 P4 119(4) . . ? C432 C431 P4 123(3) . . ? C433 C432 C431 121(2) . . ? C433 C432 H432 119.6 . . ? C431 C432 H432 119.6 . . ? C434 C433 C432 121.8(13) . . ? C434 C433 H433 119.1 . . ? C432 C433 H433 119.1 . . ? C435 C434 C433 115(2) . . ? C435 C434 H434 122.6 . . ? C433 C434 H434 122.6 . . ? C434 C435 C436 127(4) . . ? C434 C435 H435 116.6 . . ? C436 C435 H435 116.6 . . ? C431 C436 C435 119(3) . . ? C431 C436 H436 120.7 . . ? C435 C436 H436 120.7 . . ? P4 C0 P5 108.83(14) . . ? P4 C0 H0A 109.9 . . ? P5 C0 H0A 109.9 . . ? P4 C0 H0B 109.9 . . ? P5 C0 H0B 109.9 . . ? H0A C0 H0B 108.3 . . ? C521 P5 C511 103.33(16) . . ? C521 P5 C0 102.33(15) . . ? C511 P5 C0 104.84(13) . . ? C521 P5 Co5 121.32(11) . . ? C511 P5 Co5 112.74(12) . . ? C0 P5 Co5 110.63(10) . . ? C516 C511 C512 116.7(4) . . ? C516 C511 P5 122.9(3) . . ? C512 C511 P5 119.9(3) . . ? C511 C512 C513 121.3(4) . . ? C511 C512 H512 119.3 . . ? C513 C512 H512 119.3 . . ? C514 C513 C512 121.1(4) '. ' . ? data_br1081 _database_code_depnum_ccdc_archive 'CCDC 754938' #TrackingRef '11.br1081.cif' _audit_creation_date 2009-04-28T20:41:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C46 H25 Co3 O17 Os3 P2' _chemical_formula_sum 'C46 H25 Co3 O17 Os3 P2' _chemical_formula_weight 1658.99 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _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 42.439(9) _cell_length_b 11.250(2) _cell_length_c 21.854(5) _cell_angle_alpha 90 _cell_angle_beta 108.740(3) _cell_angle_gamma 90 _cell_volume 9881(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6291 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.9 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.23 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6208 _exptl_special_details ; Bruker SMART CCD diffractometer ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.84 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_unetI/netI 0.0986 _diffrn_reflns_number 44937 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 8667 _reflns_number_gt 5689 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1068P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8667 _refine_ls_number_parameters 334 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_gt 0.064 _refine_ls_wR_factor_ref 0.1816 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.738 _refine_diff_density_min -2.8 _refine_diff_density_rms 0.493 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.603 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Os1 Os 0.243428(15) 1.08364(5) 0.36951(3) 0.02457(18) Uani 1 1 d D . . Os2 Os 0.190879(15) 1.24493(5) 0.30230(3) 0.02242(18) Uani 1 1 d D . . Os3 Os 0.203689(16) 1.03506(5) 0.23779(3) 0.02548(18) Uani 1 1 d D . . Co4 Co 0.12819(5) 0.67311(18) 0.42457(9) 0.0240(5) Uani 1 1 d . . . Co5 Co 0.09192(5) 0.79627(19) 0.46950(9) 0.0261(5) Uani 1 1 d . . . Co6 Co 0.15240(5) 0.83697(19) 0.50087(9) 0.0283(5) Uani 1 1 d . . . C11 C 0.2883(4) 1.1423(15) 0.3876(8) 0.034(4) Uiso 1 1 d . . . O11 O 0.3144(3) 1.1826(11) 0.3988(6) 0.049(3) Uiso 1 1 d . . . C12 C 0.2556(4) 0.9282(14) 0.3885(8) 0.032(4) Uiso 1 1 d . . . O12 O 0.2629(3) 0.8265(12) 0.3980(6) 0.055(4) Uiso 1 1 d . . . C13 C 0.2400(4) 1.1040(13) 0.4536(8) 0.029(4) Uiso 1 1 d . . . O13 O 0.2371(3) 1.1195(10) 0.5042(6) 0.044(3) Uiso 1 1 d . . . C21 C 0.1990(4) 1.3996(14) 0.2701(8) 0.033(4) Uiso 1 1 d . . . O21 O 0.2020(3) 1.4881(11) 0.2494(6) 0.047(3) Uiso 1 1 d . . . C22 C 0.1442(4) 1.2416(14) 0.2571(8) 0.034(4) Uiso 1 1 d . . . O22 O 0.1165(3) 1.2347(11) 0.2293(6) 0.051(3) Uiso 1 1 d . . . C23 C 0.1847(4) 1.3010(15) 0.3787(8) 0.035(4) Uiso 1 1 d . . . O23 O 0.1820(3) 1.3341(10) 0.4266(6) 0.046(3) Uiso 1 1 d . . . C31 C 0.2229(4) 1.0459(14) 0.1676(8) 0.033(4) Uiso 1 1 d . . . O31 O 0.2347(3) 1.0528(11) 0.1282(6) 0.048(3) Uiso 1 1 d . . . C32 C 0.2086(4) 0.8680(16) 0.2449(8) 0.041(4) Uiso 1 1 d . . . O32 O 0.2116(4) 0.7684(13) 0.2522(7) 0.061(4) Uiso 1 1 d . . . C33 C 0.1588(4) 1.0188(13) 0.1821(7) 0.024(3) Uiso 1 1 d . . . O33 O 0.1317(3) 1.0155(11) 0.1513(6) 0.046(3) Uiso 1 1 d . . . C41 C 0.1320(4) 0.5574(14) 0.4834(8) 0.033(4) Uiso 1 1 d . . . O41 O 0.1359(3) 0.4900(12) 0.5233(7) 0.055(4) Uiso 1 1 d . . . C42 C 0.1613(5) 0.6430(16) 0.3950(9) 0.043(4) Uiso 1 1 d . . . O42 O 0.1829(4) 0.6258(13) 0.3753(7) 0.067(4) Uiso 1 1 d . . . C51 C 0.0883(4) 0.7349(15) 0.5409(9) 0.040(4) Uiso 1 1 d . . . O51 O 0.0870(4) 0.6975(13) 0.5905(7) 0.068(4) Uiso 1 1 d . . . C52 C 0.0795(4) 0.9428(16) 0.4733(9) 0.040(4) Uiso 1 1 d . . . O52 O 0.0708(3) 1.0377(12) 0.4727(7) 0.059(4) Uiso 1 1 d . . . C61 C 0.1609(4) 0.7516(14) 0.5746(8) 0.032(4) Uiso 1 1 d . . . O61 O 0.1666(3) 0.6968(11) 0.6215(6) 0.048(3) Uiso 1 1 d . . . C62 C 0.1909(4) 0.8398(15) 0.4835(8) 0.038(4) Uiso 1 1 d . . . O62 O 0.2159(3) 0.8433(10) 0.4768(6) 0.044(3) Uiso 1 1 d . . . C63 C 0.1523(4) 0.9901(16) 0.5190(8) 0.038(4) Uiso 1 1 d . . . O63 O 0.1513(4) 1.0910(13) 0.5280(7) 0.066(4) Uiso 1 1 d . . . C1 C 0.1924(4) 1.0599(13) 0.3247(7) 0.026(3) Uiso 1 1 d . . . C2 C 0.1663(4) 1.0019(13) 0.3404(7) 0.025(3) Uiso 1 1 d . . . C3 C 0.1431(4) 0.9599(13) 0.3500(7) 0.024(3) Uiso 1 1 d . . . C4 C 0.1135(4) 0.9188(12) 0.3620(7) 0.023(3) Uiso 1 1 d . . . O4 O 0.0857(3) 0.9501(9) 0.3280(5) 0.034(3) Uiso 1 1 d . . . C5 C 0.1183(4) 0.8375(13) 0.4175(7) 0.024(3) Uiso 1 1 d . . . P4 P 0.08963(10) 0.6145(3) 0.33580(18) 0.0248(9) Uani 1 1 d . . . C411 C 0.0975(4) 0.6346(14) 0.2596(7) 0.029(4) Uiso 1 1 d . . . C412 C 0.0919(5) 0.7385(17) 0.2264(10) 0.053(5) Uiso 1 1 d . . . H412 H 0.0835 0.8044 0.2434 0.063 Uiso 1 1 calc R . . C413 C 0.0985(6) 0.752(2) 0.1658(11) 0.065(6) Uiso 1 1 d . . . H413 H 0.0924 0.8224 0.1408 0.079 Uiso 1 1 calc R . . C414 C 0.1138(5) 0.6582(16) 0.1456(9) 0.046(5) Uiso 1 1 d . . . H414 H 0.1195 0.6661 0.1072 0.055 Uiso 1 1 calc R . . C415 C 0.1203(6) 0.562(2) 0.1775(12) 0.073(7) Uiso 1 1 d . . . H415 H 0.1299 0.4969 0.1619 0.088 Uiso 1 1 calc R . . C416 C 0.1133(5) 0.5509(19) 0.2353(10) 0.058(6) Uiso 1 1 d . . . H416 H 0.1201 0.48 0.2596 0.069 Uiso 1 1 calc R . . C421 C 0.0776(4) 0.4557(14) 0.3309(8) 0.036(4) Uiso 1 1 d . . . C422 C 0.0500(7) 0.422(3) 0.2805(15) 0.097(9) Uiso 1 1 d . . . H422 H 0.0367 0.4769 0.25 0.117 Uiso 1 1 calc R . . C423 C 0.0435(8) 0.298(3) 0.2786(16) 0.119(11) Uiso 1 1 d . . . H423 H 0.0244 0.2695 0.2459 0.143 Uiso 1 1 calc R . . C424 C 0.0634(7) 0.217(3) 0.3216(14) 0.097(9) Uiso 1 1 d . . . H424 H 0.0567 0.1366 0.3206 0.116 Uiso 1 1 calc R . . C425 C 0.0919(5) 0.2528(16) 0.3644(9) 0.046(5) Uiso 1 1 d . . . H425 H 0.1072 0.1974 0.3908 0.056 Uiso 1 1 calc R . . C426 C 0.0984(5) 0.3745(15) 0.3688(9) 0.042(4) Uiso 1 1 d . . . H426 H 0.1184 0.4017 0.3997 0.05 Uiso 1 1 calc R . . C0 C 0.0512(4) 0.6992(13) 0.3229(7) 0.023(3) Uiso 1 1 d . . . H0A H 0.0524 0.7746 0.3003 0.028 Uiso 1 1 calc R . . H0B H 0.032 0.653 0.2955 0.028 Uiso 1 1 calc R . . P5 P 0.04570(11) 0.7307(4) 0.40025(19) 0.0295(10) Uani 1 1 d . . . C511 C 0.0117(5) 0.8402(16) 0.3817(9) 0.045(5) Uiso 1 1 d . . . C512 C -0.0053(6) 0.861(2) 0.4250(13) 0.084(8) Uiso 1 1 d . . . H512 H -0.0004 0.8111 0.4619 0.101 Uiso 1 1 calc R . . C513 C -0.0303(8) 0.954(3) 0.4184(16) 0.104(9) Uiso 1 1 d . . . H513 H -0.042 0.964 0.4485 0.125 Uiso 1 1 calc R . . C514 C -0.0352(5) 1.023(2) 0.3673(11) 0.062(6) Uiso 1 1 d . . . H514 H -0.0507 1.086 0.3602 0.074 Uiso 1 1 calc R . . C515 C -0.0183(6) 1.005(2) 0.3244(12) 0.072(7) Uiso 1 1 d . . . H515 H -0.0234 1.0529 0.2868 0.086 Uiso 1 1 calc R . . C516 C 0.0061(5) 0.9178(17) 0.3343(10) 0.052(5) Uiso 1 1 d . . . H516 H 0.019 0.9143 0.3061 0.062 Uiso 1 1 calc R . . C521 C 0.0270(4) 0.5920(14) 0.4152(8) 0.035(4) Uiso 1 1 d . . . C522 C 0.0454(4) 0.5077(14) 0.4574(8) 0.036(4) Uiso 1 1 d . . . H522 H 0.0676 0.5242 0.4837 0.043 Uiso 1 1 calc R . . C523 C 0.0313(6) 0.400(2) 0.4607(11) 0.066(6) Uiso 1 1 d . . . H523 H 0.0448 0.3385 0.4856 0.079 Uiso 1 1 calc R . . C524 C -0.0032(5) 0.378(2) 0.4279(10) 0.061(6) Uiso 1 1 d . . . H524 H -0.0133 0.3041 0.4322 0.073 Uiso 1 1 calc R . . C525 C -0.0207(6) 0.4660(19) 0.3904(11) 0.064(6) Uiso 1 1 d . . . H525 H -0.0435 0.4516 0.3674 0.077 Uiso 1 1 calc R . . C526 C -0.0077(5) 0.5772(17) 0.3829(10) 0.051(5) Uiso 1 1 d . . . H526 H -0.0212 0.6387 0.3578 0.061 Uiso 1 1 calc R . . H1 H 0.202(4) 1.198(6) 0.232(5) 0.05 Uiso 1 1 d D . . H2 H 0.242(2) 1.080(14) 0.287(3) 0.05 Uiso 1 1 d D . . H3 H 0.2327(19) 1.229(8) 0.337(7) 0.05 Uiso 1 1 d 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 Os1 0.0259(4) 0.0313(4) 0.0200(3) 0.0040(3) 0.0123(3) 0.0026(3) Os2 0.0244(3) 0.0269(3) 0.0194(3) 0.0028(2) 0.0118(3) 0.0000(3) Os3 0.0346(4) 0.0297(4) 0.0181(3) 0.0016(3) 0.0168(3) 0.0000(3) Co4 0.0281(12) 0.0307(12) 0.0162(10) 0.0012(8) 0.0111(9) -0.0030(9) Co5 0.0300(12) 0.0377(12) 0.0160(10) -0.0025(9) 0.0151(9) -0.0071(10) Co6 0.0311(12) 0.0408(13) 0.0152(10) -0.0014(9) 0.0104(9) -0.0113(10) P4 0.033(2) 0.025(2) 0.0191(19) 0.0008(16) 0.0128(18) -0.0005(17) P5 0.031(2) 0.045(3) 0.017(2) 0.0007(18) 0.0134(18) -0.0024(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Os1 C12 1.832(16) . ? Os1 C13 1.904(16) . ? Os1 C11 1.932(17) . ? Os1 C1 2.087(15) . ? Os1 Os3 2.8826(10) . ? Os1 Os2 2.8841(9) . ? Os1 H2 1.79(7) . ? Os1 H3 1.79(7) . ? Os2 C23 1.881(17) . ? Os2 C22 1.908(17) . ? Os2 C21 1.948(17) . ? Os2 C1 2.134(14) . ? Os2 Os3 2.8896(9) . ? Os2 H1 1.82(7) . ? Os2 H3 1.70(7) . ? Os3 C32 1.892(18) . ? Os3 C33 1.911(15) . ? Os3 C31 1.959(17) . ? Os3 C1 2.122(15) . ? Os3 H1 1.84(7) . ? Os3 H2 1.73(7) . ? Co4 C42 1.757(19) . ? Co4 C41 1.800(17) . ? Co4 C5 1.891(14) . ? Co4 P4 2.199(4) . ? Co4 Co6 2.477(3) . ? Co4 Co5 2.495(3) . ? Co5 C52 1.741(18) . ? Co5 C51 1.757(19) . ? Co5 C5 1.891(15) . ? Co5 P5 2.185(5) . ? Co5 Co6 2.477(3) . ? Co6 C63 1.769(18) . ? Co6 C62 1.792(18) . ? Co6 C61 1.809(17) . ? Co6 C5 1.928(15) . ? C11 O11 1.150(18) . ? C12 O12 1.187(18) . ? C13 O13 1.163(18) . ? C21 O21 1.118(18) . ? C22 O22 1.141(19) . ? C23 O23 1.149(18) . ? C31 O31 1.128(19) . ? C32 O32 1.13(2) . ? C33 O33 1.132(17) . ? C41 O41 1.127(18) . ? C42 O42 1.15(2) . ? C51 O51 1.18(2) . ? C52 O52 1.128(19) . ? C61 O61 1.153(18) . ? C62 O62 1.121(19) . ? C63 O63 1.15(2) . ? C1 C2 1.42(2) . ? C2 C3 1.168(19) . ? C3 C4 1.44(2) . ? C4 O4 1.227(17) . ? C4 C5 1.48(2) . ? P4 C411 1.815(16) . ? P4 C0 1.829(14) . ? P4 C421 1.852(17) . ? C411 C412 1.36(2) . ? C411 C416 1.36(2) . ? C412 C413 1.44(3) . ? C412 H412 0.95 . ? C413 C414 1.38(3) . ? C413 H413 0.95 . ? C414 C415 1.27(3) . ? C414 H414 0.95 . ? C415 C416 1.39(3) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C426 1.35(2) . ? C421 C422 1.38(3) . ? C422 C423 1.42(4) . ? C422 H422 0.95 . ? C423 C424 1.38(4) . ? C423 H423 0.95 . ? C424 C425 1.33(3) . ? C424 H424 0.95 . ? C425 C426 1.39(2) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C0 P5 1.816(14) . ? C0 H0A 0.99 . ? C0 H0B 0.99 . ? P5 C521 1.828(17) . ? P5 C511 1.840(19) . ? C511 C516 1.32(2) . ? C511 C512 1.38(3) . ? C512 C513 1.46(3) . ? C512 H512 0.95 . ? C513 C514 1.32(3) . ? C513 H513 0.95 . ? C514 C515 1.36(3) . ? C514 H514 0.95 . ? C515 C516 1.39(3) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C522 1.38(2) . ? C521 C526 1.42(2) . ? C522 C523 1.36(3) . ? C522 H522 0.95 . ? C523 C524 1.43(3) . ? C523 H523 0.95 . ? C524 C525 1.35(3) . ? C524 H524 0.95 . ? C525 C526 1.40(3) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? 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 C12 Os1 C13 90.0(7) . . ? C12 Os1 C11 95.3(7) . . ? C13 Os1 C11 97.9(7) . . ? C12 Os1 C1 99.1(6) . . ? C13 Os1 C1 94.5(6) . . ? C11 Os1 C1 161.0(6) . . ? C12 Os1 Os3 94.4(5) . . ? C13 Os1 Os3 141.8(5) . . ? C11 Os1 Os3 119.4(5) . . ? C1 Os1 Os3 47.3(4) . . ? C12 Os1 Os2 146.2(5) . . ? C13 Os1 Os2 97.5(5) . . ? C11 Os1 Os2 116.0(5) . . ? C1 Os1 Os2 47.6(4) . . ? Os3 Os1 Os2 60.14(2) . . ? C12 Os1 H2 97(5) . . ? C13 Os1 H2 172(5) . . ? C11 Os1 H2 85(3) . . ? C1 Os1 H2 81(3) . . ? Os3 Os1 H2 34(3) . . ? Os2 Os1 H2 75(5) . . ? C12 Os1 H3 169(5) . . ? C13 Os1 H3 101(5) . . ? C11 Os1 H3 83(3) . . ? C1 Os1 H3 81(3) . . ? Os3 Os1 H3 77(5) . . ? Os2 Os1 H3 33(3) . . ? H2 Os1 H3 73(7) . . ? C23 Os2 C22 92.8(7) . . ? C23 Os2 C21 96.4(7) . . ? C22 Os2 C21 96.0(7) . . ? C23 Os2 C1 97.2(6) . . ? C22 Os2 C1 92.8(6) . . ? C21 Os2 C1 163.3(6) . . ? C23 Os2 Os1 93.7(5) . . ? C22 Os2 Os1 139.1(5) . . ? C21 Os2 Os1 123.3(5) . . ? C1 Os2 Os1 46.2(4) . . ? C23 Os2 Os3 144.0(5) . . ? C22 Os2 Os3 93.3(5) . . ? C21 Os2 Os3 118.1(5) . . ? C1 Os2 Os3 47.1(4) . . ? Os1 Os2 Os3 59.90(2) . . ? C23 Os2 H1 173(5) . . ? C22 Os2 H1 93(5) . . ? C21 Os2 H1 80(3) . . ? C1 Os2 H1 85(2) . . ? Os1 Os2 H1 83(4) . . ? Os3 Os2 H1 38(2) . . ? C23 Os2 H3 94(6) . . ? C22 Os2 H3 172(5) . . ? C21 Os2 H3 88(3) . . ? C1 Os2 H3 81(3) . . ? Os1 Os2 H3 35(3) . . ? Os3 Os2 H3 78(5) . . ? H1 Os2 H3 80(7) . . ? C32 Os3 C33 91.0(7) . . ? C32 Os3 C31 93.7(7) . . ? C33 Os3 C31 95.0(7) . . ? C32 Os3 C1 96.2(7) . . ? C33 Os3 C1 96.8(6) . . ? C31 Os3 C1 164.5(6) . . ? C32 Os3 Os1 95.3(5) . . ? C33 Os3 Os1 142.9(4) . . ? C31 Os3 Os1 120.9(5) . . ? C1 Os3 Os1 46.3(4) . . ? C32 Os3 Os2 143.5(5) . . ? C33 Os3 Os2 94.8(4) . . ? C31 Os3 Os2 121.5(5) . . ? C1 Os3 Os2 47.4(4) . . ? Os1 Os3 Os2 59.95(2) . . ? C32 Os3 H1 177(5) . . ? C33 Os3 H1 92(5) . . ? C31 Os3 H1 85(3) . . ? C1 Os3 H1 85(2) . . ? Os1 Os3 H1 83(4) . . ? Os2 Os3 H1 38(2) . . ? C32 Os3 H2 100(5) . . ? C33 Os3 H2 169(5) . . ? C31 Os3 H2 85(3) . . ? C1 Os3 H2 81(3) . . ? Os1 Os3 H2 36(3) . . ? Os2 Os3 H2 76(5) . . ? H1 Os3 H2 77(7) . . ? C42 Co4 C41 102.9(8) . . ? C42 Co4 C5 109.9(7) . . ? C41 Co4 C5 137.1(7) . . ? C42 Co4 P4 94.3(6) . . ? C41 Co4 P4 106.5(5) . . ? C5 Co4 P4 98.0(5) . . ? C42 Co4 Co6 100.5(6) . . ? C41 Co4 Co6 97.7(5) . . ? C5 Co4 Co6 50.2(4) . . ? P4 Co4 Co6 147.92(15) . . ? C42 Co4 Co5 156.8(6) . . ? C41 Co4 Co5 92.6(5) . . ? C5 Co4 Co5 48.7(5) . . ? P4 Co4 Co5 97.78(14) . . ? Co6 Co4 Co5 59.77(8) . . ? C52 Co5 C51 102.5(8) . . ? C52 Co5 C5 92.5(7) . . ? C51 Co5 C5 150.1(8) . . ? C52 Co5 P5 97.7(6) . . ? C51 Co5 P5 99.7(6) . . ? C5 Co5 P5 103.9(5) . . ? C52 Co5 Co6 96.6(6) . . ? C51 Co5 Co6 101.8(6) . . ? C5 Co5 Co6 50.2(4) . . ? P5 Co5 Co6 150.91(15) . . ? C52 Co5 Co4 141.2(6) . . ? C51 Co5 Co4 111.8(6) . . ? C5 Co5 Co4 48.7(4) . . ? P5 Co5 Co4 94.02(14) . . ? Co6 Co5 Co4 59.74(8) . . ? C63 Co6 C62 95.7(8) . . ? C63 Co6 C61 109.4(8) . . ? C62 Co6 C61 105.3(8) . . ? C63 Co6 C5 98.8(7) . . ? C62 Co6 C5 105.0(7) . . ? C61 Co6 C5 135.8(7) . . ? C63 Co6 Co4 147.8(6) . . ? C62 Co6 Co4 94.6(5) . . ? C61 Co6 Co4 97.2(5) . . ? C5 Co6 Co4 48.9(4) . . ? C63 Co6 Co5 99.5(6) . . ? C62 Co6 Co5 151.5(6) . . ? C61 Co6 Co5 92.3(5) . . ? C5 Co6 Co5 48.9(4) . . ? Co4 Co6 Co5 60.48(8) . . ? O11 C11 Os1 176.7(15) . . ? O12 C12 Os1 177.2(16) . . ? O13 C13 Os1 177.7(15) . . ? O21 C21 Os2 176.3(15) . . ? O22 C22 Os2 177.1(15) . . ? O23 C23 Os2 177.6(15) . . ? O31 C31 Os3 178.4(15) . . ? O32 C32 Os3 176.7(16) . . ? O33 C33 Os3 175.3(14) . . ? O41 C41 Co4 175.2(16) . . ? O42 C42 Co4 178.5(18) . . ? O51 C51 Co5 176.9(17) . . ? O52 C52 Co5 176.8(18) . . ? O61 C61 Co6 179.5(16) . . ? O62 C62 Co6 175.5(16) . . ? O63 C63 Co6 176.9(18) . . ? C2 C1 Os1 136.0(11) . . ? C2 C1 Os3 125.0(11) . . ? Os1 C1 Os3 86.4(6) . . ? C2 C1 Os2 122.4(11) . . ? Os1 C1 Os2 86.2(5) . . ? Os3 C1 Os2 85.5(6) . . ? C3 C2 C1 174.9(17) . . ? C2 C3 C4 174.9(16) . . ? O4 C4 C3 121.5(13) . . ? O4 C4 C5 121.8(13) . . ? C3 C4 C5 116.7(13) . . ? C4 C5 Co5 133.7(11) . . ? C4 C5 Co4 129.8(11) . . ? Co5 C5 Co4 82.5(6) . . ? C4 C5 Co6 129.8(11) . . ? Co5 C5 Co6 80.9(6) . . ? # Attachment '7.br1414.cif' data_br1414 _database_code_depnum_ccdc_archive 'CCDC 754939' #TrackingRef '7.br1414.cif' _audit_creation_date 2008-05-07T12:17:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C72 H44 Co6 O16 P4' _chemical_formula_moiety 'C72 H44 Co6 O16 P4' _chemical_formula_weight 1642.53 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.1850(8) _cell_length_b 13.2858(3) _cell_length_c 20.4563(6) _cell_angle_alpha 90 _cell_angle_beta 102.523(3) _cell_angle_gamma 90 _cell_volume 6947.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8658 _cell_measurement_theta_min 2.5291 _cell_measurement_theta_max 29.8858 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description slab _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90685 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0218471784 _diffrn_orient_matrix_ub_12 -0.0331620297 _diffrn_orient_matrix_ub_13 -0.0168961883 _diffrn_orient_matrix_ub_21 0.0279120127 _diffrn_orient_matrix_ub_22 -0.0231205703 _diffrn_orient_matrix_ub_23 -0.007217878 _diffrn_orient_matrix_ub_31 0.0022410484 _diffrn_orient_matrix_ub_32 -0.0348873087 _diffrn_orient_matrix_ub_33 0.0208020221 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_unetI/netI 0.2045 _diffrn_reflns_number 63161 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 15957 _reflns_number_gt 7185 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0626P)^2^+0.0000P] 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_number_reflns 15957 _refine_ls_number_parameters 877 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1667 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.151 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.11640(3) 0.18290(6) 0.54914(4) 0.0175(2) Uani 1 1 d . . . Co2 Co 0.10200(3) 0.36199(6) 0.51661(4) 0.0179(2) Uani 1 1 d . . . Co3 Co 0.15844(3) 0.31700(6) 0.62665(4) 0.0236(2) Uani 1 1 d . . . Co4 Co 0.39588(4) 0.74966(7) 0.59702(5) 0.0263(2) Uani 1 1 d . . . Co5 Co 0.41638(3) 0.85865(7) 0.50769(5) 0.0264(2) Uani 1 1 d . . . Co6 Co 0.43029(4) 0.67286(7) 0.50475(5) 0.0311(3) Uani 1 1 d . . . C11 C 0.0629(3) 0.1554(4) 0.5885(3) 0.0209(15) Uani 1 1 d . . . O11 O 0.03046(18) 0.1437(3) 0.6176(2) 0.0318(12) Uani 1 1 d . . . C12 C 0.1601(3) 0.0799(5) 0.5745(3) 0.0215(15) Uani 1 1 d . . . O12 O 0.18816(18) 0.0145(3) 0.5911(2) 0.0337(12) Uani 1 1 d . . . C21 C 0.0384(3) 0.3643(5) 0.5373(3) 0.0243(16) Uani 1 1 d . . . O21 O -0.00120(18) 0.3668(3) 0.5524(2) 0.0320(12) Uani 1 1 d . . . C22 C 0.1192(2) 0.4918(5) 0.5194(3) 0.0243(16) Uani 1 1 d . . . O22 O 0.13084(19) 0.5744(3) 0.5213(2) 0.0359(13) Uani 1 1 d . . . C31 C 0.1092(3) 0.3374(5) 0.6758(3) 0.0286(17) Uani 1 1 d . . . O31 O 0.0782(2) 0.3473(4) 0.7064(3) 0.0444(14) Uani 1 1 d . . . C32 C 0.2015(3) 0.2280(5) 0.6762(4) 0.041(2) Uani 1 1 d . . . O32 O 0.2295(2) 0.1705(4) 0.7064(3) 0.068(2) Uani 1 1 d . . . C33 C 0.1994(3) 0.4261(5) 0.6429(3) 0.0321(18) Uani 1 1 d . . . O33 O 0.2269(2) 0.4935(4) 0.6550(3) 0.0473(15) Uani 1 1 d . . . C41 C 0.4555(3) 0.7611(5) 0.6585(4) 0.0375(19) Uani 1 1 d . . . O41 O 0.4951(2) 0.7627(4) 0.6965(3) 0.0507(15) Uani 1 1 d . . . C42 C 0.3682(3) 0.6429(5) 0.6299(4) 0.0356(19) Uani 1 1 d . . . O42 O 0.3505(2) 0.5744(4) 0.6502(3) 0.0521(15) Uani 1 1 d . . . C51 C 0.4812(3) 0.8958(5) 0.5514(4) 0.039(2) Uani 1 1 d . . . O51 O 0.5220(2) 0.9154(4) 0.5807(3) 0.0499(16) Uani 1 1 d . . . C52 C 0.4176(3) 0.8770(6) 0.4233(4) 0.038(2) Uani 1 1 d . . . O52 O 0.4189(2) 0.8847(5) 0.3673(3) 0.0596(17) Uani 1 1 d . . . C61 C 0.5003(3) 0.6808(5) 0.5333(4) 0.0363(19) Uani 1 1 d . . . O61 O 0.5451(2) 0.6855(4) 0.5519(3) 0.0514(15) Uani 1 1 d . . . C62 C 0.4175(3) 0.5476(7) 0.5288(4) 0.050(2) Uani 1 1 d . . . O62 O 0.4103(3) 0.4671(4) 0.5434(4) 0.077(2) Uani 1 1 d . . . C63 C 0.4232(3) 0.6466(6) 0.4174(4) 0.0459(12) Uani 1 1 d . . . O63 O 0.4116(2) 0.6429(4) 0.3597(3) 0.0459(12) Uani 1 1 d . . . C1 C 0.1635(2) 0.2843(4) 0.5369(3) 0.0167(14) Uani 1 1 d . . . C2 C 0.2141(3) 0.2783(5) 0.5163(3) 0.0276(17) Uani 1 1 d . . . O2 O 0.23395(17) 0.2001(3) 0.5036(3) 0.0379(13) Uani 1 1 d . . . C3 C 0.2396(2) 0.3748(6) 0.5114(3) 0.0281(17) Uani 1 1 d . . . C4 C 0.2583(3) 0.4550(5) 0.5023(4) 0.0308(18) Uani 1 1 d . . . C5 C 0.2794(3) 0.5450(6) 0.4913(4) 0.0349(19) Uani 1 1 d . . . C6 C 0.2978(3) 0.6248(6) 0.4804(4) 0.0364(19) Uani 1 1 d . . . C7 C 0.3182(3) 0.7175(5) 0.4604(4) 0.0287(18) Uani 1 1 d . . . O7 O 0.29329(17) 0.7640(3) 0.4144(2) 0.0314(12) Uani 1 1 d . . . C8 C 0.3673(3) 0.7554(6) 0.5050(3) 0.0344(19) Uani 1 1 d . . . P1 P 0.09184(6) 0.13050(12) 0.44573(8) 0.0163(4) Uani 1 1 d . . . C111 C 0.1209(2) 0.0108(4) 0.4288(3) 0.0192(15) Uani 1 1 d . . . C112 C 0.1702(3) 0.0043(5) 0.4155(3) 0.0309(18) Uani 1 1 d . . . H112 H 0.1884 0.064 0.4089 0.037 Uiso 1 1 calc R . . C113 C 0.1934(3) -0.0898(5) 0.4117(4) 0.0361(19) Uani 1 1 d . . . H113 H 0.2271 -0.0941 0.4016 0.043 Uiso 1 1 calc R . . C114 C 0.1677(3) -0.1749(5) 0.4225(3) 0.0321(18) Uani 1 1 d . . . H114 H 0.1837 -0.2386 0.4202 0.038 Uiso 1 1 calc R . . C115 C 0.1189(3) -0.1701(5) 0.4365(3) 0.0313(18) Uani 1 1 d . . . H115 H 0.1016 -0.2302 0.4444 0.038 Uiso 1 1 calc R . . C116 C 0.0950(2) -0.0787(5) 0.4391(3) 0.0230(16) Uani 1 1 d . . . H116 H 0.0608 -0.0759 0.4479 0.028 Uiso 1 1 calc R . . C121 C 0.0229(2) 0.1142(4) 0.4059(3) 0.0182(15) Uani 1 1 d . . . C122 C 0.0098(3) 0.0780(4) 0.3412(3) 0.0224(15) Uani 1 1 d . . . H122 H 0.0368 0.059 0.3192 0.027 Uiso 1 1 calc R . . C123 C -0.0418(3) 0.0687(5) 0.3078(3) 0.0287(17) Uani 1 1 d . . . H123 H -0.0503 0.044 0.2632 0.034 Uiso 1 1 calc R . . C124 C -0.0806(3) 0.0954(5) 0.3397(4) 0.0277(17) Uani 1 1 d . . . H124 H -0.1162 0.0902 0.3167 0.033 Uiso 1 1 calc R . . C125 C -0.0689(2) 0.1297(5) 0.4044(4) 0.0259(16) Uani 1 1 d . . . H125 H -0.0961 0.1462 0.4266 0.031 Uiso 1 1 calc R . . C126 C -0.0165(2) 0.1401(4) 0.4376(3) 0.0207(15) Uani 1 1 d . . . H126 H -0.0082 0.1652 0.4822 0.025 Uiso 1 1 calc R . . C01 C 0.1128(2) 0.2188(4) 0.3888(3) 0.0161(14) Uani 1 1 d . . . H01A H 0.0974 0.2004 0.3418 0.019 Uiso 1 1 calc R . . H01B H 0.1514 0.2176 0.3953 0.019 Uiso 1 1 calc R . . P2 P 0.09082(6) 0.34450(11) 0.40724(8) 0.0170(4) Uani 1 1 d . . . C211 C 0.1302(3) 0.4302(5) 0.3680(3) 0.0216(15) Uani 1 1 d . . . C212 C 0.1763(3) 0.4032(5) 0.3509(4) 0.0354(19) Uani 1 1 d . . . H212 H 0.1881 0.3354 0.356 0.043 Uiso 1 1 calc R . . C213 C 0.2056(3) 0.4751(6) 0.3261(4) 0.050(2) Uani 1 1 d . . . H213 H 0.2378 0.4569 0.315 0.06 Uiso 1 1 calc R . . C214 C 0.1879(3) 0.5724(6) 0.3178(4) 0.045(2) Uani 1 1 d . . . H214 H 0.2081 0.6213 0.3008 0.054 Uiso 1 1 calc R . . C215 C 0.1421(3) 0.6000(5) 0.3335(3) 0.038(2) Uani 1 1 d . . . H215 H 0.13 0.6674 0.3265 0.046 Uiso 1 1 calc R . . C216 C 0.1128(3) 0.5288(5) 0.3597(3) 0.0272(17) Uani 1 1 d . . . H216 H 0.0812 0.5478 0.3719 0.033 Uiso 1 1 calc R . . C221 C 0.0258(2) 0.3580(4) 0.3510(3) 0.0179(14) Uani 1 1 d . . . C222 C 0.0195(2) 0.3364(4) 0.2841(3) 0.0214(15) Uani 1 1 d . . . H222 H 0.0486 0.3149 0.267 0.026 Uiso 1 1 calc R . . C223 C -0.0291(2) 0.3459(4) 0.2412(3) 0.0224(15) Uani 1 1 d . . . H223 H -0.0332 0.3292 0.1952 0.027 Uiso 1 1 calc R . . C224 C -0.0716(3) 0.3796(5) 0.2651(3) 0.0246(16) Uani 1 1 d . . . H224 H -0.1049 0.3868 0.2356 0.03 Uiso 1 1 calc R . . C225 C -0.0652(3) 0.4022(5) 0.3314(4) 0.0322(18) Uani 1 1 d . . . H225 H -0.0942 0.426 0.3481 0.039 Uiso 1 1 calc R . . C226 C -0.0169(3) 0.3909(5) 0.3747(3) 0.0268(16) Uani 1 1 d . . . H226 H -0.0131 0.4058 0.4209 0.032 Uiso 1 1 calc R . . P4 P 0.34228(7) 0.85992(13) 0.62584(9) 0.0245(4) Uani 1 1 d . . . C411 C 0.2876(3) 0.8032(5) 0.6538(3) 0.0248(16) Uani 1 1 d . . . C412 C 0.2389(3) 0.7868(5) 0.6106(4) 0.0328(18) Uani 1 1 d . . . H412 H 0.2331 0.8075 0.5652 0.039 Uiso 1 1 calc R . . C413 C 0.1993(3) 0.7401(5) 0.6349(4) 0.0343(19) Uani 1 1 d . . . H413 H 0.1662 0.7296 0.6058 0.041 Uiso 1 1 calc R . . C414 C 0.2074(3) 0.7089(5) 0.7006(4) 0.036(2) Uani 1 1 d . . . H414 H 0.1802 0.6766 0.7167 0.044 Uiso 1 1 calc R . . C415 C 0.2556(3) 0.7253(5) 0.7429(4) 0.0373(19) Uani 1 1 d . . . H415 H 0.2607 0.7056 0.7885 0.045 Uiso 1 1 calc R . . C416 C 0.2957(3) 0.7688(5) 0.7209(3) 0.0350(18) Uani 1 1 d . . . H416 H 0.329 0.7762 0.7502 0.042 Uiso 1 1 calc R . . C421 C 0.3660(3) 0.9506(5) 0.6925(3) 0.0248(16) Uani 1 1 d . . . C422 C 0.3298(3) 1.0033(5) 0.7221(4) 0.0328(18) Uani 1 1 d . . . H422 H 0.2936 0.9879 0.7091 0.039 Uiso 1 1 calc R . . C423 C 0.3466(3) 1.0766(5) 0.7695(4) 0.048(2) Uani 1 1 d . . . H423 H 0.3222 1.1112 0.7896 0.058 Uiso 1 1 calc R . . C424 C 0.3997(3) 1.0993(5) 0.7876(4) 0.042(2) Uani 1 1 d . . . H424 H 0.4115 1.1509 0.8194 0.051 Uiso 1 1 calc R . . C425 C 0.4354(3) 1.0479(5) 0.7598(4) 0.041(2) Uani 1 1 d . . . H425 H 0.4716 1.062 0.774 0.049 Uiso 1 1 calc R . . C426 C 0.4186(3) 0.9760(5) 0.7111(4) 0.0317(18) Uani 1 1 d . . . H426 H 0.4432 0.9436 0.6903 0.038 Uiso 1 1 calc R . . C02 C 0.3128(2) 0.9411(5) 0.5541(3) 0.0267(16) Uani 1 1 d . . . H02A H 0.2881 0.9017 0.5202 0.032 Uiso 1 1 calc R . . H02B H 0.2935 0.9974 0.5693 0.032 Uiso 1 1 calc R . . P5 P 0.36567(7) 0.98963(13) 0.51815(10) 0.0283(5) Uani 1 1 d . . . C511 C 0.3338(3) 1.0529(6) 0.4407(4) 0.0369(19) Uani 1 1 d . . . C512 C 0.3145(3) 0.9960(6) 0.3837(4) 0.049(2) Uani 1 1 d . . . H512 H 0.3172 0.9248 0.3868 0.059 Uiso 1 1 calc R . . C513 C 0.2915(4) 1.0383(7) 0.3231(5) 0.083(4) Uani 1 1 d . . . H513 H 0.2776 0.9972 0.2855 0.099 Uiso 1 1 calc R . . C514 C 0.2894(4) 1.1426(8) 0.3184(5) 0.089(4) Uani 1 1 d . . . H514 H 0.2737 1.1741 0.2772 0.106 Uiso 1 1 calc R . . C515 C 0.3103(4) 1.2008(7) 0.3745(5) 0.073(3) Uani 1 1 d . . . H515 H 0.3096 1.2721 0.371 0.088 Uiso 1 1 calc R . . C516 C 0.3320(4) 1.1564(6) 0.4352(4) 0.055(2) Uani 1 1 d . . . H516 H 0.3457 1.197 0.4732 0.066 Uiso 1 1 calc R . . C521 C 0.3903(3) 1.0983(5) 0.5717(4) 0.0349(19) Uani 1 1 d . . . C522 C 0.3559(3) 1.1586(5) 0.5988(4) 0.037(2) Uani 1 1 d . . . H522 H 0.3201 1.1403 0.5923 0.044 Uiso 1 1 calc R . . C523 C 0.3738(3) 1.2441(5) 0.6348(4) 0.046(2) Uani 1 1 d . . . H523 H 0.3503 1.2856 0.652 0.055 Uiso 1 1 calc R . . C524 C 0.4259(3) 1.2688(5) 0.6455(4) 0.046(2) Uani 1 1 d . . . H524 H 0.4383 1.3269 0.6711 0.055 Uiso 1 1 calc R . . C525 C 0.4596(3) 1.2120(6) 0.6203(4) 0.049(2) Uani 1 1 d . . . H525 H 0.4955 1.2301 0.628 0.059 Uiso 1 1 calc R . . C526 C 0.4418(3) 1.1272(5) 0.5832(4) 0.041(2) Uani 1 1 d . . . H526 H 0.4658 1.0879 0.5653 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0198(5) 0.0187(5) 0.0140(5) 0.0015(4) 0.0035(4) -0.0029(4) Co2 0.0241(5) 0.0177(5) 0.0119(5) -0.0009(4) 0.0043(4) -0.0018(4) Co3 0.0321(6) 0.0227(5) 0.0136(5) 0.0001(4) -0.0005(4) -0.0042(4) Co4 0.0304(6) 0.0258(5) 0.0225(5) 0.0023(4) 0.0055(4) 0.0024(4) Co5 0.0273(5) 0.0274(5) 0.0231(5) 0.0035(4) 0.0026(4) -0.0044(4) Co6 0.0343(6) 0.0306(6) 0.0310(6) -0.0059(5) 0.0130(5) -0.0011(5) C11 0.024(4) 0.020(4) 0.017(4) 0.001(3) 0.001(3) -0.005(3) O11 0.038(3) 0.036(3) 0.024(3) 0.002(2) 0.014(2) -0.008(2) C12 0.023(4) 0.019(4) 0.021(4) 0.002(3) 0.001(3) -0.006(3) O12 0.032(3) 0.027(3) 0.037(3) 0.007(2) -0.003(2) 0.009(2) C21 0.036(4) 0.020(4) 0.013(4) -0.003(3) -0.003(3) -0.001(3) O21 0.031(3) 0.039(3) 0.030(3) -0.001(2) 0.015(2) 0.008(2) C22 0.027(4) 0.041(5) 0.003(3) -0.001(3) 0.000(3) -0.001(3) O22 0.061(4) 0.016(3) 0.026(3) -0.002(2) 0.001(3) -0.007(2) C31 0.041(5) 0.027(4) 0.014(4) 0.003(3) 0.000(3) -0.007(3) O31 0.071(4) 0.043(3) 0.029(3) -0.004(3) 0.031(3) -0.003(3) C32 0.055(6) 0.028(4) 0.033(5) -0.008(4) -0.005(4) -0.001(4) O32 0.091(5) 0.035(3) 0.055(4) 0.005(3) -0.036(4) 0.017(3) C33 0.046(5) 0.030(4) 0.020(4) 0.007(3) 0.005(4) 0.010(4) O33 0.060(4) 0.040(3) 0.035(3) -0.005(3) -0.005(3) -0.023(3) C41 0.044(5) 0.032(4) 0.036(5) 0.004(4) 0.008(4) 0.010(4) O41 0.044(4) 0.057(4) 0.043(4) -0.004(3) -0.008(3) 0.013(3) C42 0.040(5) 0.027(4) 0.048(5) 0.017(4) 0.028(4) 0.015(4) O42 0.066(4) 0.043(3) 0.053(4) 0.007(3) 0.025(3) -0.005(3) C51 0.051(6) 0.022(4) 0.038(5) 0.006(4) -0.003(4) -0.004(4) O51 0.031(3) 0.037(3) 0.070(4) 0.008(3) -0.016(3) -0.005(3) C52 0.033(5) 0.051(5) 0.031(5) 0.014(4) 0.006(4) -0.004(4) O52 0.057(4) 0.094(5) 0.028(4) -0.002(3) 0.008(3) -0.008(3) C61 0.053(6) 0.032(4) 0.028(4) 0.000(4) 0.017(4) 0.013(4) O61 0.033(3) 0.072(4) 0.045(4) -0.009(3) -0.001(3) 0.009(3) C62 0.051(6) 0.050(6) 0.056(6) -0.007(5) 0.025(5) 0.016(5) O62 0.110(6) 0.024(3) 0.116(6) 0.006(4) 0.065(5) 0.005(3) C63 0.057(3) 0.050(3) 0.038(3) -0.023(3) 0.025(3) -0.020(2) O63 0.057(3) 0.050(3) 0.038(3) -0.023(3) 0.025(3) -0.020(2) C1 0.019(4) 0.019(3) 0.011(3) 0.005(3) 0.000(3) -0.008(3) C2 0.034(5) 0.029(4) 0.017(4) -0.002(3) -0.001(3) -0.006(3) O2 0.021(3) 0.033(3) 0.063(4) -0.013(3) 0.017(3) -0.004(2) C3 0.015(4) 0.046(5) 0.024(4) -0.001(4) 0.004(3) -0.004(3) C4 0.022(4) 0.036(4) 0.037(5) -0.004(4) 0.009(3) -0.010(3) C5 0.025(4) 0.044(5) 0.035(5) -0.003(4) 0.008(4) -0.006(4) C6 0.028(4) 0.047(5) 0.033(5) -0.003(4) 0.005(3) -0.010(4) C7 0.017(4) 0.030(4) 0.042(5) 0.015(4) 0.013(4) 0.002(3) O7 0.029(3) 0.024(3) 0.038(3) 0.003(2) 0.001(2) -0.007(2) C8 0.020(4) 0.074(5) 0.007(3) 0.009(4) -0.002(3) -0.021(4) P1 0.0184(9) 0.0159(8) 0.0146(9) -0.0001(7) 0.0037(7) -0.0007(7) C111 0.019(4) 0.020(3) 0.018(4) 0.001(3) 0.002(3) 0.007(3) C112 0.024(4) 0.035(4) 0.031(5) -0.004(3) 0.001(3) 0.000(3) C113 0.023(4) 0.041(5) 0.040(5) -0.011(4) -0.002(4) 0.005(4) C114 0.027(4) 0.032(4) 0.028(4) -0.010(3) -0.014(3) 0.017(4) C115 0.038(5) 0.015(4) 0.034(4) 0.006(3) -0.008(4) 0.002(3) C116 0.023(4) 0.026(4) 0.022(4) -0.005(3) 0.006(3) 0.000(3) C121 0.026(4) 0.011(3) 0.020(4) 0.001(3) 0.010(3) -0.001(3) C122 0.027(4) 0.016(3) 0.024(4) -0.001(3) 0.004(3) -0.002(3) C123 0.036(5) 0.025(4) 0.021(4) -0.003(3) -0.004(3) -0.005(3) C124 0.021(4) 0.025(4) 0.032(4) 0.006(3) -0.004(3) 0.001(3) C125 0.016(4) 0.027(4) 0.036(4) 0.002(3) 0.007(3) 0.007(3) C126 0.027(4) 0.019(3) 0.016(4) -0.004(3) 0.004(3) -0.002(3) C01 0.016(4) 0.021(3) 0.013(3) 0.004(3) 0.008(3) 0.001(3) P2 0.0212(9) 0.0177(9) 0.0133(9) -0.0007(7) 0.0063(7) -0.0039(7) C211 0.032(4) 0.022(4) 0.013(4) -0.002(3) 0.009(3) -0.007(3) C212 0.050(5) 0.029(4) 0.032(5) -0.009(4) 0.020(4) -0.014(4) C213 0.046(5) 0.055(6) 0.055(6) -0.004(5) 0.025(5) -0.027(4) C214 0.060(6) 0.041(5) 0.034(5) 0.002(4) 0.011(4) -0.033(5) C215 0.065(6) 0.026(4) 0.015(4) 0.005(3) -0.012(4) -0.019(4) C216 0.039(4) 0.028(4) 0.010(4) 0.005(3) -0.004(3) -0.005(3) C221 0.024(4) 0.015(3) 0.015(3) 0.001(3) 0.006(3) 0.002(3) C222 0.020(4) 0.026(4) 0.020(4) -0.001(3) 0.006(3) 0.002(3) C223 0.031(4) 0.027(4) 0.010(3) 0.004(3) 0.007(3) -0.002(3) C224 0.028(4) 0.028(4) 0.016(4) 0.003(3) 0.001(3) -0.004(3) C225 0.028(4) 0.040(4) 0.028(4) -0.001(4) 0.005(3) 0.014(3) C226 0.035(4) 0.031(4) 0.015(4) 0.002(3) 0.007(3) 0.007(3) P4 0.0273(10) 0.0261(10) 0.0202(10) 0.0020(8) 0.0053(8) 0.0001(8) C411 0.025(4) 0.025(4) 0.025(4) -0.004(3) 0.009(3) -0.002(3) C412 0.039(5) 0.028(4) 0.031(5) -0.008(3) 0.007(4) 0.000(3) C413 0.018(4) 0.030(4) 0.052(5) 0.004(4) -0.001(4) -0.005(3) C414 0.037(5) 0.021(4) 0.058(6) -0.004(4) 0.025(4) -0.004(3) C415 0.050(5) 0.033(4) 0.033(5) -0.006(4) 0.016(4) -0.001(4) C416 0.044(5) 0.047(5) 0.015(4) -0.005(3) 0.008(4) -0.003(4) C421 0.027(4) 0.030(4) 0.018(4) 0.004(3) 0.005(3) -0.002(3) C422 0.027(4) 0.030(4) 0.040(5) -0.010(4) 0.005(4) -0.006(3) C423 0.050(6) 0.042(5) 0.053(6) -0.025(4) 0.012(4) 0.006(4) C424 0.050(6) 0.037(5) 0.037(5) -0.015(4) 0.003(4) -0.015(4) C425 0.045(5) 0.039(5) 0.033(5) -0.008(4) -0.006(4) -0.012(4) C426 0.028(4) 0.033(4) 0.033(5) 0.001(4) 0.005(3) -0.006(3) C02 0.025(4) 0.027(4) 0.028(4) 0.000(3) 0.004(3) 0.006(3) P5 0.0321(11) 0.0265(10) 0.0263(11) 0.0072(8) 0.0062(9) -0.0003(9) C511 0.032(5) 0.037(5) 0.042(5) 0.014(4) 0.008(4) -0.002(4) C512 0.045(5) 0.041(5) 0.051(6) 0.027(4) -0.013(4) -0.016(4) C513 0.082(8) 0.073(7) 0.072(8) 0.044(6) -0.030(6) -0.023(6) C514 0.091(8) 0.084(8) 0.065(8) 0.042(7) -0.040(6) -0.022(7) C515 0.090(8) 0.056(6) 0.072(8) 0.041(6) 0.012(6) 0.005(6) C516 0.095(7) 0.032(5) 0.040(5) 0.015(4) 0.017(5) 0.005(5) C521 0.043(5) 0.023(4) 0.038(5) 0.005(3) 0.008(4) -0.002(4) C522 0.032(5) 0.025(4) 0.052(5) -0.001(4) 0.004(4) -0.002(3) C523 0.057(6) 0.026(4) 0.058(6) 0.000(4) 0.019(5) 0.012(4) C524 0.058(6) 0.023(4) 0.056(6) 0.000(4) 0.012(5) -0.011(4) C525 0.054(6) 0.032(5) 0.066(7) -0.010(4) 0.022(5) -0.017(4) C526 0.043(5) 0.032(4) 0.055(6) -0.005(4) 0.025(4) -0.004(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.786(7) . ? Co1 C11 1.800(7) . ? Co1 C1 1.879(6) . ? Co1 P1 2.1870(18) . ? Co1 Co2 2.4773(11) . ? Co1 Co3 2.4785(12) . ? Co2 C22 1.781(7) . ? Co2 C21 1.807(8) . ? Co2 C1 1.881(6) . ? Co2 P2 2.2048(18) . ? Co2 Co3 2.4829(12) . ? Co3 C32 1.790(8) . ? Co3 C33 1.792(8) . ? Co3 C31 1.817(8) . ? Co3 C1 1.919(6) . ? Co4 C41 1.787(8) . ? Co4 C42 1.789(8) . ? Co4 C8 1.871(6) . ? Co4 P4 2.196(2) . ? Co4 Co5 2.4799(13) . ? Co4 Co6 2.4806(13) . ? Co5 C52 1.751(8) . ? Co5 C51 1.807(8) . ? Co5 C8 1.871(7) . ? Co5 P5 2.227(2) . ? Co5 Co6 2.4976(13) . ? Co6 C62 1.789(9) . ? Co6 C63 1.789(8) . ? Co6 C61 1.801(9) . ? Co6 C8 1.981(8) . ? C11 O11 1.146(7) . ? C12 O12 1.142(7) . ? C21 O21 1.143(7) . ? C22 O22 1.137(7) . ? C31 O31 1.135(8) . ? C32 O32 1.142(8) . ? C33 O33 1.142(8) . ? C41 O41 1.153(8) . ? C42 O42 1.140(8) . ? C51 O51 1.135(8) . ? C52 O52 1.158(8) . ? C61 O61 1.155(8) . ? C62 O62 1.137(9) . ? C63 O63 1.156(9) . ? C1 C2 1.478(9) . ? C2 O2 1.215(7) . ? C2 C3 1.458(9) . ? C3 C4 1.203(9) . ? C4 C5 1.357(10) . ? C5 C6 1.206(9) . ? C6 C7 1.436(10) . ? C7 O7 1.195(7) . ? C7 C8 1.494(9) . ? P1 C01 1.820(6) . ? P1 C121 1.825(6) . ? P1 C111 1.828(6) . ? C111 C112 1.378(9) . ? C111 C116 1.408(8) . ? C112 C113 1.400(9) . ? C112 H112 0.95 . ? C113 C114 1.359(9) . ? C113 H113 0.95 . ? C114 C115 1.369(10) . ? C114 H114 0.95 . ? C115 C116 1.372(8) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.377(8) . ? C121 C122 1.380(8) . ? C122 C123 1.382(8) . ? C122 H122 0.95 . ? C123 C124 1.369(9) . ? C123 H123 0.95 . ? C124 C125 1.371(9) . ? C124 H124 0.95 . ? C125 C126 1.398(8) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C01 P2 1.832(6) . ? C01 H01A 0.99 . ? C01 H01B 0.99 . ? P2 C211 1.834(6) . ? P2 C221 1.845(6) . ? C211 C212 1.376(9) . ? C211 C216 1.385(8) . ? C212 C213 1.387(9) . ? C212 H212 0.95 . ? C213 C214 1.371(10) . ? C213 H213 0.95 . ? C214 C215 1.359(11) . ? C214 H214 0.95 . ? C215 C216 1.396(9) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.373(8) . ? C221 C226 1.383(9) . ? C222 C223 1.385(8) . ? C222 H222 0.95 . ? C223 C224 1.383(9) . ? C223 H223 0.95 . ? C224 C225 1.365(9) . ? C224 H224 0.95 . ? C225 C226 1.386(9) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? P4 C411 1.818(7) . ? P4 C421 1.824(7) . ? P4 C02 1.850(7) . ? C411 C412 1.401(9) . ? C411 C416 1.417(9) . ? C412 C413 1.389(10) . ? C412 H412 0.95 . ? C413 C414 1.378(10) . ? C413 H413 0.95 . ? C414 C415 1.383(10) . ? C414 H414 0.95 . ? C415 C416 1.360(10) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C426 1.388(9) . ? C421 C422 1.417(9) . ? C422 C423 1.377(9) . ? C422 H422 0.95 . ? C423 C424 1.394(10) . ? C423 H423 0.95 . ? C424 C425 1.374(10) . ? C424 H424 0.95 . ? C425 C426 1.381(9) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C02 P5 1.819(7) . ? C02 H02A 0.99 . ? C02 H02B 0.99 . ? P5 C511 1.828(7) . ? P5 C521 1.842(7) . ? C511 C516 1.379(9) . ? C511 C512 1.389(10) . ? C512 C513 1.375(11) . ? C512 H512 0.95 . ? C513 C514 1.390(12) . ? C513 H513 0.95 . ? C514 C515 1.394(13) . ? C514 H514 0.95 . ? C515 C516 1.380(11) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C526 1.370(9) . ? C521 C522 1.407(10) . ? C522 C523 1.379(10) . ? C522 H522 0.95 . ? C523 C524 1.373(10) . ? C523 H523 0.95 . ? C524 C525 1.345(10) . ? C524 H524 0.95 . ? C525 C526 1.382(10) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? 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 C12 Co1 C11 103.1(3) . . ? C12 Co1 C1 101.0(3) . . ? C11 Co1 C1 143.4(3) . . ? C12 Co1 P1 94.2(2) . . ? C11 Co1 P1 105.9(2) . . ? C1 Co1 P1 99.38(19) . . ? C12 Co1 Co2 149.8(2) . . ? C11 Co1 Co2 103.15(19) . . ? C1 Co1 Co2 48.81(19) . . ? P1 Co1 Co2 92.88(5) . . ? C12 Co1 Co3 101.4(2) . . ? C11 Co1 Co3 98.1(2) . . ? C1 Co1 Co3 49.97(19) . . ? P1 Co1 Co3 147.59(6) . . ? Co2 Co1 Co3 60.13(3) . . ? C22 Co2 C21 102.5(3) . . ? C22 Co2 C1 109.0(3) . . ? C21 Co2 C1 138.3(3) . . ? C22 Co2 P2 96.4(2) . . ? C21 Co2 P2 108.3(2) . . ? C1 Co2 P2 94.87(19) . . ? C22 Co2 Co1 154.0(2) . . ? C21 Co2 Co1 92.8(2) . . ? C1 Co2 Co1 48.75(17) . . ? P2 Co2 Co1 98.65(5) . . ? C22 Co2 Co3 96.17(19) . . ? C21 Co2 Co3 100.9(2) . . ? C1 Co2 Co3 49.88(19) . . ? P2 Co2 Co3 144.74(6) . . ? Co1 Co2 Co3 59.96(3) . . ? C32 Co3 C33 98.7(3) . . ? C32 Co3 C31 102.7(3) . . ? C33 Co3 C31 104.2(3) . . ? C32 Co3 C1 103.1(3) . . ? C33 Co3 C1 101.4(3) . . ? C31 Co3 C1 140.0(3) . . ? C32 Co3 Co1 91.4(2) . . ? C33 Co3 Co1 150.0(2) . . ? C31 Co3 Co1 101.0(2) . . ? C1 Co3 Co1 48.56(17) . . ? C32 Co3 Co2 148.3(2) . . ? C33 Co3 Co2 100.9(2) . . ? C31 Co3 Co2 96.4(2) . . ? C1 Co3 Co2 48.53(18) . . ? Co1 Co3 Co2 59.91(3) . . ? C41 Co4 C42 99.6(3) . . ? C41 Co4 C8 143.3(3) . . ? C42 Co4 C8 107.7(3) . . ? C41 Co4 P4 105.4(2) . . ? C42 Co4 P4 95.4(2) . . ? C8 Co4 P4 96.0(2) . . ? C41 Co4 Co5 99.9(2) . . ? C42 Co4 Co5 155.5(3) . . ? C8 Co4 Co5 48.5(2) . . ? P4 Co4 Co5 93.52(6) . . ? C41 Co4 Co6 99.4(2) . . ? C42 Co4 Co6 101.7(2) . . ? C8 Co4 Co6 51.9(2) . . ? P4 Co4 Co6 146.87(7) . . ? Co5 Co4 Co6 60.46(4) . . ? C52 Co5 C51 103.5(3) . . ? C52 Co5 C8 103.4(3) . . ? C51 Co5 C8 141.2(3) . . ? C52 Co5 P5 97.1(3) . . ? C51 Co5 P5 104.8(2) . . ? C8 Co5 P5 99.0(2) . . ? C52 Co5 Co4 149.5(3) . . ? C51 Co5 Co4 97.2(2) . . ? C8 Co5 Co4 48.49(19) . . ? P5 Co5 Co4 99.01(6) . . ? C52 Co5 Co6 94.6(3) . . ? C51 Co5 Co6 99.0(2) . . ? C8 Co5 Co6 51.5(2) . . ? P5 Co5 Co6 150.17(7) . . ? Co4 Co5 Co6 59.78(4) . . ? C62 Co6 C63 96.2(4) . . ? C62 Co6 C61 101.8(4) . . ? C63 Co6 C61 102.3(3) . . ? C62 Co6 C8 108.0(3) . . ? C63 Co6 C8 101.8(3) . . ? C61 Co6 C8 139.0(3) . . ? C62 Co6 Co4 93.0(3) . . ? C63 Co6 Co4 149.7(3) . . ? C61 Co6 Co4 103.9(2) . . ? C8 Co6 Co4 47.99(18) . . ? C62 Co6 Co5 151.2(3) . . ? C63 Co6 Co5 103.4(3) . . ? C61 Co6 Co5 94.4(2) . . ? C8 Co6 Co5 47.7(2) . . ? Co4 Co6 Co5 59.75(4) . . ? O11 C11 Co1 174.3(6) . . ? O12 C12 Co1 179.5(7) . . ? O21 C21 Co2 177.9(6) . . ? O22 C22 Co2 179.2(6) . . ? O31 C31 Co3 178.1(6) . . ? O32 C32 Co3 178.2(8) . . ? O33 C33 Co3 177.4(7) . . ? O41 C41 Co4 175.5(7) . . ? O42 C42 Co4 179.4(7) . . ? O51 C51 Co5 176.8(7) . . ? O52 C52 Co5 177.0(8) . . ? O61 C61 Co6 179.5(8) . . ? O62 C62 Co6 178.3(8) . . ? O63 C63 Co6 167.5(8) . . ? C2 C1 Co1 130.9(5) . . ? C2 C1 Co2 138.1(5) . . ? Co1 C1 Co2 82.4(2) . . ? C2 C1 Co3 122.4(4) . . ? Co1 C1 Co3 81.5(2) . . ? Co2 C1 Co3 81.6(3) . . ? O2 C2 C3 120.9(6) . . ? O2 C2 C1 124.0(6) . . ? C3 C2 C1 115.1(6) . . ? C4 C3 C2 174.9(7) . . ? C3 C4 C5 179.2(8) . . ? C6 C5 C4 178.9(9) . . ? C5 C6 C7 174.3(8) . . ? O7 C7 C6 119.6(6) . . ? O7 C7 C8 123.8(6) . . ? C6 C7 C8 116.1(6) . . ? C7 C8 Co4 134.7(5) . . ? C7 C8 Co5 139.5(5) . . ? Co4 C8 Co5 83.0(3) . . ? C7 C8 Co6 114.7(5) . . ? Co4 C8 Co6 80.1(3) . . ? Co5 C8 Co6 80.8(3) . . ? C01 P1 C121 101.4(3) . . ? C01 P1 C111 104.1(3) . . ? C121 P1 C111 103.0(3) . . ? C01 P1 Co1 110.3(2) . . ? C121 P1 Co1 121.6(2) . . ? C111 P1 Co1 114.4(2) . . ? C112 C111 C116 118.7(6) . . ? C112 C111 P1 122.5(5) . . ? C116 C111 P1 118.2(5) . . ? C111 C112 C113 120.2(7) . . ? C111 C112 H112 119.9 . . ? C113 C112 H112 119.9 . . ? C114 C113 C112 119.8(7) . . ? C114 C113 H113 120.1 . . ? C112 C113 H113 120.1 . . ? C113 C114 C115 120.8(6) . . ? C113 C114 H114 119.6 . . ? C115 C114 H114 119.6 . . ? C114 C115 C116 120.3(6) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 120.1(6) . . ? C115 C116 H116 120 . . ? C111 C116 H116 120 . . ? C126 C121 C122 118.9(6) . . ? C126 C121 P1 122.0(5) . . ? C122 C121 P1 119.0(5) . . ? C121 C122 C123 121.2(6) . . ? C121 C122 H122 119.4 . . ? C123 C122 H122 119.4 . . ? C124 C123 C122 119.3(7) . . ? C124 C123 H123 120.4 . . ? C122 C123 H123 120.4 . . ? C123 C124 C125 120.8(6) . . ? C123 C124 H124 119.6 . . ? C125 C124 H124 119.6 . . ? C124 C125 C126 119.6(6) . . ? C124 C125 H125 120.2 . . ? C126 C125 H125 120.2 . . ? C121 C126 C125 120.1(6) . . ? C121 C126 H126 119.9 . . ? C125 C126 H126 119.9 . . ? P1 C01 P2 107.7(3) . . ? P1 C01 H01A 110.2 . . ? P2 C01 H01A 110.2 . . ? P1 C01 H01B 110.2 . . ? P2 C01 H01B 110.2 . . ? H01A C01 H01B 108.5 . . ? C01 P2 C211 104.1(3) . . ? C01 P2 C221 104.4(3) . . ? C211 P2 C221 101.4(3) . . ? C01 P2 Co2 109.0(2) . . ? C211 P2 Co2 114.5(2) . . ? C221 P2 Co2 121.6(2) . . ? C212 C211 C216 119.9(6) . . ? C212 C211 P2 123.9(5) . . ? C216 C211 P2 116.0(5) . . ? C211 C212 C213 119.9(7) . . ? C211 C212 H212 120 . . ? C213 C212 H212 120 . . ? C214 C213 C212 119.7(8) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C215 C214 C213 121.2(7) . . ? C215 C214 H214 119.4 . . ? C213 C214 H214 119.4 . . ? C214 C215 C216 119.6(7) . . ? C214 C215 H215 120.2 . . ? C216 C215 H215 120.2 . . ? C211 C216 C215 119.7(7) . . ? C211 C216 H216 120.2 . . ? C215 C216 H216 120.2 . . ? C222 C221 C226 118.9(6) . . ? C222 C221 P2 119.8(5) . . ? C226 C221 P2 121.3(5) . . ? C221 C222 C223 120.5(6) . . ? C221 C222 H222 119.7 . . ? C223 C222 H222 119.7 . . ? C224 C223 C222 120.4(6) . . ? C224 C223 H223 119.8 . . ? C222 C223 H223 119.8 . . ? C225 C224 C223 119.2(6) . . ? C225 C224 H224 120.4 . . ? C223 C224 H224 120.4 . . ? C224 C225 C226 120.6(7) . . ? C224 C225 H225 119.7 . . ? C226 C225 H225 119.7 . . ? C221 C226 C225 120.4(6) . . ? C221 C226 H226 119.8 . . ? C225 C226 H226 119.8 . . ? C411 P4 C421 101.7(3) . . ? C411 P4 C02 105.7(3) . . ? C421 P4 C02 102.9(3) . . ? C411 P4 Co4 113.6(2) . . ? C421 P4 Co4 120.4(2) . . ? C02 P4 Co4 110.9(2) . . ? C412 C411 C416 119.1(6) . . ? C412 C411 P4 122.5(5) . . ? C416 C411 P4 118.3(5) . . ? C413 C412 C411 119.4(7) . . ? C413 C412 H412 120.3 . . ? C411 C412 H412 120.3 . . ? C414 C413 C412 120.9(7) . . ? C414 C413 H413 119.5 . . ? C412 C413 H413 119.5 . . ? C413 C414 C415 119.3(7) . . ? C413 C414 H414 120.4 . . ? C415 C414 H414 120.4 . . ? C416 C415 C414 121.7(8) . . ? C416 C415 H415 119.1 . . ? C414 C415 H415 119.1 . . ? C415 C416 C411 119.5(7) . . ? C415 C416 H416 120.3 . . ? C411 C416 H416 120.3 . . ? C426 C421 C422 118.6(6) . . ? C426 C421 P4 121.6(5) . . ? C422 C421 P4 119.6(5) . . ? C423 C422 C421 120.6(7) . . ? C423 C422 H422 119.7 . . ? C421 C422 H422 119.7 . . ? C422 C423 C424 119.2(7) . . ? C422 C423 H423 120.4 . . ? C424 C423 H423 120.4 . . ? C425 C424 C423 120.7(7) . . ? C425 C424 H424 119.6 . . ? C423 C424 H424 119.6 . . ? C424 C425 C426 120.2(7) . . ? C424 C425 H425 119.9 . . ? C426 C425 H425 119.9 . . ? C425 C426 C421 120.5(7) . . ? C425 C426 H426 119.7 . . ? C421 C426 H426 119.7 . . ? P5 C02 P4 107.7(3) . . ? P5 C02 H02A 110.2 . . ? P4 C02 H02A 110.2 . . ? # Attachment '9.br1415b.cif' data_br1415b _database_code_depnum_ccdc_archive 'CCDC 754940' #TrackingRef '9.br1415b.cif' _audit_creation_date 2008-05-13T21:32:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C81 H51 Cl9 Co6 O16 P4' _chemical_formula_moiety 'C78 H48 Co6 O16 P4, 3(C H Cl3)' _chemical_formula_weight 2076.73 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.2045(13) _cell_length_b 17.0237(8) _cell_length_c 23.6203(11) _cell_angle_alpha 90 _cell_angle_beta 118.502(7) _cell_angle_gamma 90 _cell_volume 8553.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20941 _cell_measurement_theta_min 2.5397 _cell_measurement_theta_max 27.8869 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour deep_red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.96123 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.007137868 _diffrn_orient_matrix_ub_12 0.0377919064 _diffrn_orient_matrix_ub_13 0.0139172753 _diffrn_orient_matrix_ub_21 0.0135099386 _diffrn_orient_matrix_ub_22 -0.0168656873 _diffrn_orient_matrix_ub_23 0.0311088921 _diffrn_orient_matrix_ub_31 0.0295085935 _diffrn_orient_matrix_ub_32 -0.0013687203 _diffrn_orient_matrix_ub_33 0.0007256145 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0672 _diffrn_reflns_number 14969 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 14969 _reflns_number_gt 9737 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0842P)^2^+88.6829P] 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_number_reflns 14969 _refine_ls_number_parameters 1062 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2251 _refine_ls_wR_factor_gt 0.2091 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 2.098 _refine_diff_density_min -1.37 _refine_diff_density_rms 0.132 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.46412(4) 0.39586(7) 0.37507(4) 0.0319(2) Uani 1 1 d . . . Co2 Co 0.39007(4) 0.41702(6) 0.25965(4) 0.0306(2) Uani 1 1 d . . . Co3 Co 0.42893(4) 0.53099(7) 0.33397(4) 0.0355(3) Uani 1 1 d . . . Co4 Co 1.12307(4) 0.67556(7) 0.69356(4) 0.0386(3) Uani 1 1 d . A . Co5 Co 1.04837(4) 0.64798(7) 0.57990(4) 0.0347(2) Uani 1 1 d . A . Co6 Co 1.07214(4) 0.54502(7) 0.66249(4) 0.0368(3) Uani 1 1 d . . . C101 C 0.4037(3) 0.3657(4) 0.3937(3) 0.0315(17) Uani 1 1 d . . . O101 O 0.3624(2) 0.3495(3) 0.4033(2) 0.0379(13) Uani 1 1 d . . . C102 C 0.5248(3) 0.4275(5) 0.4506(3) 0.042(2) Uani 1 1 d . . . O102 O 0.5633(2) 0.4485(4) 0.4990(2) 0.0561(17) Uani 1 1 d . . . C21 C 0.3128(3) 0.4123(5) 0.2541(3) 0.0299(17) Uani 1 1 d . . . O21 O 0.2655(2) 0.4144(4) 0.2514(2) 0.0432(14) Uani 1 1 d . . . C22 C 0.3753(3) 0.4624(5) 0.1860(3) 0.0381(19) Uani 1 1 d . . . O22 O 0.3660(2) 0.4944(4) 0.1397(2) 0.0444(14) Uani 1 1 d . . . C31 C 0.3648(3) 0.5357(5) 0.3533(3) 0.0357(18) Uani 1 1 d . . . O31 O 0.3250(2) 0.5393(4) 0.3654(2) 0.0453(14) Uani 1 1 d . . . C32 C 0.4887(3) 0.5859(6) 0.3989(4) 0.050(2) Uani 1 1 d . . . O32 O 0.5263(3) 0.6220(5) 0.4399(3) 0.073(2) Uani 1 1 d . . . C33 C 0.4081(3) 0.6030(6) 0.2710(3) 0.045(2) Uani 1 1 d . . . O33 O 0.3966(3) 0.6490(4) 0.2318(3) 0.0627(18) Uani 1 1 d . . . C41 C 1.1995(3) 0.6485(6) 0.7017(3) 0.054(2) Uani 1 1 d . . . O41 O 1.2466(2) 0.6289(4) 0.7081(3) 0.065(2) Uani 1 1 d . . . C42 C 1.1402(3) 0.6782(6) 0.7755(4) 0.050(2) Uani 1 1 d . . . O42 O 1.1509(3) 0.6777(5) 0.8281(3) 0.068(2) Uani 1 1 d . . . C51 C 1.1095(3) 0.6304(5) 0.5588(3) 0.042(2) Uani 1 1 d . . . O51 O 1.1501(2) 0.6157(4) 0.5485(2) 0.0538(17) Uani 1 1 d . . . C52 C 0.9815(3) 0.6019(5) 0.5168(3) 0.0373(19) Uani 1 1 d . . . O52 O 0.9381(2) 0.5747(4) 0.4760(2) 0.0515(16) Uani 1 1 d . . . C61 C 1.1356(3) 0.4940(5) 0.6576(3) 0.041(2) Uani 1 1 d . . . O61 O 1.1751(2) 0.4643(4) 0.6534(3) 0.0583(18) Uani 1 1 d . . . C62 C 1.0817(4) 0.5196(6) 0.7403(4) 0.059(2) Uani 1 1 d . . . O62 O 1.0845(4) 0.5008(4) 0.7874(3) 0.091(2) Uani 1 1 d . . . C63 C 1.0068(3) 0.4849(5) 0.6126(3) 0.0411(19) Uani 1 1 d . . . O63 O 0.9656(2) 0.4449(4) 0.5793(3) 0.0545(15) Uani 1 1 d . . . C1 C 0.4722(3) 0.4523(5) 0.3113(3) 0.0309(17) Uani 1 1 d . . . C2 C 0.5257(3) 0.4696(5) 0.3003(3) 0.0346(18) Uani 1 1 d . . . O2 O 0.5254(2) 0.4561(4) 0.2487(2) 0.0452(15) Uani 1 1 d . . . C3 C 0.5816(3) 0.5002(5) 0.3543(3) 0.0306(17) Uani 1 1 d . . . C4 C 0.6313(3) 0.5191(5) 0.3982(3) 0.0330(17) Uani 1 1 d . . . C5 C 0.6920(3) 0.5415(4) 0.4468(3) 0.0240(15) Uani 1 1 d . . . C6 C 0.7388(3) 0.5564(5) 0.4289(3) 0.0340(18) Uani 1 1 d . . . H6 H 0.73 0.5494 0.3855 0.041 Uiso 1 1 calc R . . C7 C 0.7968(3) 0.5809(5) 0.4741(3) 0.0351(18) Uani 1 1 d . . . H7 H 0.8282 0.5909 0.4618 0.042 Uiso 1 1 calc R . . C8 C 0.8110(3) 0.5913(4) 0.5379(3) 0.0253(15) Uani 1 1 d . . . C9 C 0.7642(3) 0.5775(4) 0.5552(3) 0.0283(16) Uani 1 1 d . . . H9 H 0.7732 0.5848 0.5987 0.034 Uiso 1 1 calc R . . C10 C 0.7053(3) 0.5536(4) 0.5101(3) 0.0262(16) Uani 1 1 d . . . H10 H 0.6736 0.5454 0.5223 0.031 Uiso 1 1 calc R . . C11 C 0.8731(3) 0.6164(4) 0.5851(3) 0.0308(17) Uani 1 1 d . . . C12 C 0.9248(3) 0.6350(4) 0.6222(3) 0.0294(16) Uani 1 1 d . . . C13 C 0.9873(3) 0.6646(5) 0.6689(3) 0.0389(19) Uani 1 1 d . . . O13 O 0.9936(2) 0.6981(4) 0.7173(2) 0.0589(17) Uani 1 1 d . . . C14 C 1.0382(3) 0.6498(4) 0.6538(3) 0.0272(16) Uani 1 1 d . . . P1 P 0.51362(7) 0.29139(13) 0.36639(8) 0.0322(5) Uani 1 1 d . . . C111 C 0.5989(3) 0.2986(5) 0.4063(3) 0.0370(19) Uani 1 1 d . . . C112 C 0.6330(3) 0.3163(5) 0.3745(3) 0.0367(19) Uani 1 1 d . . . H112 H 0.6121 0.3231 0.329 0.044 Uiso 1 1 calc R . . C113 C 0.6975(3) 0.3241(6) 0.4095(4) 0.050(2) Uani 1 1 d . . . H113 H 0.7209 0.3321 0.3872 0.06 Uiso 1 1 calc R . . C114 C 0.7286(4) 0.3207(7) 0.4754(4) 0.069(3) Uani 1 1 d . . . H114 H 0.7729 0.3275 0.4987 0.082 Uiso 1 1 calc R . . C115 C 0.6945(4) 0.3071(6) 0.5074(4) 0.058(3) Uani 1 1 d . . . H115 H 0.7153 0.3057 0.5531 0.069 Uiso 1 1 calc R . . C116 C 0.6305(3) 0.2954(6) 0.4734(4) 0.055(3) Uani 1 1 d . . . H116 H 0.6076 0.2852 0.4959 0.066 Uiso 1 1 calc R . . C121 C 0.5026(3) 0.1938(5) 0.3916(3) 0.0312(18) Uani 1 1 d . . . C122 C 0.4583(3) 0.1801(5) 0.4116(3) 0.0343(17) Uani 1 1 d . . . H122 H 0.4351 0.2226 0.4158 0.041 Uiso 1 1 calc R . . C123 C 0.4479(3) 0.1044(5) 0.4255(3) 0.0390(19) Uani 1 1 d . . . H123 H 0.4166 0.0949 0.4382 0.047 Uiso 1 1 calc R . . C124 C 0.4822(3) 0.0432(5) 0.4213(3) 0.0398(19) Uani 1 1 d . . . H124 H 0.4752 -0.0085 0.4316 0.048 Uiso 1 1 calc R . . C125 C 0.5267(3) 0.0559(5) 0.4023(4) 0.046(2) Uani 1 1 d . . . H125 H 0.55 0.0131 0.3988 0.056 Uiso 1 1 calc R . . C126 C 0.5376(3) 0.1327(5) 0.3879(3) 0.045(2) Uani 1 1 d . . . H126 H 0.5691 0.1422 0.3757 0.053 Uiso 1 1 calc R . . C01 C 1.0362(3) 0.8283(5) 0.6183(4) 0.049(2) Uani 1 1 d . A . H01A H 1.0346 0.8846 0.6071 0.059 Uiso 1 1 calc R . . H01B H 1.0056 0.819 0.6341 0.059 Uiso 1 1 calc R . . P2 P 0.40762(7) 0.29923(12) 0.23388(7) 0.0295(4) Uani 1 1 d . . . C211 C 0.3941(3) 0.2879(5) 0.1512(3) 0.0302(17) Uani 1 1 d . . . C212 C 0.4332(3) 0.3294(5) 0.1323(3) 0.041(2) Uani 1 1 d . . . H212 H 0.4673 0.3594 0.1632 0.049 Uiso 1 1 calc R . . C213 C 0.4221(4) 0.3266(6) 0.0696(3) 0.049(2) Uani 1 1 d . . . H213 H 0.4496 0.3529 0.0576 0.058 Uiso 1 1 calc R . . C214 C 0.3719(4) 0.2861(5) 0.0248(4) 0.049(2) Uani 1 1 d . . . H214 H 0.3639 0.2856 -0.0186 0.059 Uiso 1 1 calc R . . C215 C 0.3327(4) 0.2463(5) 0.0410(3) 0.044(2) Uani 1 1 d . . . H215 H 0.2978 0.2181 0.0091 0.053 Uiso 1 1 calc R . . C216 C 0.3442(4) 0.2472(5) 0.1053(3) 0.041(2) Uani 1 1 d . . . H216 H 0.3171 0.2192 0.1168 0.05 Uiso 1 1 calc R . . C221 C 0.3699(3) 0.2127(4) 0.2453(3) 0.0269(16) Uani 1 1 d . . . C222 C 0.3219(3) 0.2195(5) 0.2619(3) 0.0357(18) Uani 1 1 d . . . H222 H 0.3074 0.2698 0.2662 0.043 Uiso 1 1 calc R . . C223 C 0.2955(3) 0.1523(5) 0.2719(4) 0.046(2) Uani 1 1 d . . . H223 H 0.2626 0.157 0.2827 0.055 Uiso 1 1 calc R . . C224 C 0.3160(3) 0.0796(5) 0.2666(3) 0.039(2) Uani 1 1 d . . . H224 H 0.2974 0.0343 0.2742 0.047 Uiso 1 1 calc R . . C225 C 0.3640(3) 0.0708(5) 0.2502(3) 0.0367(18) Uani 1 1 d . . . H225 H 0.3782 0.0201 0.2464 0.044 Uiso 1 1 calc R . . C226 C 0.3903(3) 0.1371(5) 0.2397(3) 0.0370(19) Uani 1 1 d . . . H226 H 0.423 0.1318 0.2285 0.044 Uiso 1 1 calc R . . P4 P 1.11449(9) 0.80294(15) 0.68035(10) 0.0511(6) Uani 1 1 d . . . C411 C 1.1218(4) 0.8533(6) 0.7509(4) 0.063(3) Uani 1 1 d . A . C412 C 1.0711(4) 0.8571(7) 0.7643(4) 0.075(3) Uani 1 1 d . . . H412 H 1.0308 0.8389 0.7333 0.09 Uiso 1 1 calc R A . C413 C 1.0797(4) 0.8869(7) 0.8214(5) 0.077(3) Uani 1 1 d . A . H413 H 1.0454 0.8889 0.8304 0.093 Uiso 1 1 calc R . . C414 C 1.1371(4) 0.9137(6) 0.8657(4) 0.063(3) Uani 1 1 d . . . H414 H 1.1424 0.9341 0.9054 0.075 Uiso 1 1 calc R A . C415 C 1.1873(4) 0.9120(6) 0.8545(4) 0.057(2) Uani 1 1 d . A . H415 H 1.2274 0.9303 0.886 0.068 Uiso 1 1 calc R . . C416 C 1.1783(3) 0.8821(4) 0.7946(3) 0.051(2) Uani 1 1 d . . . H416 H 1.2122 0.8823 0.7851 0.062 Uiso 1 1 calc R A . C421 C 1.1575(3) 0.8690(4) 0.6514(3) 0.026(3) Uiso 0.5 1 d PR A 1 C422 C 1.1502(3) 0.9502(4) 0.6477(3) 0.037(3) Uiso 0.5 1 d PR A 1 H422 H 1.1262 0.9759 0.6644 0.044 Uiso 0.5 1 d PR B 1 C423 C 1.1784(7) 0.9933(10) 0.6197(7) 0.038(4) Uiso 0.5 1 d P A 1 H423 H 1.1736 1.0488 0.6176 0.045 Uiso 0.5 1 calc PR A 1 C424 C 1.2146(7) 0.9585(10) 0.5936(7) 0.038(4) Uiso 0.5 1 d P A 1 H424 H 1.2335 0.9896 0.5741 0.046 Uiso 0.5 1 calc PR A 1 C425 C 1.2216(7) 0.8746(11) 0.5977(7) 0.040(4) Uiso 0.5 1 d P A 1 H425 H 1.245 0.8486 0.5804 0.048 Uiso 0.5 1 calc PR A 1 C426 C 1.1942(5) 0.8332(7) 0.6266(5) 0.024(3) Uiso 0.5 1 d P A 1 H426 H 1.1998 0.7778 0.6303 0.029 Uiso 0.5 1 calc PR A 1 C431 C 1.1713(5) 0.8460(7) 0.6589(5) 0.066(6) Uiso 0.5 1 d PR A 2 C432 C 1.1713(5) 0.9277(7) 0.6604(5) 0.081(7) Uiso 0.5 1 d PR A 2 H432 H 1.1359 0.9532 0.6593 0.097 Uiso 0.5 1 d PR A 2 C433 C 1.2060(11) 0.9712(16) 0.6347(11) 0.080(7) Uiso 0.5 1 d P A 2 H433 H 1.2096 1.0268 0.6354 0.096 Uiso 0.5 1 calc PR A 2 C434 C 1.2323(9) 0.9226(14) 0.6099(10) 0.064(5) Uiso 0.5 1 d P A 2 H434 H 1.2496 0.9487 0.5864 0.076 Uiso 0.5 1 calc PR A 2 C435 C 1.2392(10) 0.8423(14) 0.6118(10) 0.073(6) Uiso 0.5 1 d P A 2 H435 H 1.2654 0.8163 0.5978 0.088 Uiso 0.5 1 calc PR A 2 C436 C 1.2048(9) 0.8025(14) 0.6357(9) 0.060(5) Uiso 0.5 1 d P A 2 H436 H 1.2041 0.7467 0.6362 0.072 Uiso 0.5 1 calc PR A 2 C02 C 0.4916(3) 0.2757(5) 0.2810(3) 0.0329(18) Uani 1 1 d . . . H02A H 0.5166 0.3103 0.2682 0.039 Uiso 1 1 calc R . . H02B H 0.4992 0.2204 0.2737 0.039 Uiso 1 1 calc R . . P5 P 1.01618(9) 0.76821(14) 0.54728(9) 0.0442(5) Uani 1 1 d . . . C511 C 0.9315(4) 0.7816(5) 0.4969(4) 0.048(2) Uani 1 1 d . A . C512 C 0.8912(4) 0.8004(7) 0.5206(4) 0.069(3) Uani 1 1 d . . . H512 H 0.907 0.8057 0.5658 0.082 Uiso 1 1 calc R A . C513 C 0.8265(4) 0.8117(8) 0.4786(5) 0.079(4) Uani 1 1 d . A . H513 H 0.7994 0.8284 0.4949 0.095 Uiso 1 1 calc R . . C514 C 0.8036(5) 0.7984(7) 0.4146(5) 0.073(3) Uani 1 1 d . . . H514 H 0.7598 0.8042 0.3864 0.088 Uiso 1 1 calc R A . C515 C 0.8409(5) 0.7776(9) 0.3912(5) 0.090(4) Uani 1 1 d . A . H515 H 0.8238 0.7691 0.3462 0.108 Uiso 1 1 calc R . . C516 C 0.9054(5) 0.7679(8) 0.4317(5) 0.086(4) Uani 1 1 d . . . H516 H 0.9315 0.7518 0.414 0.103 Uiso 1 1 calc R A . C521 C 1.0455(4) 0.8167(6) 0.4985(4) 0.055(2) Uani 1 1 d . A . C522 C 1.0593(4) 0.7739(6) 0.4581(4) 0.059(2) Uani 1 1 d . . . H522 H 1.0575 0.7182 0.4589 0.071 Uiso 1 1 calc R A . C523 C 1.0760(5) 0.8105(8) 0.4158(5) 0.093(3) Uani 1 1 d . A . H523 H 1.0843 0.7806 0.3867 0.112 Uiso 1 1 calc R . . C524 C 1.0803(6) 0.8936(8) 0.4172(6) 0.107(4) Uani 1 1 d . . . H524 H 1.091 0.9195 0.3882 0.128 Uiso 1 1 calc R A . C525 C 1.0694(6) 0.9366(9) 0.4587(6) 0.120(4) Uani 1 1 d . A . H525 H 1.0759 0.9918 0.4613 0.144 Uiso 1 1 calc R . . C526 C 1.0485(5) 0.8998(7) 0.4981(5) 0.079(3) Uani 1 1 d . . . H526 H 1.0365 0.9302 0.5242 0.095 Uiso 1 1 calc R A . Cl11 Cl 0.09812(12) 0.18544(18) 0.21739(12) 0.0752(8) Uani 1 1 d . C . Cl12 Cl 0.1725(2) 0.1932(3) 0.35456(16) 0.0908(14) Uani 0.751(4) 1 d P C 1 Cl13 Cl 0.17508(14) 0.3196(2) 0.27571(15) 0.0740(10) Uani 0.751(4) 1 d P C 1 Cl14 Cl 0.2045(5) 0.2674(9) 0.3281(8) 0.120(5) Uani 0.249(4) 1 d P C 2 Cl15 Cl 0.1253(12) 0.1661(16) 0.3421(13) 0.210(12) Uani 0.249(4) 1 d P C 2 C100 C 0.1283(4) 0.2459(6) 0.2860(4) 0.061(3) Uani 1 1 d . . . H10A H 0.0927 0.2715 0.2891 0.073 Uiso 0.751(4) 1 calc PR C 1 H10B H 0.1005 0.2917 0.281 0.073 Uiso 0.249(4) 1 d PR C 2 Cl21 Cl 0.60095(9) 0.35914(16) 0.19185(10) 0.0584(6) Uani 1 1 d . . . Cl22 Cl 0.58088(15) 0.3342(3) 0.06461(13) 0.1222(14) Uani 1 1 d . . . Cl23 Cl 0.67218(17) 0.24078(18) 0.16495(15) 0.0983(11) Uani 1 1 d . . . C200 C 0.6360(5) 0.3283(6) 0.1448(4) 0.070(3) Uani 1 1 d . . . H20A H 0.6692 0.3679 0.1518 0.083 Uiso 1 1 calc R . . Cl31 Cl 0.71582(17) 0.3868(2) 0.02843(18) 0.1131(11) Uani 1 1 d . D . Cl32 Cl 0.7515(2) 0.4815(3) 0.1473(2) 0.0822(15) Uani 0.593(4) 1 d P D 1 Cl33 Cl 0.7125(3) 0.5497(3) 0.0240(2) 0.0903(19) Uani 0.593(4) 1 d P D 1 Cl34 Cl 0.7730(4) 0.5385(5) 0.0313(4) 0.110(3) Uani 0.407(4) 1 d P D 2 Cl35 Cl 0.7016(4) 0.5172(7) 0.0977(4) 0.119(3) Uani 0.407(4) 1 d P D 2 C300 C 0.7494(10) 0.4759(13) 0.0706(10) 0.177(8) Uiso 1 1 d . . . H30A H 0.7939 0.4779 0.0787 0.212 Uiso 0.593(4) 1 calc PR D 1 H30B H 0.7885 0.46 0.1103 0.212 Uiso 0.407(4) 1 d PR D 2 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 0.0228(4) 0.0579(7) 0.0204(4) -0.0067(4) 0.0146(3) -0.0093(4) Co2 0.0182(3) 0.0557(6) 0.0217(4) -0.0078(4) 0.0127(3) -0.0037(4) Co3 0.0270(4) 0.0591(7) 0.0270(4) -0.0115(4) 0.0181(3) -0.0083(4) Co4 0.0250(4) 0.0666(7) 0.0308(4) -0.0211(5) 0.0186(3) -0.0158(5) Co5 0.0246(4) 0.0594(7) 0.0277(4) -0.0157(4) 0.0185(3) -0.0128(4) Co6 0.0313(4) 0.0555(7) 0.0299(4) -0.0123(4) 0.0196(3) -0.0063(5) C101 0.033(3) 0.045(4) 0.020(3) -0.006(3) 0.015(2) -0.009(3) O101 0.031(2) 0.058(3) 0.036(2) -0.003(2) 0.0258(18) -0.007(2) C102 0.038(3) 0.067(6) 0.028(3) -0.007(3) 0.022(3) -0.013(4) O102 0.049(3) 0.090(5) 0.027(2) -0.014(3) 0.017(2) -0.022(3) C21 0.018(3) 0.047(4) 0.028(3) -0.001(3) 0.013(2) 0.003(3) O21 0.026(2) 0.067(4) 0.042(3) -0.003(3) 0.0212(19) -0.004(2) C22 0.019(3) 0.062(5) 0.036(3) -0.004(4) 0.015(3) -0.004(3) O22 0.037(2) 0.072(4) 0.030(2) 0.004(2) 0.0205(19) -0.002(3) C31 0.028(3) 0.053(5) 0.029(3) 0.004(3) 0.016(3) 0.007(3) O31 0.030(2) 0.074(4) 0.040(2) 0.002(3) 0.023(2) 0.003(3) C32 0.038(3) 0.080(6) 0.042(4) -0.029(4) 0.028(3) -0.022(4) O32 0.051(3) 0.122(6) 0.057(3) -0.047(3) 0.035(2) -0.032(4) C33 0.033(3) 0.071(6) 0.033(3) -0.014(4) 0.018(3) -0.010(4) O33 0.087(4) 0.061(4) 0.051(3) 0.000(3) 0.041(3) -0.004(3) C41 0.031(3) 0.100(7) 0.034(3) -0.034(4) 0.018(3) -0.026(4) O41 0.024(2) 0.121(6) 0.054(3) -0.026(3) 0.021(2) -0.006(3) C42 0.033(3) 0.078(6) 0.049(4) -0.022(4) 0.026(3) -0.013(4) O42 0.053(3) 0.117(6) 0.039(3) -0.025(3) 0.026(2) -0.011(4) C51 0.033(3) 0.067(6) 0.029(3) -0.014(3) 0.017(3) -0.019(4) O51 0.031(2) 0.099(5) 0.043(3) -0.026(3) 0.027(2) -0.011(3) C52 0.035(3) 0.063(5) 0.035(3) -0.020(3) 0.024(2) -0.003(3) O52 0.030(2) 0.091(4) 0.038(2) -0.031(3) 0.020(2) -0.017(3) C61 0.028(3) 0.060(5) 0.030(3) -0.007(3) 0.012(3) 0.004(4) O61 0.038(3) 0.085(5) 0.052(3) -0.008(3) 0.021(2) 0.013(3) C62 0.075(5) 0.060(6) 0.051(4) -0.012(4) 0.039(4) 0.013(5) O62 0.171(6) 0.074(5) 0.049(3) -0.003(3) 0.069(4) 0.009(5) C63 0.043(3) 0.055(5) 0.044(3) -0.007(3) 0.036(3) -0.002(4) O63 0.055(3) 0.066(4) 0.064(3) -0.032(3) 0.045(2) -0.029(3) C1 0.025(3) 0.052(5) 0.016(3) -0.015(3) 0.010(2) -0.007(3) C2 0.023(3) 0.060(5) 0.022(3) 0.002(3) 0.013(2) 0.004(3) O2 0.032(2) 0.083(4) 0.030(2) -0.011(2) 0.0226(18) -0.014(3) C3 0.025(3) 0.048(5) 0.026(3) 0.004(3) 0.018(2) 0.000(3) C4 0.029(3) 0.049(5) 0.032(3) -0.001(3) 0.023(2) -0.007(3) C5 0.018(2) 0.028(4) 0.028(3) 0.000(3) 0.013(2) 0.002(3) C6 0.025(3) 0.050(5) 0.035(3) -0.009(3) 0.020(2) -0.002(3) C7 0.024(3) 0.051(5) 0.037(3) -0.008(3) 0.020(3) -0.005(3) C8 0.020(3) 0.023(4) 0.032(3) -0.003(3) 0.011(2) -0.003(3) C9 0.033(3) 0.031(4) 0.023(3) 0.003(3) 0.015(2) 0.003(3) C10 0.017(3) 0.034(4) 0.030(3) 0.003(3) 0.013(2) -0.005(3) C11 0.026(3) 0.042(4) 0.033(3) 0.000(3) 0.021(2) 0.002(3) C12 0.023(3) 0.045(4) 0.026(3) -0.010(3) 0.017(2) -0.008(3) C13 0.032(3) 0.059(5) 0.033(3) -0.013(3) 0.022(3) -0.013(3) O13 0.034(2) 0.107(5) 0.047(3) -0.047(3) 0.028(2) -0.018(3) C14 0.018(3) 0.039(4) 0.024(3) -0.016(3) 0.009(2) -0.011(3) P1 0.0201(7) 0.0608(13) 0.0189(7) 0.0009(8) 0.0118(6) -0.0026(8) C111 0.025(3) 0.061(5) 0.024(3) 0.000(3) 0.011(3) -0.002(3) C112 0.022(3) 0.057(5) 0.038(3) 0.001(3) 0.021(3) 0.005(3) C113 0.024(3) 0.092(7) 0.042(4) 0.003(4) 0.021(3) 0.001(4) C114 0.029(4) 0.126(9) 0.049(5) 0.008(5) 0.017(3) -0.007(5) C115 0.035(4) 0.092(7) 0.036(4) 0.009(5) 0.008(3) -0.001(5) C116 0.033(4) 0.097(7) 0.033(4) 0.012(4) 0.014(3) -0.016(4) C121 0.021(3) 0.051(5) 0.017(3) 0.009(3) 0.006(2) 0.006(3) C122 0.039(3) 0.040(4) 0.036(3) -0.003(3) 0.028(3) -0.005(3) C123 0.037(3) 0.053(5) 0.032(3) -0.002(3) 0.021(3) 0.005(4) C124 0.045(4) 0.043(5) 0.030(3) -0.001(3) 0.017(3) -0.001(4) C125 0.047(4) 0.055(5) 0.045(4) 0.010(4) 0.028(3) 0.012(4) C126 0.042(3) 0.064(6) 0.036(3) 0.019(4) 0.026(3) 0.009(4) C01 0.059(4) 0.053(5) 0.060(4) -0.021(4) 0.048(3) -0.022(4) P2 0.0184(7) 0.0542(12) 0.0186(7) -0.0033(7) 0.0110(6) 0.0012(8) C211 0.023(3) 0.048(4) 0.019(3) 0.002(3) 0.010(2) 0.007(3) C212 0.030(3) 0.070(6) 0.028(3) -0.007(3) 0.018(3) -0.002(4) C213 0.046(4) 0.073(6) 0.029(3) -0.010(4) 0.020(3) -0.010(4) C214 0.081(5) 0.041(5) 0.036(3) -0.010(3) 0.037(3) 0.005(4) C215 0.068(5) 0.030(4) 0.016(3) -0.002(3) 0.006(3) -0.009(4) C216 0.054(4) 0.034(4) 0.032(4) -0.002(3) 0.017(3) -0.004(4) C221 0.027(3) 0.033(4) 0.022(3) -0.004(3) 0.013(2) -0.005(3) C222 0.025(3) 0.042(4) 0.048(4) -0.007(3) 0.023(3) -0.007(3) C223 0.032(3) 0.067(6) 0.048(4) -0.006(4) 0.027(3) 0.007(4) C224 0.034(3) 0.053(5) 0.030(3) 0.004(3) 0.015(3) -0.007(4) C225 0.040(3) 0.048(5) 0.027(3) 0.003(3) 0.020(3) 0.011(3) C226 0.034(3) 0.052(5) 0.032(3) 0.002(3) 0.022(3) 0.008(3) P4 0.0553(9) 0.0656(15) 0.0534(10) -0.0335(10) 0.0429(8) -0.0324(10) C411 0.065(4) 0.086(7) 0.061(4) -0.045(4) 0.049(3) -0.035(5) C412 0.059(4) 0.110(8) 0.071(5) -0.062(5) 0.044(4) -0.035(5) C413 0.078(5) 0.099(8) 0.085(5) -0.055(5) 0.064(4) -0.040(5) C414 0.062(4) 0.083(7) 0.057(4) -0.039(4) 0.040(4) -0.020(5) C415 0.054(4) 0.066(6) 0.050(4) -0.032(4) 0.025(4) -0.024(4) C416 0.050(4) 0.063(6) 0.056(4) -0.015(4) 0.037(3) -0.010(4) C02 0.016(3) 0.062(5) 0.019(3) -0.001(3) 0.008(2) 0.000(3) P5 0.0477(9) 0.0555(14) 0.0438(9) -0.0086(9) 0.0335(8) -0.0125(10) C511 0.051(4) 0.047(5) 0.055(4) 0.013(4) 0.033(3) 0.004(4) C512 0.057(5) 0.101(8) 0.055(5) 0.006(5) 0.034(4) -0.016(5) C513 0.048(5) 0.115(10) 0.073(6) -0.014(6) 0.028(5) -0.011(6) C514 0.055(5) 0.094(8) 0.058(5) 0.031(5) 0.017(5) 0.006(6) C515 0.061(6) 0.165(13) 0.040(5) 0.013(6) 0.021(4) 0.005(7) C516 0.073(6) 0.144(12) 0.051(5) 0.003(6) 0.038(4) 0.008(7) C521 0.060(4) 0.070(6) 0.055(4) 0.002(4) 0.043(3) -0.014(4) C522 0.079(5) 0.058(6) 0.059(5) 0.003(4) 0.048(4) -0.013(5) C523 0.143(6) 0.096(9) 0.096(6) -0.008(6) 0.102(5) -0.014(7) C524 0.168(7) 0.102(10) 0.112(6) -0.011(6) 0.117(6) -0.043(8) C525 0.186(8) 0.099(10) 0.148(8) -0.008(7) 0.138(7) -0.051(8) C526 0.108(6) 0.080(8) 0.082(6) -0.006(5) 0.070(5) -0.030(6) Cl11 0.0824(14) 0.0855(19) 0.0686(13) -0.0210(13) 0.0447(11) -0.0226(14) Cl12 0.115(3) 0.102(3) 0.0522(17) 0.0132(19) 0.0378(18) 0.044(2) Cl13 0.0858(16) 0.086(2) 0.0854(17) -0.0436(16) 0.0689(13) -0.0483(17) Cl14 0.080(5) 0.110(10) 0.213(11) -0.073(9) 0.105(6) -0.022(7) Cl15 0.175(17) 0.21(2) 0.23(2) 0.091(18) 0.079(17) -0.050(17) C100 0.049(4) 0.074(7) 0.068(5) -0.020(5) 0.034(4) -0.010(5) Cl21 0.0420(9) 0.0934(18) 0.0444(10) -0.0157(11) 0.0244(8) -0.0039(11) Cl22 0.1086(19) 0.199(4) 0.0433(13) -0.0113(17) 0.0233(13) 0.081(2) Cl23 0.131(2) 0.0601(17) 0.0902(19) 0.0011(15) 0.0414(18) 0.0309(18) C200 0.084(6) 0.064(6) 0.059(5) -0.008(5) 0.032(5) 0.024(5) Cl31 0.143(2) 0.091(2) 0.135(2) -0.0473(19) 0.0904(19) -0.026(2) Cl32 0.113(3) 0.092(4) 0.062(2) -0.012(2) 0.059(2) -0.003(3) Cl33 0.121(4) 0.076(3) 0.051(2) 0.008(2) 0.023(2) 0.003(3) Cl34 0.115(5) 0.109(6) 0.138(5) -0.066(5) 0.087(4) -0.057(5) Cl35 0.122(5) 0.162(9) 0.093(5) -0.027(5) 0.067(4) 0.031(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C102 1.769(7) . ? Co1 C101 1.793(7) . ? Co1 C1 1.874(7) . ? Co1 P1 2.208(2) . ? Co1 Co2 2.4721(12) . ? Co1 Co3 2.4841(16) . ? Co2 C22 1.776(8) . ? Co2 C21 1.814(6) . ? Co2 C1 1.867(6) . ? Co2 P2 2.195(2) . ? Co2 Co3 2.4809(14) . ? Co3 C32 1.790(7) . ? Co3 C33 1.803(9) . ? Co3 C31 1.817(7) . ? Co3 C1 1.926(7) . ? Co4 C42 1.776(8) . ? Co4 C41 1.824(8) . ? Co4 C14 1.858(6) . ? Co4 P4 2.186(3) . ? Co4 Co5 2.4626(12) . ? Co4 Co6 2.4767(16) . ? Co5 C52 1.776(7) . ? Co5 C51 1.797(8) . ? Co5 C14 1.876(7) . ? Co5 P5 2.195(3) . ? Co5 Co6 2.4776(15) . ? Co6 C63 1.777(8) . ? Co6 C62 1.792(9) . ? Co6 C61 1.816(8) . ? Co6 C14 1.933(7) . ? C101 O101 1.157(8) . ? C102 O102 1.134(8) . ? C21 O21 1.115(7) . ? C22 O22 1.145(9) . ? C31 O31 1.131(8) . ? C32 O32 1.141(9) . ? C33 O33 1.141(10) . ? C41 O41 1.128(9) . ? C42 O42 1.141(9) . ? C51 O51 1.147(9) . ? C52 O52 1.132(8) . ? C61 O61 1.127(9) . ? C62 O62 1.129(11) . ? C63 O63 1.152(8) . ? C1 C2 1.469(9) . ? C2 O2 1.237(8) . ? C2 C3 1.442(9) . ? C3 C4 1.198(8) . ? C4 C5 1.419(8) . ? C5 C10 1.387(9) . ? C5 C6 1.409(9) . ? C6 C7 1.362(9) . ? C6 H6 0.95 . ? C7 C8 1.387(9) . ? C7 H7 0.95 . ? C8 C9 1.395(9) . ? C8 C11 1.445(8) . ? C9 C10 1.373(8) . ? C9 H9 0.95 . ? C10 H10 0.95 . ? C11 C12 1.177(8) . ? C12 C13 1.472(9) . ? C13 O13 1.219(9) . ? C13 C14 1.460(9) . ? P1 C111 1.819(7) . ? P1 C121 1.827(8) . ? P1 C02 1.843(6) . ? C111 C112 1.388(10) . ? C111 C116 1.393(10) . ? C112 C113 1.380(9) . ? C112 H112 0.95 . ? C113 C114 1.370(11) . ? C113 H113 0.95 . ? C114 C115 1.378(13) . ? C114 H114 0.95 . ? C115 C116 1.377(10) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.369(11) . ? C121 C122 1.383(10) . ? C122 C123 1.382(11) . ? C122 H122 0.95 . ? C123 C124 1.366(11) . ? C123 H123 0.95 . ? C124 C125 1.365(11) . ? C124 H124 0.95 . ? C125 C126 1.408(12) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C01 P4 1.809(8) . ? C01 P5 1.821(8) . ? C01 H01A 0.99 . ? C01 H01B 0.99 . ? P2 C221 1.819(7) . ? P2 C211 1.830(7) . ? P2 C02 1.835(6) . ? C211 C216 1.367(10) . ? C211 C212 1.411(10) . ? C212 C213 1.376(10) . ? C212 H212 0.95 . ? C213 C214 1.359(11) . ? C213 H213 0.95 . ? C214 C215 1.360(12) . ? C214 H214 0.95 . ? C215 C216 1.407(10) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.399(9) . ? C221 C226 1.406(10) . ? C222 C223 1.384(11) . ? C222 H222 0.95 . ? C223 C224 1.361(12) . ? C223 H223 0.95 . ? C224 C225 1.398(10) . ? C224 H224 0.95 . ? C225 C226 1.376(11) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? P4 C411 1.807(8) . ? P4 C431 1.830(11) . ? P4 C421 1.871(7) . ? C411 C416 1.352(10) . ? C411 C412 1.405(12) . ? C412 C413 1.363(12) . ? C412 H412 0.95 . ? C413 C414 1.360(12) . ? C413 H413 0.95 . ? C414 C415 1.362(12) . ? C414 H414 0.95 . ? C415 C416 1.419(10) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C422 1.39 . ? C421 C426 1.413(14) . ? C422 C423 1.369(18) . ? C422 H422 0.95 . ? C422 H432 0.5356 . ? C423 C424 1.42(2) . ? C423 H423 0.95 . ? C424 C425 1.44(2) . ? C424 H424 0.95 . ? C425 C426 1.35(2) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C431 C436 1.39(3) . ? C431 C432 1.39 . ? C432 C433 1.45(3) . ? C432 H432 0.95 . ? C433 C434 1.34(3) . ? C433 H433 0.95 . ? C434 C435 1.38(3) . ? C434 H434 0.95 . ? C435 C436 1.39(3) . ? C435 H435 0.95 . ? C436 H436 0.95 . ? C02 H02A 0.99 . ? C02 H02B 0.99 . ? P5 C521 1.815(9) . ? P5 C511 1.827(8) . ? C511 C512 1.375(13) . ? C511 C516 1.377(12) . ? C512 C513 1.410(12) . ? C512 H512 0.95 . ? C513 C514 1.358(14) . ? C513 H513 0.95 . ? C514 C515 1.312(16) . ? C514 H514 0.95 . ? C515 C516 1.399(14) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C522 1.362(13) . ? C521 C526 1.416(15) . ? C522 C523 1.390(14) . ? C522 H522 0.95 . ? C523 C524 1.419(18) . ? C523 H523 0.95 . ? C524 C525 1.345(18) . ? C524 H524 0.95 . ? C525 C526 1.402(15) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? Cl11 C100 1.758(9) . ? Cl12 C100 1.708(10) . ? Cl13 C100 1.782(10) . ? Cl14 C100 1.664(14) . ? Cl15 C100 1.92(2) . ? C100 H10A 1 . ? C100 H10B 1 . ? Cl21 C200 1.771(11) . ? Cl22 C200 1.721(9) . ? Cl23 C200 1.678(10) . ? C200 H20A 1 . ? Cl31 C300 1.78(2) . ? Cl32 C300 1.79(2) . ? Cl32 H30B 1.5654 . ? Cl33 C300 1.63(2) . ? Cl34 C300 1.68(2) . ? Cl35 C300 1.72(2) . ? C300 H30A 1 . ? C300 H30B 1 . ? 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 C102 Co1 C101 102.8(3) . . ? C102 Co1 C1 107.4(3) . . ? C101 Co1 C1 139.0(3) . . ? C102 Co1 P1 96.4(3) . . ? C101 Co1 P1 109.6(3) . . ? C1 Co1 P1 94.0(2) . . ? C102 Co1 Co2 152.1(3) . . ? C101 Co1 Co2 93.75(19) . . ? C1 Co1 Co2 48.51(18) . . ? P1 Co1 Co2 98.91(6) . . ? C102 Co1 Co3 94.4(3) . . ? C101 Co1 Co3 101.2(2) . . ? C1 Co1 Co3 50.1(2) . . ? P1 Co1 Co3 144.07(7) . . ? Co2 Co1 Co3 60.07(4) . . ? C22 Co2 C21 103.3(3) . . ? C22 Co2 C1 98.9(3) . . ? C21 Co2 C1 143.2(3) . . ? C22 Co2 P2 95.8(3) . . ? C21 Co2 P2 105.6(2) . . ? C1 Co2 P2 100.9(2) . . ? C22 Co2 Co1 147.6(2) . . ? C21 Co2 Co1 104.7(2) . . ? C1 Co2 Co1 48.7(2) . . ? P2 Co2 Co1 92.20(6) . . ? C22 Co2 Co3 100.6(3) . . ? C21 Co2 Co3 96.6(2) . . ? C1 Co2 Co3 50.2(2) . . ? P2 Co2 Co3 148.48(6) . . ? Co1 Co2 Co3 60.20(4) . . ? C32 Co3 C33 98.3(4) . . ? C32 Co3 C31 101.6(3) . . ? C33 Co3 C31 104.0(3) . . ? C32 Co3 C1 106.1(3) . . ? C33 Co3 C1 102.6(3) . . ? C31 Co3 C1 138.0(3) . . ? C32 Co3 Co2 153.3(3) . . ? C33 Co3 Co2 94.9(3) . . ? C31 Co3 Co2 97.6(2) . . ? C1 Co3 Co2 48.12(18) . . ? C32 Co3 Co1 99.4(3) . . ? C33 Co3 Co1 149.4(3) . . ? C31 Co3 Co1 96.7(3) . . ? C1 Co3 Co1 48.3(2) . . ? Co2 Co3 Co1 59.72(4) . . ? C42 Co4 C41 101.2(3) . . ? C42 Co4 C14 100.6(3) . . ? C41 Co4 C14 144.5(3) . . ? C42 Co4 P4 95.0(3) . . ? C41 Co4 P4 106.8(3) . . ? C14 Co4 P4 98.9(2) . . ? C42 Co4 Co5 149.4(2) . . ? C41 Co4 Co5 104.3(2) . . ? C14 Co4 Co5 49.1(2) . . ? P4 Co4 Co5 93.62(7) . . ? C42 Co4 Co6 99.8(3) . . ? C41 Co4 Co6 98.1(3) . . ? C14 Co4 Co6 50.5(2) . . ? P4 Co4 Co6 147.96(7) . . ? Co5 Co4 Co6 60.21(4) . . ? C52 Co5 C51 103.6(3) . . ? C52 Co5 C14 108.4(3) . . ? C51 Co5 C14 138.7(3) . . ? C52 Co5 P5 95.1(3) . . ? C51 Co5 P5 105.0(3) . . ? C14 Co5 P5 97.4(2) . . ? C52 Co5 Co4 154.1(2) . . ? C51 Co5 Co4 93.5(2) . . ? C14 Co5 Co4 48.42(17) . . ? P5 Co5 Co4 99.08(7) . . ? C52 Co5 Co6 97.1(3) . . ? C51 Co5 Co6 100.8(3) . . ? C14 Co5 Co6 50.4(2) . . ? P5 Co5 Co6 147.82(7) . . ? Co4 Co5 Co6 60.18(4) . . ? C63 Co6 C62 100.4(4) . . ? C63 Co6 C61 101.2(3) . . ? C62 Co6 C61 104.5(4) . . ? C63 Co6 C14 105.2(3) . . ? C62 Co6 C14 99.9(4) . . ? C61 Co6 C14 139.8(3) . . ? C63 Co6 Co4 150.8(3) . . ? C62 Co6 Co4 96.3(3) . . ? C61 Co6 Co4 97.6(3) . . ? C14 Co6 Co4 47.90(18) . . ? C63 Co6 Co5 95.0(3) . . ? C62 Co6 Co5 147.8(3) . . ? C61 Co6 Co5 100.0(3) . . ? C14 Co6 Co5 48.4(2) . . ? Co4 Co6 Co5 59.61(4) . . ? O101 C101 Co1 176.1(6) . . ? O102 C102 Co1 179.2(9) . . ? O21 C21 Co2 175.6(7) . . ? O22 C22 Co2 177.3(8) . . ? O31 C31 Co3 179.4(8) . . ? O32 C32 Co3 178.9(10) . . ? O33 C33 Co3 178.2(7) . . ? O41 C41 Co4 177.1(9) . . ? O42 C42 Co4 178.1(9) . . ? O51 C51 Co5 175.6(7) . . ? O52 C52 Co5 177.9(8) . . ? O61 C61 Co6 177.7(8) . . ? O62 C62 Co6 175.7(9) . . ? O63 C63 Co6 177.8(7) . . ? C2 C1 Co2 134.7(5) . . ? C2 C1 Co1 133.2(5) . . ? Co2 C1 Co1 82.7(3) . . ? C2 C1 Co3 123.5(6) . . ? Co2 C1 Co3 81.7(3) . . ? Co1 C1 Co3 81.6(3) . . ? O2 C2 C3 120.1(6) . . ? O2 C2 C1 123.1(6) . . ? C3 C2 C1 116.7(6) . . ? C4 C3 C2 173.2(8) . . ? C3 C4 C5 175.6(7) . . ? C10 C5 C6 119.4(5) . . ? C10 C5 C4 122.1(6) . . ? C6 C5 C4 118.5(6) . . ? C7 C6 C5 119.7(6) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 121.3(6) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 118.9(5) . . ? C7 C8 C11 120.1(6) . . ? C9 C8 C11 121.0(6) . . ? C10 C9 C8 120.6(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C5 120.2(6) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C12 C11 C8 177.2(8) . . ? C11 C12 C13 175.3(8) . . ? O13 C13 C14 124.5(6) . . ? O13 C13 C12 119.2(6) . . ? C14 C13 C12 116.3(6) . . ? C13 C14 Co4 134.0(5) . . ? C13 C14 Co5 137.0(5) . . ? Co4 C14 Co5 82.5(3) . . ? C13 C14 Co6 119.9(5) . . ? Co4 C14 Co6 81.5(2) . . ? Co5 C14 Co6 81.1(3) . . ? C111 P1 C121 101.4(3) . . ? C111 P1 C02 104.0(3) . . ? C121 P1 C02 102.3(3) . . ? C111 P1 Co1 115.5(3) . . ? C121 P1 Co1 122.2(2) . . ? C02 P1 Co1 109.4(3) . . ? C112 C111 C116 118.6(6) . . ? C112 C111 P1 123.7(5) . . ? C116 C111 P1 117.2(6) . . ? C113 C112 C111 119.4(7) . . ? C113 C112 H112 120.3 . . ? C111 C112 H112 120.3 . . ? C114 C113 C112 121.9(7) . . ? C114 C113 H113 119.1 . . ? C112 C113 H113 119.1 . . ? C113 C114 C115 118.8(7) . . ? C113 C114 H114 120.6 . . ? C115 C114 H114 120.6 . . ? C116 C115 C114 120.3(8) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C115 C116 C111 120.8(8) . . ? C115 C116 H116 119.6 . . ? C111 C116 H116 119.6 . . ? C126 C121 C122 119.9(7) . . ? C126 C121 P1 118.6(6) . . ? C122 C121 P1 121.4(6) . . ? C123 C122 C121 119.8(7) . . ? C123 C122 H122 120.1 . . ? C121 C122 H122 120.1 . . ? C124 C123 C122 120.5(7) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C125 C124 C123 120.4(8) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.8 . . ? C124 C125 C126 119.6(8) . . ? C124 C125 H125 120.2 . . ? C126 C125 H125 120.2 . . ? C121 C126 C125 119.8(7) . . ? C121 C126 H126 120.1 . . ? C125 C126 H126 120.1 . . ? P4 C01 P5 109.2(4) . . ? P4 C01 H01A 109.8 . . ? P5 C01 H01A 109.8 . . ? P4 C01 H01B 109.8 . . ? P5 C01 H01B 109.8 . . ? H01A C01 H01B 108.3 . . ? C221 P2 C211 103.1(3) . . ? C221 P2 C02 102.8(3) . . ? C211 P2 C02 101.9(3) . . ? C221 P2 Co2 121.4(2) . . ? C211 P2 Co2 115.6(3) . . ? C02 P2 Co2 109.6(3) . . ? C216 C211 C212 118.3(6) . . ? C216 C211 P2 122.7(6) . . ? C212 C211 P2 118.6(5) . . ? C213 C212 C211 120.6(7) . . ? C213 C212 H212 119.7 . . ? C211 C212 H212 119.7 . . ? C214 C213 C212 119.8(8) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C213 C214 C215 121.4(7) . . ? C213 C214 H214 119.3 . . ? C215 C214 H214 119.3 . . ? C214 C215 C216 119.4(7) . . ? C214 C215 H215 120.3 . . ? C216 C215 H215 120.3 . . ? C211 C216 C215 120.5(8) . . ? C211 C216 H216 119.7 . . ? C215 C216 H216 119.7 . . ? C222 C221 C226 118.6(7) . . ? C222 C221 P2 121.2(6) . . ? C226 C221 P2 120.2(5) . . ? C223 C222 C221 119.5(7) . . ? C223 C222 H222 120.2 . . ? C221 C222 H222 120.2 . . ? C224 C223 C222 121.3(7) . . ? C224 C223 H223 119.4 . . ? C222 C223 H223 119.4 . . ? C223 C224 C225 120.6(8) . . ? C223 C224 H224 119.7 . . ? C225 C224 H224 119.7 . . ? C226 C225 C224 118.8(7) . . ? C226 C225 H225 120.6 . . ? C224 C225 H225 120.6 . . ? C225 C226 C221 121.3(7) . . ? C225 C226 H226 119.3 . . ? C221 C226 H226 119.3 . . ? C411 P4 C01 103.8(4) . . ? C411 P4 C431 108.1(5) . . ? C01 P4 C431 108.3(4) . . ? C411 P4 C421 103.1(4) . . ? C01 P4 C421 96.4(3) . . ? C411 P4 Co4 112.2(4) . . ? C01 P4 Co4 110.1(3) . . ? C431 P4 Co4 113.9(4) . . ? C421 P4 Co4 128.1(2) . . ? C416 C411 C412 119.0(7) . . ? C416 C411 P4 119.6(6) . . ? C412 C411 P4 121.2(6) . . ? C413 C412 C411 120.2(8) . . ? C413 C412 H412 119.9 . . ? C411 C412 H412 119.9 . . ? C414 C413 C412 120.2(9) . . ? C414 C413 H413 119.9 . . ? C412 C413 H413 119.9 . . ? C413 C414 C415 121.5(8) . . ? C413 C414 H414 119.2 . . ? C415 C414 H414 119.2 . . ? C414 C415 C416 118.3(7) . . ? C414 C415 H415 120.8 . . ? C416 C415 H415 120.8 . . ? C411 C416 C415 120.6(7) . . ? C411 C416 H416 119.7 . . ? C415 C416 H416 119.7 . . ? C422 C421 C426 119.4(6) . . ? C422 C421 P4 122.9(2) . . ? C426 C421 P4 117.4(6) . . ? C423 C422 C421 119.0(8) . . ? C423 C422 H422 119.9 . . ? C421 C422 H422 121.1 . . ? C422 C423 C424 122.7(14) . . ? C422 C423 H423 118.7 . . ? C424 C423 H423 118.7 . . ? C423 C424 C425 117.6(15) . . ? C423 C424 H424 121.2 . . ? C425 C424 H424 121.2 . . ? C426 C425 C424 118.7(15) . . ? C426 C425 H425 120.6 . . ? C424 C425 H425 120.6 . . ? C425 C426 C421 122.6(12) . . ? C425 C426 H426 118.7 . . ? C421 C426 H426 118.7 . . ? C436 C431 C432 123.3(11) . . ? C436 C431 P4 123.5(12) . . ? C432 C431 P4 112.7(4) . . ? C431 C432 C433 119.5(12) . . ? C431 C432 H432 117.9 . . ? C433 C432 H432 116.7 . . ? C434 C433 C432 111(2) . . ? C434 C433 H433 124.5 . . ? C432 C433 H433 124.5 . . ? C433 C434 H434 113.7 . . ? C435 C434 H434 113.7 . . ? C434 C435 C436 114(2) . . ? C434 C435 H435 122.9 . . ? C436 C435 H435 122.9 . . ? C435 C436 C431 119(2) . . ? C435 C436 H436 120.7 . . ? C431 C436 H436 120.7 . . ? P2 C02 P1 106.9(3) . . ? P2 C02 H02A 110.3 . . ? P1 C02 H02A 110.3 . . ? P2 C02 H02B 110.3 . . ? P1 C02 H02B 110.3 . . ? H02A C02 H02B 108.6 . . ? C521 P5 C01 108.4(4) . . ? C521 P5 C511 100.7(4) . . ? C01 P5 C511 104.6(4) . . ? C521 P5 Co5 117.8(3) . . ? C01 P5 Co5 107.8(3) . . ? C511 P5 Co5 116.4(3) . . ? C512 C511 C516 117.3(8) . . ? C512 C511 P5 123.9(6) . . ? C516 C511 P5 118.7(7) . . ? C511 C512 C513 120.7(9) . . ? C511 C512 H512 119.6 . . ? C513 C512 H512 119.6 . . ? C514 C513 C512 119.2(10) . . ? C514 C513 H513 120.4 . . ? C512 C513 H513 120.4 . . ? C515 C514 C513 121.0(9) . . ? C515 C514 H514 119.5 . . ? C513 C514 H514 119.5 . . ? C514 C515 C516 120.8(10) . . ? C514 C515 H515 119.6 . . ? C516 C515 H515 119.6 . . ? C511 C516 C515 120.7(10) . . ? C511 C516 H516 119.6 . . ? C515 C516 H516 119.6 . . ? C522 C521 C526 119.9(9) . . ? C522 C521 P5 120.1(8) . . ? C526 C521 P5 119.7(7) . . ? C521 C522 C523 121.1(10) . . ? C521 C522 H522 119.5 . . ? C523 C522 H522 119.5 . . ? C522 C523 C524 118.2(11) . . ? C522 C523 H523 120.9 . . ? C524 C523 H523 120.9 . . ? C525 C524 C523 121.5(11) . . ? C525 C524 H524 119.2 . . ? C523 C524 H524 119.2 . . ? C524 C525 C526 119.8(13) . . ? C524 C525 H525 120.1 . . ? C526 C525 H525 120.1 . . ? C525 C526 C521 119.1(11) . . ? C525 C526 H526 120.4 . . ? C521 C526 H526 120.4 . . ? Cl14 C100 Cl11 122.3(7) . . ? Cl12 C100 Cl11 111.3(6) . . ? Cl12 C100 Cl13 110.4(5) . . ? Cl11 C100 Cl13 107.4(5) . . ? Cl14 C100 Cl15 98.0(10) . . ? Cl11 C100 Cl15 94.9(10) . . ? Cl12 C100 H10A 109.2 . . ? Cl11 C100 H10A 109.2 . . ? Cl13 C100 H10A 109.2 . . ? Cl14 C100 H10B 113 . . ? Cl11 C100 H10B 112.8 . . ? Cl15 C100 H10B 112.7 . . ? Cl23 C200 Cl22 113.0(6) . . ? Cl23 C200 Cl21 115.2(6) . . ? Cl22 C200 Cl21 108.7(5) . . ? Cl23 C200 H20A 106.4 . . ? Cl22 C200 H20A 106.4 . . ? Cl21 C200 H20A 106.4 . . ? Cl34 C300 Cl35 114.4(14) . . ? Cl33 C300 Cl31 108.8(11) . . ? Cl34 C300 Cl31 114.5(13) . . ? Cl35 C300 Cl31 110.3(13) . . ? Cl33 C300 Cl32 112.6(13) . . ? Cl31 C300 Cl32 113.3(13) . . ? Cl33 C300 H30A 107.3 . . ? Cl31 C300 H30A 107.3 . . ? Cl32 C300 H30A 107.3 . . ? Cl34 C300 H30B 105.6 . . ? Cl35 C300 H30B 105.5 . . ? Cl31 C300 H30B 105.6 . . ? #===END # Attachment '5.br1417.cif' data_br1417 _database_code_depnum_ccdc_archive 'CCDC 754941' #TrackingRef '5.br1417.cif' _audit_creation_date 2008-05-15T12:07:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C69 H44 Co6 O15 P4' _chemical_formula_moiety 'C69 H44 Co6 O15 P4' _chemical_formula_weight 1590.5 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7940(10) _cell_length_b 12.1450(10) _cell_length_c 24.9760(10) _cell_angle_alpha 87.249(6) _cell_angle_beta 78.279(6) _cell_angle_gamma 75.971(10) _cell_volume 3398.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6086 _cell_measurement_theta_min 2.9917 _cell_measurement_theta_max 27.2824 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.63387 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0016318396 _diffrn_orient_matrix_ub_12 -0.0009871089 _diffrn_orient_matrix_ub_13 0.0290722299 _diffrn_orient_matrix_ub_21 0.0636598631 _diffrn_orient_matrix_ub_22 -0.0224121996 _diffrn_orient_matrix_ub_23 -0.0049547049 _diffrn_orient_matrix_ub_31 0.0088658481 _diffrn_orient_matrix_ub_32 0.0568088582 _diffrn_orient_matrix_ub_33 -0.001463804 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.1071 _diffrn_reflns_number 10982 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.92 _diffrn_measured_fraction_theta_max 0.92 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 10982 _reflns_number_gt 7150 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0000P)^2^+49.8644P] 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_number_reflns 10982 _refine_ls_number_parameters 823 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1436 _refine_ls_R_factor_gt 0.0967 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.167 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.063 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.14 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 1.07284(13) 0.18872(12) 0.15478(5) 0.0251(3) Uani 1 1 d . . . Co2 Co 1.12861(14) 0.33861(12) 0.08927(5) 0.0276(4) Uani 1 1 d . . . Co3 Co 0.92053(14) 0.31628(12) 0.10995(5) 0.0283(4) Uani 1 1 d . . . Co4 Co 0.71517(13) 0.67245(12) 0.33812(5) 0.0244(3) Uani 1 1 d . . . Co5 Co 0.83827(13) 0.60085(11) 0.40725(5) 0.0211(3) Uani 1 1 d . . . Co6 Co 0.75812(13) 0.46785(12) 0.36079(5) 0.0243(3) Uani 1 1 d . . . C11 C 1.1013(10) 0.0624(10) 0.1130(4) 0.031(3) Uani 1 1 d . . . O11 O 1.1131(7) -0.0131(7) 0.0858(3) 0.043(2) Uani 1 1 d . . . C12 C 0.9804(12) 0.1616(9) 0.2165(4) 0.037(3) Uani 1 1 d . . . O12 O 0.9221(7) 0.1493(7) 0.2585(3) 0.043(2) Uani 1 1 d . . . C21 C 1.1985(10) 0.2425(10) 0.0328(4) 0.030(3) Uani 1 1 d . . . O21 O 1.2409(7) 0.1793(7) -0.0027(3) 0.044(2) Uani 1 1 d . . . C22 C 1.0972(10) 0.4704(9) 0.0561(4) 0.029(3) Uani 1 1 d . . . O22 O 1.0718(8) 0.5589(7) 0.0351(3) 0.047(2) Uani 1 1 d . . . C31 C 0.9381(10) 0.2337(9) 0.0486(4) 0.033(3) Uani 1 1 d . . . O31 O 0.9518(7) 0.1806(7) 0.0103(3) 0.047(2) Uani 1 1 d . . . C32 C 0.7992(11) 0.2726(10) 0.1527(4) 0.032(3) Uani 1 1 d . . . O32 O 0.7180(8) 0.2430(7) 0.1774(3) 0.045(2) Uani 1 1 d . . . C33 C 0.8416(12) 0.4563(11) 0.0946(4) 0.039(3) Uani 1 1 d . . . O33 O 0.7867(9) 0.5436(8) 0.0861(4) 0.059(3) Uani 1 1 d . . . C41 C 0.5971(10) 0.7310(10) 0.3920(5) 0.0362(16) Uani 1 1 d . . . O41 O 0.5175(6) 0.7690(6) 0.4276(3) 0.0362(16) Uani 1 1 d . . . C42 C 0.6403(13) 0.6699(12) 0.2841(5) 0.055(2) Uani 1 1 d . . . O42 O 0.5848(8) 0.6724(8) 0.2507(3) 0.055(2) Uani 1 1 d . . . C51 C 0.7419(9) 0.6202(8) 0.4748(4) 0.023(2) Uani 1 1 d . . . O51 O 0.6845(7) 0.6265(6) 0.5179(3) 0.040(2) Uani 1 1 d . . . C52 C 0.9625(10) 0.5039(9) 0.4226(4) 0.023(2) Uani 1 1 d . . . O52 O 1.0493(7) 0.4412(6) 0.4304(3) 0.0340(18) Uani 1 1 d . . . C61 C 0.6332(10) 0.4598(9) 0.4135(4) 0.031(3) Uani 1 1 d . . . O61 O 0.5557(8) 0.4498(7) 0.4478(3) 0.049(2) Uani 1 1 d . . . C62 C 0.7133(10) 0.4292(10) 0.3013(4) 0.034(3) Uani 1 1 d . . . O62 O 0.6854(9) 0.4034(8) 0.2635(3) 0.062(3) Uani 1 1 d . . . C63 C 0.8577(9) 0.3365(10) 0.3716(4) 0.029(3) Uani 1 1 d . . . O63 O 0.9140(8) 0.2477(7) 0.3799(3) 0.048(2) Uani 1 1 d . . . P1 P 1.2333(3) 0.1622(2) 0.19023(10) 0.0259(6) Uani 1 1 d . . . C111 C 1.2126(9) 0.1317(9) 0.2639(4) 0.0230(16) Uani 1 1 d . . . C112 C 1.1979(9) 0.2152(10) 0.3026(4) 0.028(3) Uani 1 1 d . . . H112 H 1.2008 0.2904 0.2911 0.034 Uiso 1 1 calc R . . C113 C 1.1790(9) 0.1893(10) 0.3583(4) 0.028(3) Uani 1 1 d . . . H113 H 1.17 0.2463 0.3845 0.034 Uiso 1 1 calc R . . C114 C 1.1734(10) 0.0789(10) 0.3752(4) 0.037(3) Uani 1 1 d . . . H114 H 1.1624 0.0606 0.413 0.045 Uiso 1 1 calc R . . C115 C 1.1838(10) -0.0027(10) 0.3374(4) 0.037(3) Uani 1 1 d . . . H115 H 1.1775 -0.0768 0.3494 0.044 Uiso 1 1 calc R . . C116 C 1.2034(10) 0.0216(9) 0.2817(4) 0.035(3) Uani 1 1 d . . . H116 H 1.2106 -0.0357 0.2558 0.042 Uiso 1 1 calc R . . C121 C 1.3625(9) 0.0499(9) 0.1619(4) 0.0230(16) Uani 1 1 d . . . C122 C 1.4494(10) 0.0009(10) 0.1926(5) 0.037(3) Uani 1 1 d . . . H122 H 1.4406 0.0258 0.229 0.044 Uiso 1 1 calc R . . C123 C 1.5463(11) -0.0818(11) 0.1708(5) 0.045(3) Uani 1 1 d . . . H123 H 1.6033 -0.115 0.1924 0.054 Uiso 1 1 calc R . . C124 C 1.5628(11) -0.1181(11) 0.1177(5) 0.043(3) Uani 1 1 d . . . H124 H 1.6303 -0.1763 0.103 0.052 Uiso 1 1 calc R . . C125 C 1.4804(10) -0.0692(10) 0.0858(5) 0.039(3) Uani 1 1 d . . . H125 H 1.4922 -0.0918 0.0488 0.047 Uiso 1 1 calc R . . C126 C 1.3809(10) 0.0128(10) 0.1085(4) 0.035(3) Uani 1 1 d . . . H126 H 1.3234 0.0446 0.0869 0.042 Uiso 1 1 calc R . . C10 C 1.2887(10) 0.2898(9) 0.1861(4) 0.030(3) Uani 1 1 d . . . H10A H 1.3716 0.27 0.1921 0.036 Uiso 1 1 calc R . . H10B H 1.2395 0.3431 0.2154 0.036 Uiso 1 1 calc R . . P2 P 1.2849(3) 0.3600(2) 0.11946(10) 0.0280(7) Uani 1 1 d . . . C211 C 1.2962(11) 0.5038(10) 0.1376(4) 0.034(3) Uani 1 1 d . . . C212 C 1.1969(13) 0.5921(10) 0.1455(4) 0.043(3) Uani 1 1 d . . . H212 H 1.1226 0.5819 0.1401 0.052 Uiso 1 1 calc R . . C213 C 1.2071(14) 0.7000(11) 0.1620(5) 0.056(4) Uani 1 1 d . . . H213 H 1.1393 0.7623 0.1676 0.067 Uiso 1 1 calc R . . C214 C 1.3127(13) 0.7129(13) 0.1696(5) 0.051(4) Uani 1 1 d . . . H214 H 1.3181 0.7851 0.1804 0.061 Uiso 1 1 calc R . . C215 C 1.4131(15) 0.6253(12) 0.1624(5) 0.054(4) Uani 1 1 d . . . H215 H 1.4868 0.6365 0.168 0.065 Uiso 1 1 calc R . . C216 C 1.4041(12) 0.5168(11) 0.1460(4) 0.045(3) Uani 1 1 d . . . H216 H 1.4718 0.4545 0.1411 0.053 Uiso 1 1 calc R . . C221 C 1.4291(9) 0.3070(9) 0.0754(4) 0.028(3) Uani 1 1 d . . . C222 C 1.5228(11) 0.2252(12) 0.0903(4) 0.047(4) Uani 1 1 d . . . H222 H 1.5128 0.1929 0.1259 0.057 Uiso 1 1 calc R . . C223 C 1.6288(12) 0.1910(12) 0.0544(5) 0.051(4) Uani 1 1 d . . . H223 H 1.6916 0.1345 0.0649 0.061 Uiso 1 1 calc R . . C224 C 1.6451(12) 0.2395(12) 0.0020(5) 0.047(3) Uani 1 1 d . . . H224 H 1.7188 0.2159 -0.0229 0.056 Uiso 1 1 calc R . . C225 C 1.5532(12) 0.3219(11) -0.0132(4) 0.043(3) Uani 1 1 d . . . H225 H 1.5646 0.3556 -0.0484 0.052 Uiso 1 1 calc R . . C226 C 1.4457(11) 0.3549(10) 0.0224(4) 0.039(3) Uani 1 1 d . . . H226 H 1.3824 0.41 0.0115 0.046 Uiso 1 1 calc R . . C1 C 1.0192(9) 0.3481(9) 0.1556(4) 0.027(2) Uani 1 1 d . . . C2 C 0.9938(10) 0.4180(8) 0.2031(4) 0.025(2) Uani 1 1 d . . . C3 C 0.9770(10) 0.4713(9) 0.2442(4) 0.028(2) Uani 1 1 d . . . C4 C 0.9759(10) 0.5316(9) 0.2933(4) 0.0243(17) Uani 1 1 d . . . O4 O 1.0705(7) 0.5511(7) 0.3003(3) 0.045(2) Uani 1 1 d . . . C5 C 0.8606(9) 0.5625(9) 0.3330(4) 0.0243(17) Uani 1 1 d . . . P4 P 0.7845(2) 0.8213(2) 0.30902(10) 0.0215(6) Uani 1 1 d . . . C411 C 0.8216(9) 0.8415(9) 0.2349(4) 0.026(2) Uani 1 1 d . . . C412 C 0.8561(11) 0.7447(10) 0.2005(4) 0.039(3) Uani 1 1 d . . . H412 H 0.8594 0.671 0.2158 0.046 Uiso 1 1 calc R . . C413 C 0.8853(11) 0.7591(10) 0.1437(4) 0.040(3) Uani 1 1 d . . . H413 H 0.9086 0.6946 0.1203 0.049 Uiso 1 1 calc R . . C414 C 0.8806(10) 0.8654(10) 0.1215(4) 0.033(3) Uani 1 1 d . . . H414 H 0.9005 0.8743 0.083 0.039 Uiso 1 1 calc R . . C415 C 0.8465(10) 0.9600(9) 0.1555(4) 0.033(3) Uani 1 1 d . . . H415 H 0.8436 1.0334 0.1401 0.04 Uiso 1 1 calc R . . C416 C 0.8169(9) 0.9484(8) 0.2115(4) 0.024(2) Uani 1 1 d . . . H416 H 0.7932 1.0138 0.2343 0.028 Uiso 1 1 calc R . . C421 C 0.6881(9) 0.9585(8) 0.3325(3) 0.021(2) Uani 1 1 d . . . C422 C 0.7271(10) 1.0489(9) 0.3503(4) 0.027(2) Uani 1 1 d . . . H422 H 0.8094 1.0409 0.3501 0.032 Uiso 1 1 calc R . . C423 C 0.6471(11) 1.1479(10) 0.3678(4) 0.037(3) Uani 1 1 d . . . H423 H 0.6738 1.2065 0.3816 0.044 Uiso 1 1 calc R . . C424 C 0.5303(13) 1.1643(10) 0.3659(5) 0.047(3) Uani 1 1 d . . . H424 H 0.476 1.2341 0.378 0.057 Uiso 1 1 calc R . . C425 C 0.4902(12) 1.0796(11) 0.3462(5) 0.052(3) Uani 1 1 d . . . H425 H 0.4088 1.0919 0.3438 0.062 Uiso 1 1 calc R . . C426 C 0.5687(10) 0.9762(10) 0.3301(4) 0.035(3) Uani 1 1 d . . . H426 H 0.5404 0.9174 0.3173 0.042 Uiso 1 1 calc R . . C20 C 0.9257(9) 0.8098(8) 0.3311(4) 0.023(2) Uani 1 1 d . . . H20A H 0.9917 0.7614 0.3052 0.028 Uiso 1 1 calc R . . H20B H 0.942 0.886 0.3315 0.028 Uiso 1 1 calc R . . P5 P 0.9176(2) 0.7482(2) 0.39930(10) 0.0216(6) Uani 1 1 d . . . C511 C 1.0703(9) 0.7152(8) 0.4100(4) 0.021(2) Uani 1 1 d . . . C512 C 1.1693(11) 0.6951(9) 0.3681(4) 0.035(3) Uani 1 1 d . . . H512 H 1.1596 0.707 0.3312 0.042 Uiso 1 1 calc R . . C513 C 1.2834(10) 0.6573(9) 0.3794(5) 0.036(3) Uani 1 1 d . . . H513 H 1.3514 0.6432 0.3505 0.043 Uiso 1 1 calc R . . C514 C 1.2960(10) 0.6407(9) 0.4331(5) 0.037(3) Uani 1 1 d . . . H514 H 1.3735 0.6151 0.4411 0.045 Uiso 1 1 calc R . . C515 C 1.1991(10) 0.6603(9) 0.4749(4) 0.030(3) Uani 1 1 d . . . H515 H 1.21 0.6481 0.5115 0.035 Uiso 1 1 calc R . . C516 C 1.0861(11) 0.6975(8) 0.4646(4) 0.030(3) Uani 1 1 d . . . H516 H 1.019 0.7112 0.4939 0.036 Uiso 1 1 calc R . . C521 C 0.8464(9) 0.8717(8) 0.4437(3) 0.019(2) Uani 1 1 d . . . C522 C 0.9091(9) 0.9548(8) 0.4468(4) 0.022(2) Uani 1 1 d . . . H522 H 0.9898 0.9432 0.4282 0.026 Uiso 1 1 calc R . . C523 C 0.8554(10) 1.0532(9) 0.4765(4) 0.029(3) Uani 1 1 d . . . H523 H 0.8989 1.1088 0.4784 0.035 Uiso 1 1 calc R . . C524 C 0.7375(10) 1.0703(9) 0.5035(4) 0.027(2) Uani 1 1 d . . . H524 H 0.6997 1.1385 0.5234 0.033 Uiso 1 1 calc R . . C525 C 0.6752(9) 0.9891(9) 0.5015(4) 0.026(2) Uani 1 1 d . . . H525 H 0.5952 1.0001 0.5209 0.031 Uiso 1 1 calc R . . C526 C 0.7296(9) 0.8906(9) 0.4710(4) 0.025(2) Uani 1 1 d . . . H526 H 0.6855 0.8355 0.469 0.03 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0335(9) 0.0291(8) 0.0157(7) -0.0026(6) -0.0072(6) -0.0107(7) Co2 0.0401(10) 0.0344(9) 0.0112(7) -0.0021(6) -0.0076(6) -0.0121(7) Co3 0.0382(10) 0.0320(9) 0.0164(7) -0.0049(6) -0.0081(6) -0.0083(7) Co4 0.0273(9) 0.0296(8) 0.0199(7) -0.0025(6) -0.0114(6) -0.0078(7) Co5 0.0273(8) 0.0249(8) 0.0140(6) -0.0022(5) -0.0088(6) -0.0076(6) Co6 0.0291(9) 0.0284(8) 0.0194(7) -0.0047(6) -0.0102(6) -0.0092(7) C11 0.030(7) 0.048(8) 0.021(5) 0.002(5) -0.012(5) -0.012(6) O11 0.044(6) 0.049(5) 0.038(5) -0.018(4) -0.004(4) -0.016(4) C12 0.066(9) 0.020(6) 0.026(6) -0.001(5) -0.007(6) -0.014(6) O12 0.054(6) 0.058(6) 0.026(4) 0.000(4) -0.005(4) -0.034(5) C21 0.027(7) 0.047(7) 0.024(6) 0.001(5) -0.013(5) -0.018(6) O21 0.049(6) 0.064(6) 0.024(4) -0.019(4) -0.004(4) -0.025(5) C22 0.040(7) 0.029(6) 0.019(5) 0.001(5) -0.008(5) -0.008(5) O22 0.075(7) 0.042(5) 0.023(4) 0.000(4) -0.016(4) -0.007(5) C31 0.037(7) 0.028(6) 0.035(6) 0.003(5) -0.008(5) -0.009(5) O31 0.049(6) 0.071(6) 0.027(4) -0.017(4) -0.013(4) -0.016(5) C32 0.035(7) 0.041(7) 0.024(6) -0.009(5) -0.017(5) -0.005(6) O32 0.049(6) 0.058(6) 0.038(5) -0.013(4) -0.006(4) -0.030(5) C33 0.055(9) 0.041(8) 0.020(6) 0.005(5) -0.010(5) -0.008(7) O33 0.067(7) 0.042(6) 0.066(6) -0.003(5) -0.026(5) 0.004(5) C41 0.018(4) 0.044(4) 0.047(4) -0.004(3) -0.009(3) -0.005(3) O41 0.018(4) 0.044(4) 0.047(4) -0.004(3) -0.009(3) -0.005(3) C42 0.059(5) 0.066(5) 0.062(5) 0.008(4) -0.043(4) -0.032(4) O42 0.059(5) 0.066(5) 0.062(5) 0.008(4) -0.043(4) -0.032(4) C51 0.021(6) 0.020(6) 0.032(6) -0.004(4) -0.009(5) -0.010(5) O51 0.047(5) 0.041(5) 0.027(4) -0.003(4) 0.003(4) -0.008(4) C52 0.027(7) 0.031(6) 0.013(5) -0.001(4) -0.012(4) -0.004(5) O52 0.032(5) 0.039(5) 0.036(4) -0.004(4) -0.018(4) -0.008(4) C61 0.025(7) 0.040(7) 0.027(6) -0.004(5) -0.011(5) 0.000(5) O61 0.042(6) 0.052(6) 0.050(5) -0.004(4) 0.000(4) -0.012(5) C62 0.034(7) 0.040(7) 0.041(7) -0.002(5) -0.020(5) -0.020(6) O62 0.105(8) 0.063(6) 0.037(5) -0.010(4) -0.036(5) -0.032(6) C63 0.011(6) 0.042(7) 0.030(6) -0.001(5) -0.006(5) -0.001(5) O63 0.037(6) 0.042(5) 0.064(6) 0.003(4) -0.011(4) -0.007(4) P1 0.0310(17) 0.0366(17) 0.0121(12) -0.0006(11) -0.0056(11) -0.0106(13) C111 0.020(4) 0.032(4) 0.016(3) 0.002(3) -0.003(3) -0.004(3) C112 0.020(6) 0.047(7) 0.018(5) 0.001(5) -0.006(4) -0.008(5) C113 0.018(6) 0.048(7) 0.021(5) 0.001(5) -0.008(4) -0.010(5) C114 0.032(7) 0.062(9) 0.016(5) 0.009(5) -0.008(5) -0.006(6) C115 0.034(7) 0.044(7) 0.034(6) 0.012(5) -0.009(5) -0.013(6) C116 0.044(8) 0.029(7) 0.032(6) 0.002(5) -0.007(5) -0.006(6) C121 0.020(4) 0.032(4) 0.016(3) 0.002(3) -0.003(3) -0.004(3) C122 0.033(7) 0.042(7) 0.037(6) 0.000(5) -0.005(5) -0.014(6) C123 0.039(8) 0.062(9) 0.036(7) 0.004(6) -0.012(6) -0.013(7) C124 0.027(7) 0.061(9) 0.040(7) -0.012(6) -0.006(6) -0.005(6) C125 0.028(7) 0.054(8) 0.034(6) -0.008(6) -0.006(5) -0.009(6) C126 0.030(7) 0.047(8) 0.032(6) 0.004(5) -0.017(5) -0.008(6) C10 0.039(7) 0.045(7) 0.013(5) 0.001(5) -0.009(5) -0.022(6) P2 0.0392(19) 0.0394(18) 0.0125(12) 0.0009(11) -0.0099(12) -0.0193(14) C211 0.053(8) 0.046(8) 0.016(5) 0.002(5) -0.021(5) -0.023(7) C212 0.064(10) 0.038(7) 0.032(6) 0.002(5) -0.011(6) -0.020(7) C213 0.088(12) 0.052(9) 0.032(7) -0.011(6) -0.005(7) -0.031(8) C214 0.064(10) 0.074(11) 0.033(7) -0.004(7) -0.015(7) -0.045(9) C215 0.085(12) 0.063(10) 0.035(7) 0.006(6) -0.030(7) -0.045(9) C216 0.067(10) 0.050(8) 0.028(6) 0.013(5) -0.025(6) -0.024(7) C221 0.024(6) 0.040(7) 0.022(5) -0.005(5) -0.008(5) -0.009(5) C222 0.040(8) 0.086(11) 0.023(6) 0.000(6) -0.003(6) -0.028(8) C223 0.050(9) 0.072(10) 0.041(7) 0.001(7) -0.015(7) -0.028(8) C224 0.045(9) 0.070(10) 0.029(6) -0.013(6) -0.004(6) -0.020(7) C225 0.061(9) 0.051(8) 0.020(6) 0.009(5) -0.006(6) -0.023(7) C226 0.047(8) 0.049(8) 0.020(6) -0.003(5) -0.004(5) -0.014(6) C1 0.027(6) 0.031(6) 0.024(5) 0.001(4) -0.014(5) -0.003(5) C2 0.038(7) 0.027(6) 0.012(5) 0.000(4) -0.007(4) -0.012(5) C3 0.032(7) 0.035(6) 0.018(5) 0.002(5) -0.010(5) -0.007(5) C4 0.031(5) 0.033(4) 0.012(3) -0.003(3) -0.014(3) -0.005(4) O4 0.043(5) 0.069(6) 0.026(4) -0.020(4) -0.007(4) -0.018(5) C5 0.031(5) 0.033(4) 0.012(3) -0.003(3) -0.014(3) -0.005(4) P4 0.0221(16) 0.0268(15) 0.0174(13) -0.0013(11) -0.0085(11) -0.0049(12) C411 0.029(6) 0.027(6) 0.022(5) -0.001(4) -0.009(5) -0.005(5) C412 0.060(9) 0.030(7) 0.026(6) -0.005(5) -0.017(6) -0.005(6) C413 0.052(9) 0.046(8) 0.023(6) -0.007(5) -0.007(5) -0.011(6) C414 0.033(7) 0.048(8) 0.019(5) 0.000(5) -0.007(5) -0.011(6) C415 0.049(8) 0.032(7) 0.025(6) 0.007(5) -0.014(5) -0.016(6) C416 0.036(7) 0.023(6) 0.020(5) -0.003(4) -0.010(5) -0.018(5) C421 0.020(6) 0.026(6) 0.012(5) -0.004(4) -0.005(4) 0.004(4) C422 0.034(7) 0.032(6) 0.020(5) 0.002(4) -0.016(5) -0.009(5) C423 0.045(8) 0.033(7) 0.028(6) 0.003(5) -0.011(6) -0.001(6) C424 0.064(10) 0.025(7) 0.044(7) -0.001(5) -0.007(7) 0.002(6) C425 0.040(9) 0.050(9) 0.065(9) -0.005(7) -0.012(7) -0.008(7) C426 0.036(7) 0.037(7) 0.037(6) -0.003(5) -0.018(5) -0.011(6) C20 0.031(6) 0.017(5) 0.016(5) -0.004(4) -0.008(4) 0.009(5) P5 0.0296(17) 0.0233(15) 0.0140(12) -0.0021(10) -0.0077(11) -0.0072(12) C511 0.018(6) 0.024(6) 0.029(5) -0.001(4) -0.008(4) -0.014(5) C512 0.043(8) 0.034(7) 0.032(6) 0.002(5) -0.013(6) -0.012(6) C513 0.026(7) 0.036(7) 0.044(7) 0.004(5) -0.005(5) -0.005(5) C514 0.027(7) 0.028(7) 0.064(8) -0.002(6) -0.023(6) -0.006(5) C515 0.023(6) 0.041(7) 0.033(6) 0.002(5) -0.019(5) -0.013(5) C516 0.048(8) 0.014(5) 0.030(6) 0.000(4) -0.014(5) -0.006(5) C521 0.032(6) 0.018(5) 0.014(5) 0.003(4) -0.016(4) -0.011(5) C522 0.026(6) 0.022(6) 0.023(5) 0.004(4) -0.011(4) -0.009(5) C523 0.044(8) 0.025(6) 0.030(6) -0.002(5) -0.021(5) -0.017(5) C524 0.031(7) 0.030(6) 0.019(5) -0.005(4) -0.010(5) 0.003(5) C525 0.019(6) 0.035(6) 0.026(5) -0.007(5) -0.010(4) -0.005(5) C526 0.025(6) 0.034(6) 0.023(5) 0.003(4) -0.013(5) -0.013(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.765(12) . ? Co1 C11 1.822(11) . ? Co1 C1 1.884(10) . ? Co1 P1 2.197(3) . ? Co1 Co3 2.486(2) . ? Co1 Co2 2.506(2) . ? Co2 C22 1.759(11) . ? Co2 C21 1.803(11) . ? Co2 C1 1.872(10) . ? Co2 P2 2.203(3) . ? Co2 Co3 2.481(2) . ? Co3 C32 1.778(12) . ? Co3 C33 1.794(13) . ? Co3 C31 1.821(11) . ? Co3 C1 1.899(10) . ? Co4 C42 1.762(12) . ? Co4 C41 1.762(11) . ? Co4 C5 1.887(11) . ? Co4 P4 2.193(3) . ? Co4 Co5 2.4711(19) . ? Co4 Co6 2.474(2) . ? Co5 C52 1.740(11) . ? Co5 C51 1.824(10) . ? Co5 C5 1.883(9) . ? Co5 P5 2.195(3) . ? Co5 Co6 2.4929(18) . ? Co6 C63 1.783(12) . ? Co6 C61 1.784(12) . ? Co6 C62 1.792(10) . ? Co6 C5 1.876(10) . ? C11 O11 1.130(12) . ? C12 O12 1.158(12) . ? C21 O21 1.151(12) . ? C22 O22 1.172(12) . ? C31 O31 1.140(12) . ? C32 O32 1.154(12) . ? C33 O33 1.136(13) . ? C41 O41 1.173(12) . ? C42 O42 1.155(13) . ? C51 O51 1.144(11) . ? C52 O52 1.165(12) . ? C61 O61 1.144(12) . ? C62 O62 1.143(12) . ? C63 O63 1.155(12) . ? P1 C10 1.813(10) . ? P1 C121 1.825(10) . ? P1 C111 1.839(9) . ? C111 C112 1.390(13) . ? C111 C116 1.411(14) . ? C112 C113 1.394(13) . ? C112 H112 0.95 . ? C113 C114 1.399(15) . ? C113 H113 0.95 . ? C114 C115 1.368(15) . ? C114 H114 0.95 . ? C115 C116 1.393(14) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.387(13) . ? C121 C122 1.404(15) . ? C122 C123 1.362(16) . ? C122 H122 0.95 . ? C123 C124 1.378(15) . ? C123 H123 0.95 . ? C124 C125 1.386(16) . ? C124 H124 0.95 . ? C125 C126 1.381(15) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 P2 1.837(10) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? P2 C221 1.815(11) . ? P2 C211 1.868(11) . ? C211 C212 1.371(16) . ? C211 C216 1.377(16) . ? C212 C213 1.431(16) . ? C212 H212 0.95 . ? C213 C214 1.345(18) . ? C213 H213 0.95 . ? C214 C215 1.373(19) . ? C214 H214 0.95 . ? C215 C216 1.432(16) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.395(16) . ? C221 C226 1.416(14) . ? C222 C223 1.367(16) . ? C222 H222 0.95 . ? C223 C224 1.406(16) . ? C223 H223 0.95 . ? C224 C225 1.388(17) . ? C224 H224 0.95 . ? C225 C226 1.375(16) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C1 C2 1.430(13) . ? C2 C3 1.196(13) . ? C3 C4 1.455(13) . ? C4 O4 1.241(12) . ? C4 C5 1.488(14) . ? P4 C421 1.822(10) . ? P4 C20 1.832(10) . ? P4 C411 1.833(10) . ? C411 C416 1.391(13) . ? C411 C412 1.417(13) . ? C412 C413 1.405(14) . ? C412 H412 0.95 . ? C413 C414 1.373(15) . ? C413 H413 0.95 . ? C414 C415 1.392(14) . ? C414 H414 0.95 . ? C415 C416 1.380(13) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C426 1.386(14) . ? C421 C422 1.411(13) . ? C422 C423 1.364(14) . ? C422 H422 0.95 . ? C423 C424 1.354(17) . ? C423 H423 0.95 . ? C424 C425 1.379(17) . ? C424 H424 0.95 . ? C425 C426 1.389(16) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C20 P5 1.820(9) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P5 C511 1.820(10) . ? P5 C521 1.832(9) . ? C511 C512 1.381(14) . ? C511 C516 1.413(13) . ? C512 C513 1.394(15) . ? C512 H512 0.95 . ? C513 C514 1.380(15) . ? C513 H513 0.95 . ? C514 C515 1.363(15) . ? C514 H514 0.95 . ? C515 C516 1.373(14) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C526 1.377(13) . ? C521 C522 1.401(12) . ? C522 C523 1.381(13) . ? C522 H522 0.95 . ? C523 C524 1.387(14) . ? C523 H523 0.95 . ? C524 C525 1.374(14) . ? C524 H524 0.95 . ? C525 C526 1.393(13) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? 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 C12 Co1 C11 105.4(5) . . ? C12 Co1 C1 97.5(5) . . ? C11 Co1 C1 143.9(4) . . ? C12 Co1 P1 94.5(4) . . ? C11 Co1 P1 103.2(4) . . ? C1 Co1 P1 102.4(3) . . ? C12 Co1 Co3 99.5(4) . . ? C11 Co1 Co3 99.0(3) . . ? C1 Co1 Co3 49.2(3) . . ? P1 Co1 Co3 149.54(10) . . ? C12 Co1 Co2 145.5(4) . . ? C11 Co1 Co2 105.0(3) . . ? C1 Co1 Co2 47.9(3) . . ? P1 Co1 Co2 94.31(9) . . ? Co3 Co1 Co2 59.60(6) . . ? C22 Co2 C21 102.3(5) . . ? C22 Co2 C1 107.8(5) . . ? C21 Co2 C1 140.4(5) . . ? C22 Co2 P2 97.7(4) . . ? C21 Co2 P2 101.3(3) . . ? C1 Co2 P2 99.5(3) . . ? C22 Co2 Co3 96.0(4) . . ? C21 Co2 Co3 103.1(3) . . ? C1 Co2 Co3 49.3(3) . . ? P2 Co2 Co3 148.65(9) . . ? C22 Co2 Co1 153.1(4) . . ? C21 Co2 Co1 95.2(3) . . ? C1 Co2 Co1 48.4(3) . . ? P2 Co2 Co1 98.76(9) . . ? Co3 Co2 Co1 59.80(6) . . ? C32 Co3 C33 98.0(5) . . ? C32 Co3 C31 100.7(5) . . ? C33 Co3 C31 104.8(5) . . ? C32 Co3 C1 107.7(4) . . ? C33 Co3 C1 101.7(5) . . ? C31 Co3 C1 137.7(5) . . ? C32 Co3 Co2 152.3(3) . . ? C33 Co3 Co2 100.6(4) . . ? C31 Co3 Co2 94.3(4) . . ? C1 Co3 Co2 48.4(3) . . ? C32 Co3 Co1 93.8(4) . . ? C33 Co3 Co1 150.3(4) . . ? C31 Co3 Co1 99.6(4) . . ? C1 Co3 Co1 48.7(3) . . ? Co2 Co3 Co1 60.60(6) . . ? C42 Co4 C41 102.2(6) . . ? C42 Co4 C5 114.7(6) . . ? C41 Co4 C5 134.9(5) . . ? C42 Co4 P4 95.9(4) . . ? C41 Co4 P4 101.6(4) . . ? C5 Co4 P4 99.3(3) . . ? C42 Co4 Co5 159.0(5) . . ? C41 Co4 Co5 88.2(4) . . ? C5 Co4 Co5 49.0(3) . . ? P4 Co4 Co5 99.81(9) . . ? C42 Co4 Co6 99.1(4) . . ? C41 Co4 Co6 102.5(4) . . ? C5 Co4 Co6 48.7(3) . . ? P4 Co4 Co6 148.02(10) . . ? Co5 Co4 Co6 60.54(5) . . ? C52 Co5 C51 100.2(4) . . ? C52 Co5 C5 97.9(4) . . ? C51 Co5 C5 148.7(4) . . ? C52 Co5 P5 95.8(3) . . ? C51 Co5 P5 103.1(3) . . ? C5 Co5 P5 100.1(3) . . ? C52 Co5 Co4 146.9(3) . . ? C51 Co5 Co4 108.5(3) . . ? C5 Co5 Co4 49.1(3) . . ? P5 Co5 Co4 93.36(9) . . ? C52 Co5 Co6 98.1(3) . . ? C51 Co5 Co6 103.6(3) . . ? C5 Co5 Co6 48.3(3) . . ? P5 Co5 Co6 146.96(9) . . ? Co4 Co5 Co6 59.80(5) . . ? C63 Co6 C61 99.9(5) . . ? C63 Co6 C62 98.6(5) . . ? C61 Co6 C62 102.1(5) . . ? C63 Co6 C5 103.3(5) . . ? C61 Co6 C5 142.0(5) . . ? C62 Co6 C5 103.6(4) . . ? C63 Co6 Co4 152.0(4) . . ? C61 Co6 Co4 102.1(4) . . ? C62 Co6 Co4 93.5(4) . . ? C5 Co6 Co4 49.1(3) . . ? C63 Co6 Co5 100.3(3) . . ? C61 Co6 Co5 98.0(3) . . ? C62 Co6 Co5 149.4(4) . . ? C5 Co6 Co5 48.6(3) . . ? Co4 Co6 Co5 59.66(5) . . ? O11 C11 Co1 176.0(10) . . ? O12 C12 Co1 175.4(10) . . ? O21 C21 Co2 178.1(10) . . ? O22 C22 Co2 177.4(10) . . ? O31 C31 Co3 178.3(11) . . ? O32 C32 Co3 175.5(9) . . ? O33 C33 Co3 176.7(12) . . ? O41 C41 Co4 179.0(10) . . ? O42 C42 Co4 175.7(14) . . ? O51 C51 Co5 176.3(9) . . ? O52 C52 Co5 176.3(9) . . ? O61 C61 Co6 176.9(11) . . ? O62 C62 Co6 179.3(12) . . ? O63 C63 Co6 174.3(10) . . ? C10 P1 C121 105.1(5) . . ? C10 P1 C111 101.8(4) . . ? C121 P1 C111 102.5(4) . . ? C10 P1 Co1 111.4(4) . . ? C121 P1 Co1 118.4(3) . . ? C111 P1 Co1 115.8(3) . . ? C112 C111 C116 119.2(9) . . ? C112 C111 P1 122.2(8) . . ? C116 C111 P1 118.5(7) . . ? C111 C112 C113 120.4(10) . . ? C111 C112 H112 119.8 . . ? C113 C112 H112 119.8 . . ? C112 C113 C114 119.8(10) . . ? C112 C113 H113 120.1 . . ? C114 C113 H113 120.1 . . ? C115 C114 C113 120.1(10) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C114 C115 C116 120.8(11) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? C115 C116 C111 119.6(10) . . ? C115 C116 H116 120.2 . . ? C111 C116 H116 120.2 . . ? C126 C121 C122 117.4(10) . . ? C126 C121 P1 121.1(8) . . ? C122 C121 P1 121.4(8) . . ? C123 C122 C121 120.9(11) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C122 C123 C124 120.9(12) . . ? C122 C123 H123 119.6 . . ? C124 C123 H123 119.6 . . ? C123 C124 C125 119.7(12) . . ? C123 C124 H124 120.1 . . ? C125 C124 H124 120.1 . . ? C126 C125 C124 119.1(10) . . ? C126 C125 H125 120.4 . . ? C124 C125 H125 120.4 . . ? C125 C126 C121 121.9(10) . . ? C125 C126 H126 119 . . ? C121 C126 H126 119 . . ? P1 C10 P2 111.7(5) . . ? P1 C10 H10A 109.3 . . ? P2 C10 H10A 109.3 . . ? P1 C10 H10B 109.3 . . ? P2 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C221 P2 C10 107.6(5) . . ? C221 P2 C211 101.6(5) . . ? C10 P2 C211 99.5(4) . . ? C221 P2 Co2 116.2(3) . . ? C10 P2 Co2 109.6(3) . . ? C211 P2 Co2 120.5(4) . . ? C212 C211 C216 121.3(11) . . ? C212 C211 P2 120.0(9) . . ? C216 C211 P2 118.5(10) . . ? C211 C212 C213 118.7(13) . . ? C211 C212 H212 120.6 . . ? C213 C212 H212 120.6 . . ? C214 C213 C212 119.9(15) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C213 C214 C215 122.3(13) . . ? C213 C214 H214 118.9 . . ? C215 C214 H214 118.9 . . ? C214 C215 C216 118.5(13) . . ? C214 C215 H215 120.8 . . ? C216 C215 H215 120.8 . . ? C211 C216 C215 119.3(13) . . ? C211 C216 H216 120.4 . . ? C215 C216 H216 120.4 . . ? C222 C221 C226 119.0(10) . . ? C222 C221 P2 124.9(8) . . ? C226 C221 P2 116.1(9) . . ? C223 C222 C221 120.8(11) . . ? C223 C222 H222 119.6 . . ? C221 C222 H222 119.6 . . ? C222 C223 C224 120.0(13) . . ? C222 C223 H223 120 . . ? C224 C223 H223 120 . . ? C225 C224 C223 119.9(12) . . ? C225 C224 H224 120.1 . . ? C223 C224 H224 120.1 . . ? C226 C225 C224 120.2(11) . . ? C226 C225 H225 119.9 . . ? C224 C225 H225 119.9 . . ? C225 C226 C221 120.1(11) . . ? C225 C226 H226 120 . . ? C221 C226 H226 120 . . ? C2 C1 Co2 133.3(8) . . ? C2 C1 Co1 125.0(7) . . ? Co2 C1 Co1 83.7(4) . . ? C2 C1 Co3 132.2(8) . . ? Co2 C1 Co3 82.3(4) . . ? Co1 C1 Co3 82.2(4) . . ? C3 C2 C1 176.0(12) . . ? C2 C3 C4 171.4(12) . . ? O4 C4 C3 118.7(9) . . ? O4 C4 C5 124.3(8) . . ? C3 C4 C5 117.0(9) . . ? C4 C5 Co6 127.3(7) . . ? C4 C5 Co5 126.9(7) . . ? Co6 C5 Co5 83.1(4) . . ? C4 C5 Co4 136.9(7) . . ? Co6 C5 Co4 82.2(4) . . ? Co5 C5 Co4 81.9(4) . . ? C421 P4 C20 107.1(4) . . ? C421 P4 C411 102.5(4) . . ? C20 P4 C411 103.8(5) . . ? C421 P4 Co4 115.9(3) . . ? C20 P4 Co4 109.0(3) . . ? C411 P4 Co4 117.4(3) . . ? C416 C411 C412 119.3(9) . . ? C416 C411 P4 122.2(7) . . ? C412 C411 P4 118.5(8) . . ? C413 C412 C411 119.1(10) . . ? C413 C412 H412 120.5 . . ? C411 C412 H412 120.5 . . ? C414 C413 C412 120.7(10) . . ? C414 C413 H413 119.7 . . ? C412 C413 H413 119.7 . . ? C413 C414 C415 119.8(10) . . ? C413 C414 H414 120.1 . . ? C415 C414 H414 120.1 . . ? C416 C415 C414 120.8(10) . . ? C416 C415 H415 119.6 . . ? C414 C415 H415 119.6 . . ? C415 C416 C411 120.4(9) . . ? C415 C416 H416 119.8 . . ? C411 C416 H416 119.8 . . ? C426 C421 C422 118.1(9) . . ? C426 C421 P4 116.9(8) . . ? C422 C421 P4 124.9(8) . . ? C423 C422 C421 120.2(11) . . ? C423 C422 H422 119.9 . . ? C421 C422 H422 119.9 . . ? C424 C423 C422 121.4(11) . . ? C424 C423 H423 119.3 . . ? C422 C423 H423 119.3 . . ? C423 C424 C425 119.8(12) . . ? C423 C424 H424 120.1 . . ? C425 C424 H424 120.1 . . ? C424 C425 C426 120.2(13) . . ? C424 C425 H425 119.9 . . ? C426 C425 H425 119.9 . . ? C421 C426 C425 120.2(11) . . ? C421 C426 H426 119.9 . . ? C425 C426 H426 119.9 . . ? P5 C20 P4 109.6(5) . . ? P5 C20 H20A 109.7 . . ? P4 C20 H20A 109.7 . . ? P5 C20 H20B 109.7 . . ? P4 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C511 P5 C20 104.6(5) . . ? C511 P5 C521 102.5(4) . . ? C20 P5 C521 102.7(4) . . ? C511 P5 Co5 113.8(3) . . ? C20 P5 Co5 112.0(3) . . ? C521 P5 Co5 119.5(3) . . ? C512 C511 C516 119.2(10) . . ? C512 C511 P5 123.8(8) . . ? C516 C511 P5 116.6(8) . . ? C511 C512 C513 120.6(10) . . ? C511 C512 H512 119.7 . . ? C513 C512 H512 119.7 . . ? C514 C513 C512 119.0(11) . . ? C514 C513 H513 120.5 . . ? C512 C513 H513 120.5 . . ? C515 C514 C513 121.2(11) . . ? C515 C514 H514 119.4 . . ? data_br1420 _database_code_depnum_ccdc_archive 'CCDC 754942' #TrackingRef '3.br1420.cif' _audit_creation_date 2008-05-28T09:26:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H27 Co3 O11 P2 W1' _chemical_formula_moiety 'C44 H27 Co3 O11 P2 W1' _chemical_formula_weight 1154.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c_1_2/c_1 _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 33.249(5) _cell_length_b 12.021(5) _cell_length_c 22.622(5) _cell_angle_alpha 90 _cell_angle_beta 110.505(5) _cell_angle_gamma 90 _cell_volume 8469(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14114 _cell_measurement_theta_min 3.3209 _cell_measurement_theta_max 32.2931 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.81652 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0223674941 _diffrn_orient_matrix_ub_12 -0.0097446957 _diffrn_orient_matrix_ub_13 0.0091495026 _diffrn_orient_matrix_ub_21 0.0016076019 _diffrn_orient_matrix_ub_22 -0.0020952924 _diffrn_orient_matrix_ub_23 0.0320852183 _diffrn_orient_matrix_ub_31 -0.0038178128 _diffrn_orient_matrix_ub_32 -0.0581311214 _diffrn_orient_matrix_ub_33 -0.0026999781 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_unetI/netI 0.0966 _diffrn_reflns_number 48119 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 32.34 _diffrn_reflns_theta_full 30.75 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 14010 _reflns_number_gt 8177 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0878P)^2^+96.3298P] 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_number_reflns 14010 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1977 _refine_ls_wR_factor_gt 0.1851 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.215 _refine_diff_density_min -1.67 _refine_diff_density_rms 0.259 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.35256(3) 0.23820(7) 0.24433(4) 0.01191(18) Uani 1 1 d . . . Co2 Co 0.38357(3) 0.08858(7) 0.19772(5) 0.0143(2) Uani 1 1 d . . . Co3 Co 0.43032(3) 0.23759(7) 0.26249(5) 0.01463(19) Uani 1 1 d . . . W4 W 0.485516(10) 0.24944(3) 0.533611(15) 0.02020(9) Uani 1 1 d . . . C11 C 0.3354(3) 0.3086(6) 0.1704(4) 0.0200(15) Uani 1 1 d . . . O11 O 0.3262(2) 0.3571(5) 0.1236(3) 0.0269(13) Uani 1 1 d . . . C12 C 0.3523(3) 0.3451(6) 0.2986(4) 0.0193(15) Uani 1 1 d . . . O12 O 0.3521(2) 0.4137(5) 0.3335(3) 0.0319(14) Uani 1 1 d . . . C21 C 0.3801(3) 0.1287(6) 0.1182(4) 0.0212(16) Uani 1 1 d . . . O21 O 0.3789(2) 0.1552(5) 0.0699(3) 0.0330(14) Uani 1 1 d . . . C22 C 0.4218(3) -0.0211(6) 0.2142(4) 0.0214(16) Uani 1 1 d . . . O22 O 0.4466(2) -0.0917(5) 0.2281(4) 0.0398(17) Uani 1 1 d . . . C31 C 0.4360(3) 0.3094(7) 0.1951(4) 0.0257(17) Uani 1 1 d . . . O31 O 0.4397(2) 0.3525(5) 0.1529(3) 0.0374(16) Uani 1 1 d . . . C32 C 0.4435(3) 0.3454(7) 0.3201(4) 0.0263(17) Uani 1 1 d . . . O32 O 0.4533(2) 0.4144(5) 0.3570(3) 0.0371(16) Uani 1 1 d . . . C33 C 0.4775(3) 0.1565(6) 0.2994(4) 0.0202(15) Uani 1 1 d . . . O33 O 0.50578(19) 0.1006(5) 0.3262(3) 0.0281(13) Uani 1 1 d . . . C41 C 0.4376(3) 0.3577(7) 0.4979(5) 0.032(2) Uani 1 1 d . . . O41 O 0.4106(2) 0.4197(5) 0.4767(4) 0.0468(19) Uani 1 1 d . . . C42 C 0.4774(3) 0.3073(9) 0.6124(5) 0.043(3) Uani 1 1 d . . . O42 O 0.4724(3) 0.3419(8) 0.6562(4) 0.060(2) Uani 1 1 d . . . C43 C 0.4591(3) 0.1157(8) 0.5593(4) 0.035(2) Uani 1 1 d . . . O43 O 0.4437(3) 0.0416(6) 0.5727(4) 0.053(2) Uani 1 1 d . . . P1 P 0.29575(6) 0.14764(14) 0.24808(9) 0.0125(3) Uani 1 1 d . . . C111 C 0.2871(2) 0.1444(5) 0.3238(3) 0.0136(13) Uani 1 1 d . . . C112 C 0.3220(2) 0.1614(5) 0.3796(3) 0.0155(14) Uani 1 1 d . . . H112 H 0.3489 0.1847 0.3777 0.019 Uiso 1 1 calc R . . C113 C 0.3176(3) 0.1441(6) 0.4383(4) 0.0216(16) Uani 1 1 d . . . H113 H 0.3415 0.1536 0.4762 0.026 Uiso 1 1 calc R . . C114 C 0.2780(3) 0.1131(6) 0.4407(4) 0.0204(16) Uani 1 1 d . . . H114 H 0.2748 0.1032 0.4805 0.025 Uiso 1 1 calc R . . C115 C 0.2432(3) 0.0964(6) 0.3857(4) 0.0183(15) Uani 1 1 d . . . H115 H 0.2163 0.0745 0.3878 0.022 Uiso 1 1 calc R . . C116 C 0.2476(2) 0.1119(5) 0.3275(4) 0.0160(14) Uani 1 1 d . . . H116 H 0.2237 0.1003 0.2899 0.019 Uiso 1 1 calc R . . C121 C 0.2442(2) 0.1886(6) 0.1905(3) 0.0145(14) Uani 1 1 d . . . C122 C 0.2101(2) 0.1148(6) 0.1632(4) 0.0176(14) Uani 1 1 d . . . H122 H 0.2132 0.0385 0.1749 0.021 Uiso 1 1 calc R . . C123 C 0.1718(2) 0.1521(6) 0.1191(4) 0.0188(15) Uani 1 1 d . . . H123 H 0.1487 0.1016 0.1017 0.023 Uiso 1 1 calc R . . C124 C 0.1671(2) 0.2619(6) 0.1005(4) 0.0205(15) Uani 1 1 d . . . H124 H 0.1415 0.2864 0.0686 0.025 Uiso 1 1 calc R . . C125 C 0.2004(3) 0.3367(6) 0.1291(4) 0.0221(16) Uani 1 1 d . . . H125 H 0.1967 0.4134 0.1184 0.026 Uiso 1 1 calc R . . C126 C 0.2380(2) 0.3005(6) 0.1723(4) 0.0169(14) Uani 1 1 d . . . H126 H 0.2605 0.3523 0.1905 0.02 Uiso 1 1 calc R . . C0 C 0.3019(2) -0.0021(5) 0.2373(3) 0.0139(13) Uani 1 1 d . . . H0A H 0.3198 -0.0362 0.2779 0.017 Uiso 1 1 calc R . . H0B H 0.2734 -0.0387 0.2229 0.017 Uiso 1 1 calc R . . P2 P 0.32765(6) -0.02086(14) 0.17840(9) 0.0134(3) Uani 1 1 d . . . C211 C 0.3424(2) -0.1676(6) 0.1812(4) 0.0176(14) Uani 1 1 d . . . C212 C 0.3504(2) -0.2316(5) 0.2350(4) 0.0178(14) Uani 1 1 d . . . H212 H 0.3444 -0.2028 0.2701 0.021 Uiso 1 1 calc R . . C213 C 0.3675(3) -0.3387(6) 0.2377(5) 0.0276(18) Uani 1 1 d . . . H213 H 0.3737 -0.3819 0.275 0.033 Uiso 1 1 calc R . . C214 C 0.3752(3) -0.3806(7) 0.1870(5) 0.034(2) Uani 1 1 d . . . H214 H 0.3862 -0.454 0.1889 0.041 Uiso 1 1 calc R . . C215 C 0.3674(3) -0.3186(7) 0.1327(4) 0.0289(19) Uani 1 1 d . . . H215 H 0.3735 -0.348 0.0978 0.035 Uiso 1 1 calc R . . C216 C 0.3503(3) -0.2122(7) 0.1302(4) 0.0223(16) Uani 1 1 d . . . H216 H 0.3439 -0.1696 0.0926 0.027 Uiso 1 1 calc R . . C221 C 0.2812(2) -0.0102(6) 0.1062(3) 0.0157(14) Uani 1 1 d . . . C222 C 0.2495(2) -0.0923(6) 0.0916(4) 0.0173(14) Uani 1 1 d . . . H222 H 0.2545 -0.1586 0.116 0.021 Uiso 1 1 calc R . . C223 C 0.2105(3) -0.0784(6) 0.0417(4) 0.0205(15) Uani 1 1 d . . . H223 H 0.1891 -0.1346 0.0326 0.025 Uiso 1 1 calc R . . C224 C 0.2033(3) 0.0169(6) 0.0057(4) 0.0216(16) Uani 1 1 d . . . H224 H 0.1767 0.0271 -0.0278 0.026 Uiso 1 1 calc R . . C225 C 0.2352(3) 0.0987(6) 0.0188(4) 0.0211(16) Uani 1 1 d . . . H225 H 0.2306 0.1637 -0.0066 0.025 Uiso 1 1 calc R . . C226 C 0.2733(3) 0.0854(6) 0.0683(3) 0.0189(15) Uani 1 1 d . . . H226 H 0.2946 0.1418 0.0769 0.023 Uiso 1 1 calc R . . C1 C 0.3941(2) 0.1285(5) 0.2827(3) 0.0148(13) Uani 1 1 d . . . C2 C 0.4041(2) 0.0633(6) 0.3412(4) 0.0185(14) Uani 1 1 d . . . O2 O 0.39328(19) -0.0326(4) 0.3416(3) 0.0255(12) Uani 1 1 d . . . C3 C 0.4268(2) 0.1241(6) 0.4003(4) 0.0188(15) Uani 1 1 d . . . C4 C 0.4458(3) 0.1703(6) 0.4474(4) 0.0208(15) Uani 1 1 d . . . C401 C 0.5342(4) 0.2250(8) 0.4820(5) 0.045(3) Uani 1 1 d . . . H401 H 0.5245 0.1933 0.4409 0.054 Uiso 1 1 calc R . . C402 C 0.5352(3) 0.3368(7) 0.4958(4) 0.0285(18) Uani 1 1 d . . . H402 H 0.5278 0.3959 0.466 0.034 Uiso 1 1 calc R . . C403 C 0.5495(3) 0.3482(7) 0.5638(5) 0.032(2) Uani 1 1 d . . . H403 H 0.5528 0.4162 0.5864 0.039 Uiso 1 1 calc R . . C404 C 0.5577(2) 0.2410(7) 0.5907(4) 0.0251(16) Uani 1 1 d . . . H404 H 0.5665 0.2238 0.6343 0.03 Uiso 1 1 calc R . . C405 C 0.5506(3) 0.1636(7) 0.5410(4) 0.0280(18) Uani 1 1 d . . . H405 H 0.5556 0.0857 0.5453 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0126(4) 0.0115(4) 0.0121(4) 0.0003(3) 0.0049(3) 0.0000(3) Co2 0.0154(5) 0.0130(4) 0.0154(5) -0.0012(4) 0.0066(4) -0.0005(4) Co3 0.0119(4) 0.0145(4) 0.0179(5) -0.0012(4) 0.0057(4) -0.0017(4) W4 0.01899(15) 0.02009(14) 0.01813(15) -0.00271(13) 0.00227(11) -0.00086(13) C11 0.020(4) 0.018(3) 0.021(4) 0.000(3) 0.006(3) 0.000(3) O11 0.030(3) 0.027(3) 0.020(3) 0.011(2) 0.005(3) 0.005(2) C12 0.022(4) 0.015(3) 0.022(4) 0.002(3) 0.010(3) 0.000(3) O12 0.036(4) 0.025(3) 0.035(4) -0.008(3) 0.013(3) 0.005(3) C21 0.021(4) 0.021(3) 0.024(4) -0.002(3) 0.011(3) -0.001(3) O21 0.040(4) 0.039(3) 0.027(3) 0.003(3) 0.020(3) -0.003(3) C22 0.016(4) 0.019(3) 0.028(4) -0.005(3) 0.007(3) -0.003(3) O22 0.028(3) 0.027(3) 0.060(5) -0.006(3) 0.010(3) 0.007(3) C31 0.025(4) 0.023(4) 0.030(5) 0.002(3) 0.010(4) 0.004(3) O31 0.053(5) 0.029(3) 0.036(4) 0.010(3) 0.024(4) -0.002(3) C32 0.021(4) 0.027(4) 0.032(5) -0.005(3) 0.010(4) -0.005(3) O32 0.035(4) 0.029(3) 0.046(4) -0.018(3) 0.012(3) -0.007(3) C33 0.021(4) 0.017(3) 0.024(4) -0.006(3) 0.009(3) -0.004(3) O33 0.021(3) 0.032(3) 0.030(3) 0.003(3) 0.009(3) 0.003(3) C41 0.030(5) 0.025(4) 0.043(6) -0.005(4) 0.015(4) -0.004(4) O41 0.039(4) 0.031(3) 0.064(5) 0.001(3) 0.010(4) 0.012(3) C42 0.029(5) 0.049(6) 0.046(6) -0.019(5) 0.007(5) -0.005(4) O42 0.041(5) 0.102(7) 0.041(5) -0.036(5) 0.020(4) -0.010(4) C43 0.041(6) 0.035(5) 0.022(5) 0.003(4) 0.002(4) 0.001(4) O43 0.054(5) 0.054(5) 0.043(5) 0.018(4) 0.007(4) -0.021(4) P1 0.0135(8) 0.0121(7) 0.0123(8) 0.0002(6) 0.0050(7) -0.0001(6) C111 0.018(3) 0.010(3) 0.014(3) 0.000(2) 0.007(3) 0.002(3) C112 0.019(4) 0.013(3) 0.015(3) -0.004(3) 0.007(3) -0.002(3) C113 0.027(4) 0.022(3) 0.016(4) 0.000(3) 0.007(3) 0.005(3) C114 0.027(4) 0.018(3) 0.017(4) 0.003(3) 0.010(3) 0.001(3) C115 0.018(4) 0.017(3) 0.024(4) 0.001(3) 0.013(3) 0.001(3) C116 0.016(3) 0.014(3) 0.019(4) -0.003(3) 0.005(3) 0.002(3) C121 0.013(3) 0.017(3) 0.015(4) -0.002(3) 0.007(3) 0.001(3) C122 0.017(4) 0.018(3) 0.016(4) 0.002(3) 0.003(3) -0.001(3) C123 0.012(3) 0.018(3) 0.026(4) 0.002(3) 0.006(3) 0.001(3) C124 0.009(3) 0.030(4) 0.021(4) 0.006(3) 0.004(3) 0.003(3) C125 0.028(4) 0.015(3) 0.024(4) 0.005(3) 0.010(3) 0.007(3) C126 0.015(3) 0.014(3) 0.022(4) -0.002(3) 0.006(3) 0.000(3) C0 0.018(3) 0.012(3) 0.010(3) 0.002(2) 0.004(3) -0.001(3) P2 0.0149(9) 0.0124(7) 0.0134(9) -0.0005(6) 0.0054(7) 0.0000(7) C211 0.019(4) 0.014(3) 0.020(4) -0.001(3) 0.008(3) 0.001(3) C212 0.016(3) 0.011(3) 0.026(4) 0.001(3) 0.006(3) -0.001(2) C213 0.025(4) 0.017(3) 0.037(5) 0.001(3) 0.006(4) -0.001(3) C214 0.032(5) 0.015(3) 0.052(6) -0.006(4) 0.012(5) 0.007(3) C215 0.024(4) 0.022(4) 0.035(5) -0.015(4) 0.004(4) 0.006(3) C216 0.019(4) 0.021(3) 0.027(4) -0.005(3) 0.008(3) 0.000(3) C221 0.020(4) 0.017(3) 0.013(3) -0.002(3) 0.010(3) -0.001(3) C222 0.019(4) 0.014(3) 0.018(4) 0.001(3) 0.005(3) -0.001(3) C223 0.023(4) 0.019(3) 0.018(4) 0.001(3) 0.005(3) -0.004(3) C224 0.024(4) 0.019(3) 0.016(4) 0.001(3) 0.000(3) -0.001(3) C225 0.024(4) 0.020(3) 0.014(4) 0.005(3) -0.001(3) -0.002(3) C226 0.022(4) 0.017(3) 0.015(4) 0.000(3) 0.003(3) -0.006(3) C1 0.017(3) 0.012(3) 0.017(3) 0.003(3) 0.008(3) 0.002(3) C2 0.013(3) 0.023(3) 0.015(4) 0.001(3) 0.000(3) 0.000(3) O2 0.029(3) 0.016(2) 0.022(3) 0.003(2) -0.002(2) -0.003(2) C3 0.019(4) 0.016(3) 0.020(4) 0.004(3) 0.004(3) -0.003(3) C4 0.022(4) 0.017(3) 0.023(4) 0.004(3) 0.007(3) 0.003(3) C401 0.073(8) 0.034(5) 0.041(6) -0.025(4) 0.035(6) -0.040(5) C402 0.026(4) 0.027(4) 0.031(5) 0.001(4) 0.008(4) -0.002(3) C403 0.022(4) 0.030(4) 0.042(6) -0.013(4) 0.007(4) -0.013(4) C404 0.012(3) 0.034(4) 0.027(4) -0.006(4) 0.004(3) -0.001(3) C405 0.023(4) 0.023(4) 0.034(5) -0.003(3) 0.004(4) 0.004(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.779(8) . ? Co1 C11 1.780(8) . ? Co1 C1 1.886(7) . ? Co1 P1 2.207(2) . ? Co1 Co3 2.4716(14) . ? Co1 Co2 2.4842(14) . ? Co2 C22 1.777(8) . ? Co2 C21 1.827(8) . ? Co2 C1 1.891(7) . ? Co2 P2 2.193(2) . ? Co2 Co3 2.4853(15) . ? Co3 C32 1.780(8) . ? Co3 C33 1.786(8) . ? Co3 C31 1.819(9) . ? Co3 C1 1.941(7) . ? W4 C41 1.996(10) . ? W4 C43 2.012(10) . ? W4 C42 2.017(11) . ? W4 C4 2.156(8) . ? W4 C404 2.296(8) . ? W4 C403 2.320(8) . ? W4 C401 2.323(11) . ? W4 C405 2.350(8) . ? W4 C402 2.357(9) . ? C11 O11 1.152(9) . ? C12 O12 1.144(9) . ? C21 O21 1.125(10) . ? C22 O22 1.149(10) . ? C31 O31 1.129(10) . ? C32 O32 1.140(10) . ? C33 O33 1.142(10) . ? C41 O41 1.135(11) . ? C42 O42 1.140(12) . ? C43 O43 1.122(11) . ? P1 C121 1.819(8) . ? P1 C111 1.834(7) . ? P1 C0 1.837(7) . ? C111 C112 1.398(10) . ? C111 C116 1.401(10) . ? C112 C113 1.404(10) . ? C112 H112 0.95 . ? C113 C114 1.387(11) . ? C113 H113 0.95 . ? C114 C115 1.386(11) . ? C114 H114 0.95 . ? C115 C116 1.387(10) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.401(10) . ? C121 C122 1.402(10) . ? C122 C123 1.388(10) . ? C122 H122 0.95 . ? C123 C124 1.377(10) . ? C123 H123 0.95 . ? C124 C125 1.396(11) . ? C124 H124 0.95 . ? C125 C126 1.361(11) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C0 P2 1.833(7) . ? C0 H0A 0.99 . ? C0 H0B 0.99 . ? P2 C221 1.817(8) . ? P2 C211 1.826(7) . ? C211 C216 1.378(11) . ? C211 C212 1.384(10) . ? C212 C213 1.399(10) . ? C212 H212 0.95 . ? C213 C214 1.358(13) . ? C213 H213 0.95 . ? C214 C215 1.381(14) . ? C214 H214 0.95 . ? C215 C216 1.394(11) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.396(10) . ? C221 C226 1.403(10) . ? C222 C223 1.401(11) . ? C222 H222 0.95 . ? C223 C224 1.376(10) . ? C223 H223 0.95 . ? C224 C225 1.402(11) . ? C224 H224 0.95 . ? C225 C226 1.373(11) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C1 C2 1.472(10) . ? C2 O2 1.208(9) . ? C2 C3 1.478(11) . ? C3 C4 1.171(11) . ? C401 C402 1.379(12) . ? C401 C405 1.454(15) . ? C401 H401 0.95 . ? C402 C403 1.450(13) . ? C402 H402 0.95 . ? C403 C404 1.410(12) . ? C403 H403 0.95 . ? C404 C405 1.413(12) . ? C404 H404 0.95 . ? C405 H405 0.95 . ? 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 C12 Co1 C11 103.1(3) . . ? C12 Co1 C1 111.6(3) . . ? C11 Co1 C1 135.0(3) . . ? C12 Co1 P1 96.8(3) . . ? C11 Co1 P1 105.8(3) . . ? C1 Co1 P1 97.8(2) . . ? C12 Co1 Co3 98.4(3) . . ? C11 Co1 Co3 97.5(3) . . ? C1 Co1 Co3 50.7(2) . . ? P1 Co1 Co3 148.38(7) . . ? C12 Co1 Co2 156.8(3) . . ? C11 Co1 Co2 89.4(2) . . ? C1 Co1 Co2 49.0(2) . . ? P1 Co1 Co2 98.46(6) . . ? Co3 Co1 Co2 60.20(4) . . ? C22 Co2 C21 101.3(4) . . ? C22 Co2 C1 96.4(3) . . ? C21 Co2 C1 149.3(3) . . ? C22 Co2 P2 95.2(2) . . ? C21 Co2 P2 101.8(3) . . ? C1 Co2 P2 101.4(2) . . ? C22 Co2 Co1 145.1(3) . . ? C21 Co2 Co1 109.5(2) . . ? C1 Co2 Co1 48.8(2) . . ? P2 Co2 Co1 94.02(6) . . ? C22 Co2 Co3 99.1(3) . . ? C21 Co2 Co3 101.6(2) . . ? C1 Co2 Co3 50.4(2) . . ? P2 Co2 Co3 149.48(7) . . ? Co1 Co2 Co3 59.65(4) . . ? C32 Co3 C33 96.0(4) . . ? C32 Co3 C31 101.3(4) . . ? C33 Co3 C31 108.6(4) . . ? C32 Co3 C1 109.5(3) . . ? C33 Co3 C1 92.1(3) . . ? C31 Co3 C1 140.7(4) . . ? C32 Co3 Co1 95.5(3) . . ? C33 Co3 Co1 140.8(2) . . ? C31 Co3 Co1 105.6(3) . . ? C1 Co3 Co1 48.8(2) . . ? C32 Co3 Co2 154.1(3) . . ? C33 Co3 Co2 98.5(2) . . ? C31 Co3 Co2 94.3(3) . . ? C1 Co3 Co2 48.7(2) . . ? Co1 Co3 Co2 60.15(4) . . ? C41 W4 C43 105.7(4) . . ? C41 W4 C42 78.3(4) . . ? C43 W4 C42 79.2(4) . . ? C41 W4 C4 76.9(3) . . ? C43 W4 C4 73.6(3) . . ? C42 W4 C4 136.2(4) . . ? C41 W4 C404 141.8(3) . . ? C43 W4 C404 106.2(4) . . ? C42 W4 C404 87.5(4) . . ? C4 W4 C404 132.6(3) . . ? C41 W4 C403 107.8(4) . . ? C43 W4 C403 140.5(4) . . ? C42 W4 C403 87.5(4) . . ? C4 W4 C403 134.4(3) . . ? C404 W4 C403 35.6(3) . . ? C41 W4 C401 118.5(4) . . ? C43 W4 C401 119.7(4) . . ? C42 W4 C401 145.2(4) . . ? C4 W4 C401 78.6(3) . . ? C404 W4 C401 60.1(4) . . ? C403 W4 C401 59.0(3) . . ? C41 W4 C405 154.1(4) . . ? C43 W4 C405 96.5(4) . . ? C42 W4 C405 119.6(4) . . ? C4 W4 C405 97.3(3) . . ? C404 W4 C405 35.4(3) . . ? C403 W4 C405 58.5(3) . . ? C401 W4 C405 36.2(4) . . ? C41 W4 C402 97.1(3) . . ? C43 W4 C402 153.3(4) . . ? C42 W4 C402 119.7(4) . . ? C4 W4 C402 98.8(3) . . ? C404 W4 C402 59.7(3) . . ? C403 W4 C402 36.1(3) . . ? C401 W4 C402 34.3(3) . . ? C405 W4 C402 58.4(3) . . ? O11 C11 Co1 176.4(7) . . ? O12 C12 Co1 179.8(8) . . ? O21 C21 Co2 178.1(8) . . ? O22 C22 Co2 176.4(8) . . ? O31 C31 Co3 179.0(8) . . ? O32 C32 Co3 177.8(8) . . ? O33 C33 Co3 173.9(7) . . ? O41 C41 W4 178.8(9) . . ? O42 C42 W4 178.6(11) . . ? O43 C43 W4 178.7(10) . . ? C121 P1 C111 105.0(3) . . ? C121 P1 C0 106.9(3) . . ? C111 P1 C0 99.4(3) . . ? C121 P1 Co1 116.3(2) . . ? C111 P1 Co1 117.5(2) . . ? C0 P1 Co1 110.0(2) . . ? C112 C111 C116 119.1(6) . . ? C112 C111 P1 119.2(5) . . ? C116 C111 P1 121.3(6) . . ? C111 C112 C113 120.3(7) . . ? C111 C112 H112 119.9 . . ? C113 C112 H112 119.9 . . ? C114 C113 C112 119.5(8) . . ? C114 C113 H113 120.3 . . ? C112 C113 H113 120.3 . . ? C115 C114 C113 120.7(7) . . ? C115 C114 H114 119.6 . . ? C113 C114 H114 119.6 . . ? C114 C115 C116 119.9(7) . . ? C114 C115 H115 120 . . ? C116 C115 H115 120 . . ? C115 C116 C111 120.5(7) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C126 C121 C122 117.7(7) . . ? C126 C121 P1 118.4(5) . . ? C122 C121 P1 123.9(5) . . ? C123 C122 C121 120.6(7) . . ? C123 C122 H122 119.7 . . ? C121 C122 H122 119.7 . . ? C124 C123 C122 120.4(7) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C123 C124 C125 119.3(7) . . ? C123 C124 H124 120.4 . . ? C125 C124 H124 120.4 . . ? C126 C125 C124 120.4(7) . . ? C126 C125 H125 119.8 . . ? C124 C125 H125 119.8 . . ? C125 C126 C121 121.5(7) . . ? C125 C126 H126 119.3 . . ? C121 C126 H126 119.3 . . ? P2 C0 P1 108.6(3) . . ? P2 C0 H0A 110 . . ? P1 C0 H0A 110 . . ? P2 C0 H0B 110 . . ? P1 C0 H0B 110 . . ? H0A C0 H0B 108.3 . . ? C221 P2 C211 103.4(3) . . ? C221 P2 C0 100.3(3) . . ? C211 P2 C0 106.4(3) . . ? C221 P2 Co2 122.1(2) . . ? C211 P2 Co2 112.0(3) . . ? C0 P2 Co2 111.1(2) . . ? C216 C211 C212 119.1(7) . . ? C216 C211 P2 118.2(6) . . ? C212 C211 P2 122.3(6) . . ? C211 C212 C213 120.0(8) . . ? C211 C212 H212 120 . . ? C213 C212 H212 120 . . ? C214 C213 C212 119.9(8) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C213 C214 C215 121.2(7) . . ? C213 C214 H214 119.4 . . ? C215 C214 H214 119.4 . . ? C214 C215 C216 118.7(8) . . ? C214 C215 H215 120.7 . . ? C216 C215 H215 120.7 . . ? C211 C216 C215 121.1(8) . . ? C211 C216 H216 119.5 . . ? C215 C216 H216 119.5 . . ? C222 C221 C226 118.0(7) . . ? C222 C221 P2 119.7(5) . . ? C226 C221 P2 121.7(6) . . ? C221 C222 C223 121.0(7) . . ? C221 C222 H222 119.5 . . ? C223 C222 H222 119.5 . . ? C224 C223 C222 119.8(7) . . ? C224 C223 H223 120.1 . . ? C222 C223 H223 120.1 . . ? C223 C224 C225 119.7(7) . . ? C223 C224 H224 120.1 . . ? C225 C224 H224 120.1 . . ? C226 C225 C224 120.3(7) . . ? C226 C225 H225 119.8 . . ? C224 C225 H225 119.8 . . ? C225 C226 C221 121.0(7) . . ? C225 C226 H226 119.5 . . ? C221 C226 H226 119.5 . . ? C2 C1 Co1 133.1(5) . . ? C2 C1 Co2 133.0(5) . . ? Co1 C1 Co2 82.2(3) . . ? C2 C1 Co3 127.5(5) . . ? Co1 C1 Co3 80.4(3) . . ? Co2 C1 Co3 80.9(3) . . ? O2 C2 C1 122.7(7) . . ? O2 C2 C3 121.6(7) . . ? C1 C2 C3 115.6(6) . . ? C4 C3 C2 177.9(9) . . ? C3 C4 W4 175.4(7) . . ? C402 C401 C405 108.4(8) . . ? C402 C401 W4 74.2(6) . . ? C405 C401 W4 72.9(5) . . ? C402 C401 H401 125.8 . . ? C405 C401 H401 125.8 . . ? W4 C401 H401 119 . . ? C401 C402 C403 107.8(8) . . ? C401 C402 W4 71.5(5) . . ? C403 C402 W4 70.6(5) . . ? C401 C402 H402 126.1 . . ? # Attachment '1.br1422.cif' data_br1422 _database_code_depnum_ccdc_archive 'CCDC 754943' #TrackingRef '1.br1422.cif' _audit_creation_date 2008-05-28T16:52:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C40 H27 Co3 O8 P2' _chemical_formula_moiety 'C40 H27 Co3 O8 P2' _chemical_formula_weight 874.35 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 11.8843(2) _cell_length_b 22.8400(5) _cell_length_c 13.6699(3) _cell_angle_alpha 90 _cell_angle_beta 92.498(2) _cell_angle_gamma 90 _cell_volume 3707.00(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20157 _cell_measurement_theta_min 2.8476 _cell_measurement_theta_max 37.1555 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.8341 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0370773247 _diffrn_orient_matrix_ub_12 -0.0163294739 _diffrn_orient_matrix_ub_13 0.0313823539 _diffrn_orient_matrix_ub_21 0.0128732413 _diffrn_orient_matrix_ub_22 0.0256890152 _diffrn_orient_matrix_ub_23 0.0273146702 _diffrn_orient_matrix_ub_31 -0.0448285009 _diffrn_orient_matrix_ub_32 -0.0061084009 _diffrn_orient_matrix_ub_33 0.030828207 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_unetI/netI 0.0717 _diffrn_reflns_number 72467 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 37.23 _diffrn_reflns_theta_full 36.25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 18460 _reflns_number_gt 11625 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0439P)^2^+0.0000P] 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_number_reflns 18460 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.081 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.874 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.221 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.680433(15) 0.586575(8) 0.350607(13) 0.01184(4) Uani 1 1 d . . . Co2 Co 0.556447(15) 0.667402(8) 0.293729(13) 0.01218(4) Uani 1 1 d . . . Co3 Co 0.555123(16) 0.633726(9) 0.466926(13) 0.01336(4) Uani 1 1 d . . . C11 C 0.60212(12) 0.52026(6) 0.32358(10) 0.0162(3) Uani 1 1 d . . . O11 O 0.54967(9) 0.47900(5) 0.30961(9) 0.0231(2) Uani 1 1 d . . . C12 C 0.78833(13) 0.56330(6) 0.43637(11) 0.0169(3) Uani 1 1 d . . . O12 O 0.85883(10) 0.54918(5) 0.49010(8) 0.0253(2) Uani 1 1 d . . . C21 C 0.45867(12) 0.61466(7) 0.24340(11) 0.0182(3) Uani 1 1 d . . . O21 O 0.39619(10) 0.57960(5) 0.21635(9) 0.0266(3) Uani 1 1 d . . . C22 C 0.47184(12) 0.73160(7) 0.30018(11) 0.0187(3) Uani 1 1 d . . . O22 O 0.41596(10) 0.77222(5) 0.30316(9) 0.0297(3) Uani 1 1 d . . . C31 C 0.44749(13) 0.57722(7) 0.46284(10) 0.0185(3) Uani 1 1 d . . . O31 O 0.38316(10) 0.54033(5) 0.46231(9) 0.0268(3) Uani 1 1 d . . . C32 C 0.63438(13) 0.61416(7) 0.57675(11) 0.0193(3) Uani 1 1 d . . . O32 O 0.68635(10) 0.60284(6) 0.64577(8) 0.0301(3) Uani 1 1 d . . . C33 C 0.48369(13) 0.69739(7) 0.51023(11) 0.0200(3) Uani 1 1 d . . . O33 O 0.44001(11) 0.73810(5) 0.53835(9) 0.0305(3) Uani 1 1 d . . . P1 P 0.79646(3) 0.594374(16) 0.23134(3) 0.01214(7) Uani 1 1 d . . . C111 C 0.94040(11) 0.57309(7) 0.26527(10) 0.0149(3) Uani 1 1 d . . . C112 C 1.01948(12) 0.61171(7) 0.30775(11) 0.0188(3) Uani 1 1 d . . . H112 H 1.0008 0.6518 0.316 0.023 Uiso 1 1 calc R . . C113 C 1.12550(13) 0.59133(8) 0.33787(11) 0.0233(3) Uani 1 1 d . . . H113 H 1.1796 0.6177 0.3659 0.028 Uiso 1 1 calc R . . C114 C 1.15298(13) 0.53270(8) 0.32726(11) 0.0239(3) Uani 1 1 d . . . H114 H 1.2261 0.5192 0.3471 0.029 Uiso 1 1 calc R . . C115 C 1.07431(13) 0.49404(8) 0.28788(11) 0.0233(3) Uani 1 1 d . . . H115 H 1.0926 0.4537 0.2822 0.028 Uiso 1 1 calc R . . C116 C 0.96865(12) 0.51384(7) 0.25656(11) 0.0186(3) Uani 1 1 d . . . H116 H 0.915 0.487 0.229 0.022 Uiso 1 1 calc R . . C121 C 0.77535(12) 0.55651(6) 0.11465(10) 0.0145(2) Uani 1 1 d . . . C122 C 0.86212(12) 0.55904(7) 0.04916(11) 0.0197(3) Uani 1 1 d . . . H122 H 0.9309 0.5779 0.0681 0.024 Uiso 1 1 calc R . . C123 C 0.84881(14) 0.53427(8) -0.04349(11) 0.0236(3) Uani 1 1 d . . . H123 H 0.9084 0.5361 -0.0875 0.028 Uiso 1 1 calc R . . C124 C 0.74885(14) 0.50701(7) -0.07132(11) 0.0234(3) Uani 1 1 d . . . H124 H 0.7392 0.4906 -0.135 0.028 Uiso 1 1 calc R . . C125 C 0.66251(13) 0.50349(8) -0.00667(12) 0.0233(3) Uani 1 1 d . . . H125 H 0.5942 0.4842 -0.0257 0.028 Uiso 1 1 calc R . . C126 C 0.67583(12) 0.52821(7) 0.08618(11) 0.0183(3) Uani 1 1 d . . . H126 H 0.6165 0.5257 0.1303 0.022 Uiso 1 1 calc R . . C0 C 0.80360(11) 0.67081(6) 0.19210(10) 0.0133(2) Uani 1 1 d . . . H0A H 0.8451 0.6739 0.1311 0.016 Uiso 1 1 calc R . . H0B H 0.8432 0.6947 0.2433 0.016 Uiso 1 1 calc R . . P2 P 0.65825(3) 0.696754(16) 0.17127(3) 0.01271(7) Uani 1 1 d . . . C211 C 0.67323(12) 0.77582(6) 0.15584(10) 0.0151(3) Uani 1 1 d . . . C212 C 0.76135(13) 0.80728(7) 0.19995(11) 0.0197(3) Uani 1 1 d . . . H212 H 0.8175 0.7875 0.239 0.024 Uiso 1 1 calc R . . C213 C 0.76816(14) 0.86753(7) 0.18750(13) 0.0250(3) Uani 1 1 d . . . H213 H 0.8292 0.8887 0.2175 0.03 Uiso 1 1 calc R . . C214 C 0.68647(15) 0.89676(7) 0.13171(13) 0.0265(3) Uani 1 1 d . . . H214 H 0.6918 0.9379 0.1227 0.032 Uiso 1 1 calc R . . C215 C 0.59687(15) 0.86605(7) 0.08891(12) 0.0268(3) Uani 1 1 d . . . H215 H 0.5398 0.8862 0.0516 0.032 Uiso 1 1 calc R . . C216 C 0.59023(14) 0.80586(7) 0.10046(12) 0.0219(3) Uani 1 1 d . . . H216 H 0.5289 0.7849 0.0705 0.026 Uiso 1 1 calc R . . C221 C 0.61640(12) 0.67480(6) 0.04604(10) 0.0156(3) Uani 1 1 d . . . C222 C 0.69352(13) 0.67690(8) -0.02841(11) 0.0220(3) Uani 1 1 d . . . H222 H 0.7692 0.6884 -0.0136 0.026 Uiso 1 1 calc R . . C223 C 0.65980(14) 0.66232(9) -0.12336(12) 0.0280(4) Uani 1 1 d . . . H223 H 0.7126 0.6631 -0.1735 0.034 Uiso 1 1 calc R . . C224 C 0.54869(14) 0.64660(8) -0.14542(12) 0.0275(4) Uani 1 1 d . . . H224 H 0.5257 0.6367 -0.2108 0.033 Uiso 1 1 calc R . . C225 C 0.47154(13) 0.64522(8) -0.07312(11) 0.0244(3) Uani 1 1 d . . . H225 H 0.3956 0.6346 -0.0886 0.029 Uiso 1 1 calc R . . C226 C 0.50540(12) 0.65950(7) 0.02257(10) 0.0188(3) Uani 1 1 d . . . H226 H 0.4521 0.6588 0.0724 0.023 Uiso 1 1 calc R . . C1 C 0.67388(11) 0.66599(6) 0.39073(10) 0.0126(2) Uani 1 1 d . . . C2 C 0.75980(12) 0.70457(6) 0.43585(10) 0.0159(3) Uani 1 1 d . . . O2 O 0.86071(9) 0.69249(5) 0.43757(9) 0.0292(3) Uani 1 1 d . . . C201 C 0.72242(12) 0.75875(6) 0.48776(10) 0.0160(3) Uani 1 1 d . . . C202 C 0.74622(13) 0.76303(7) 0.58799(11) 0.0203(3) Uani 1 1 d . . . H202 H 0.7853 0.7322 0.6216 0.024 Uiso 1 1 calc R . . C203 C 0.71302(14) 0.81220(7) 0.63921(12) 0.0243(3) Uani 1 1 d . . . H203 H 0.7273 0.8144 0.708 0.029 Uiso 1 1 calc R . . C204 C 0.65930(14) 0.85796(7) 0.59037(12) 0.0245(3) Uani 1 1 d . . . H204 H 0.6376 0.8917 0.6255 0.029 Uiso 1 1 calc R . . C205 C 0.63712(14) 0.85457(7) 0.49013(12) 0.0240(3) Uani 1 1 d . . . H205 H 0.6017 0.8863 0.4561 0.029 Uiso 1 1 calc R . . C206 C 0.66695(13) 0.80448(7) 0.43955(11) 0.0192(3) Uani 1 1 d . . . H206 H 0.6491 0.8016 0.3713 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01199(8) 0.01178(9) 0.01185(8) -0.00044(7) 0.00162(6) -0.00016(7) Co2 0.01129(8) 0.01317(9) 0.01207(8) -0.00024(7) 0.00032(6) -0.00015(7) Co3 0.01325(8) 0.01483(9) 0.01217(8) -0.00053(7) 0.00253(6) -0.00017(7) C11 0.0160(6) 0.0169(7) 0.0160(6) 0.0002(5) 0.0028(5) 0.0022(5) O11 0.0223(5) 0.0172(5) 0.0300(6) -0.0016(4) 0.0018(4) -0.0033(4) C12 0.0197(7) 0.0144(7) 0.0168(6) -0.0004(5) 0.0048(5) 0.0001(5) O12 0.0236(6) 0.0322(7) 0.0199(5) 0.0046(5) -0.0014(4) 0.0026(5) C21 0.0169(7) 0.0198(7) 0.0177(7) 0.0027(5) 0.0001(5) 0.0013(5) O21 0.0252(6) 0.0230(6) 0.0309(6) 0.0023(5) -0.0068(5) -0.0070(5) C22 0.0171(7) 0.0212(7) 0.0178(7) 0.0004(5) 0.0005(5) -0.0004(5) O22 0.0285(6) 0.0273(7) 0.0332(7) -0.0015(5) -0.0007(5) 0.0124(5) C31 0.0182(7) 0.0238(8) 0.0136(6) 0.0003(5) 0.0016(5) 0.0003(6) O31 0.0251(6) 0.0294(6) 0.0258(6) 0.0027(5) -0.0010(5) -0.0103(5) C32 0.0192(7) 0.0216(7) 0.0174(7) -0.0031(6) 0.0058(5) -0.0001(6) O32 0.0291(6) 0.0441(8) 0.0167(5) 0.0000(5) -0.0021(5) 0.0063(5) C33 0.0205(7) 0.0207(7) 0.0194(7) 0.0002(6) 0.0059(5) -0.0010(6) O33 0.0328(7) 0.0254(6) 0.0344(7) -0.0031(5) 0.0143(5) 0.0074(5) P1 0.01093(15) 0.01341(16) 0.01214(15) -0.00074(12) 0.00122(11) -0.00051(12) C111 0.0119(6) 0.0198(7) 0.0132(6) 0.0017(5) 0.0024(5) 0.0010(5) C112 0.0152(6) 0.0236(8) 0.0175(7) 0.0001(6) 0.0007(5) -0.0019(5) C113 0.0166(7) 0.0344(9) 0.0188(7) 0.0033(6) -0.0021(5) -0.0043(6) C114 0.0142(7) 0.0377(10) 0.0199(7) 0.0077(7) 0.0015(5) 0.0052(6) C115 0.0225(8) 0.0269(8) 0.0206(7) 0.0036(6) 0.0019(6) 0.0096(6) C116 0.0173(7) 0.0219(7) 0.0168(6) 0.0006(5) 0.0017(5) 0.0019(6) C121 0.0150(6) 0.0134(6) 0.0152(6) -0.0030(5) -0.0003(5) 0.0010(5) C122 0.0153(6) 0.0262(8) 0.0176(7) -0.0047(6) 0.0026(5) -0.0036(6) C123 0.0206(7) 0.0316(9) 0.0189(7) -0.0070(6) 0.0058(6) -0.0005(6) C124 0.0256(8) 0.0270(8) 0.0177(7) -0.0094(6) 0.0017(6) -0.0004(6) C125 0.0190(7) 0.0281(8) 0.0227(7) -0.0091(6) -0.0004(6) -0.0057(6) C126 0.0154(6) 0.0222(7) 0.0173(6) -0.0032(5) 0.0011(5) -0.0019(5) C0 0.0124(6) 0.0140(6) 0.0135(6) 0.0002(5) 0.0001(4) -0.0022(5) P2 0.01261(15) 0.01367(17) 0.01179(15) 0.00027(12) -0.00015(12) -0.00065(12) C211 0.0171(6) 0.0151(6) 0.0132(6) 0.0019(5) 0.0022(5) 0.0000(5) C212 0.0202(7) 0.0161(7) 0.0227(7) 0.0011(6) -0.0018(5) -0.0014(5) C213 0.0263(8) 0.0170(7) 0.0315(8) 0.0002(6) 0.0002(6) -0.0059(6) C214 0.0346(9) 0.0142(7) 0.0312(9) 0.0034(6) 0.0074(7) 0.0011(6) C215 0.0314(9) 0.0222(8) 0.0265(8) 0.0070(7) -0.0009(6) 0.0069(7) C216 0.0228(7) 0.0202(8) 0.0224(7) 0.0034(6) -0.0030(6) 0.0017(6) C221 0.0150(6) 0.0172(7) 0.0145(6) -0.0002(5) -0.0005(5) 0.0004(5) C222 0.0157(7) 0.0353(9) 0.0149(6) -0.0006(6) 0.0000(5) -0.0049(6) C223 0.0211(8) 0.0476(11) 0.0155(7) -0.0054(7) 0.0035(6) -0.0044(7) C224 0.0233(8) 0.0443(11) 0.0147(7) -0.0061(7) -0.0020(6) -0.0031(7) C225 0.0158(7) 0.0380(10) 0.0191(7) -0.0038(7) -0.0027(5) -0.0016(6) C226 0.0154(6) 0.0260(8) 0.0150(6) 0.0000(6) -0.0001(5) 0.0011(6) C1 0.0113(5) 0.0128(6) 0.0137(6) -0.0010(5) 0.0016(4) 0.0014(5) C2 0.0155(6) 0.0173(7) 0.0148(6) -0.0031(5) -0.0002(5) -0.0017(5) O2 0.0142(5) 0.0316(7) 0.0415(7) -0.0172(6) -0.0033(5) 0.0014(5) C201 0.0130(6) 0.0175(7) 0.0175(6) -0.0040(5) 0.0013(5) -0.0033(5) C202 0.0190(7) 0.0197(7) 0.0222(7) -0.0046(6) -0.0011(5) -0.0017(6) C203 0.0250(8) 0.0269(8) 0.0210(7) -0.0103(6) 0.0017(6) -0.0042(6) C204 0.0239(8) 0.0219(8) 0.0283(8) -0.0101(6) 0.0061(6) -0.0026(6) C205 0.0267(8) 0.0174(7) 0.0281(8) -0.0018(6) 0.0038(6) 0.0021(6) C206 0.0198(7) 0.0192(7) 0.0186(7) -0.0016(5) 0.0021(5) -0.0012(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.7805(15) . ? Co1 C11 1.8074(15) . ? Co1 C1 1.8976(14) . ? Co1 P1 2.1880(4) . ? Co1 Co2 2.4665(3) . ? Co1 Co3 2.4723(3) . ? Co2 C22 1.7823(16) . ? Co2 C21 1.7903(16) . ? Co2 C1 1.8830(13) . ? Co2 P2 2.2118(4) . ? Co2 Co3 2.4901(3) . ? Co3 C32 1.7938(16) . ? Co3 C33 1.7970(16) . ? Co3 C31 1.8162(16) . ? Co3 C1 1.9360(13) . ? C11 O11 1.1414(18) . ? C12 O12 1.1366(18) . ? C21 O21 1.1425(18) . ? C22 O22 1.1427(18) . ? C31 O31 1.1374(18) . ? C32 O32 1.1347(18) . ? C33 O33 1.1400(18) . ? P1 C111 1.8189(14) . ? P1 C121 1.8222(14) . ? P1 C0 1.8294(14) . ? C111 C112 1.397(2) . ? C111 C116 1.401(2) . ? C112 C113 1.389(2) . ? C112 H112 0.95 . ? C113 C114 1.387(2) . ? C113 H113 0.95 . ? C114 C115 1.378(2) . ? C114 H114 0.95 . ? C115 C116 1.385(2) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.388(2) . ? C121 C122 1.396(2) . ? C122 C123 1.390(2) . ? C122 H122 0.95 . ? C123 C124 1.380(2) . ? C123 H123 0.95 . ? C124 C125 1.385(2) . ? C124 H124 0.95 . ? C125 C126 1.392(2) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C0 P2 1.8366(14) . ? C0 H0A 0.99 . ? C0 H0B 0.99 . ? P2 C211 1.8278(15) . ? P2 C221 1.8316(14) . ? C211 C212 1.386(2) . ? C211 C216 1.397(2) . ? C212 C213 1.389(2) . ? C212 H212 0.95 . ? C213 C214 1.380(2) . ? C213 H213 0.95 . ? C214 C215 1.383(3) . ? C214 H214 0.95 . ? C215 C216 1.386(2) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.389(2) . ? C221 C222 1.400(2) . ? C222 C223 1.382(2) . ? C222 H222 0.95 . ? C223 C224 1.389(2) . ? C223 H223 0.95 . ? C224 C225 1.378(2) . ? C224 H224 0.95 . ? C225 C226 1.390(2) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C1 C2 1.4644(19) . ? C2 O2 1.2298(18) . ? C2 C201 1.503(2) . ? C201 C206 1.386(2) . ? C201 C202 1.390(2) . ? C202 C203 1.390(2) . ? C202 H202 0.95 . ? C203 C204 1.382(2) . ? C203 H203 0.95 . ? C204 C205 1.386(2) . ? C204 H204 0.95 . ? C205 C206 1.391(2) . ? C205 H205 0.95 . ? C206 H206 0.95 . ? 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 C12 Co1 C11 103.53(7) . . ? C12 Co1 C1 97.62(6) . . ? C11 Co1 C1 146.39(6) . . ? C12 Co1 P1 93.20(5) . . ? C11 Co1 P1 104.57(5) . . ? C1 Co1 P1 99.95(4) . . ? C12 Co1 Co2 146.53(5) . . ? C11 Co1 Co2 105.52(5) . . ? C1 Co1 Co2 49.02(4) . . ? P1 Co1 Co2 95.244(12) . . ? C12 Co1 Co3 98.24(5) . . ? C11 Co1 Co3 100.21(4) . . ? C1 Co1 Co3 50.52(4) . . ? P1 Co1 Co3 149.388(14) . . ? Co2 Co1 Co3 60.555(8) . . ? C22 Co2 C21 102.39(7) . . ? C22 Co2 C1 112.43(6) . . ? C21 Co2 C1 135.06(6) . . ? C22 Co2 P2 96.69(5) . . ? C21 Co2 P2 106.28(5) . . ? C1 Co2 P2 97.19(4) . . ? C22 Co2 Co1 158.55(5) . . ? C21 Co2 Co1 89.22(5) . . ? C1 Co2 Co1 49.53(4) . . ? P2 Co2 Co1 97.266(12) . . ? C22 Co2 Co3 100.38(5) . . ? C21 Co2 Co3 97.27(5) . . ? C1 Co2 Co3 50.23(4) . . ? P2 Co2 Co3 147.095(13) . . ? Co1 Co2 Co3 59.837(8) . . ? C32 Co3 C33 99.46(7) . . ? C32 Co3 C31 101.08(7) . . ? C33 Co3 C31 104.06(7) . . ? C32 Co3 C1 100.17(6) . . ? C33 Co3 C1 103.60(6) . . ? C31 Co3 C1 141.53(6) . . ? C32 Co3 Co1 96.93(5) . . ? C33 Co3 Co1 150.55(5) . . ? C31 Co3 Co1 96.54(5) . . ? C1 Co3 Co1 49.17(4) . . ? C32 Co3 Co2 147.98(5) . . ? C33 Co3 Co2 94.93(5) . . ? C31 Co3 Co2 102.94(5) . . ? C1 Co3 Co2 48.39(4) . . ? Co1 Co3 Co2 59.608(7) . . ? O11 C11 Co1 177.08(13) . . ? O12 C12 Co1 178.51(14) . . ? O21 C21 Co2 176.18(14) . . ? O22 C22 Co2 178.62(15) . . ? O31 C31 Co3 177.16(14) . . ? O32 C32 Co3 178.32(15) . . ? O33 C33 Co3 178.88(16) . . ? C111 P1 C121 100.86(6) . . ? C111 P1 C0 105.94(6) . . ? C121 P1 C0 101.69(6) . . ? C111 P1 Co1 113.86(5) . . ? C121 P1 Co1 123.12(5) . . ? C0 P1 Co1 109.57(5) . . ? C112 C111 C116 119.08(13) . . ? C112 C111 P1 123.06(11) . . ? C116 C111 P1 117.57(11) . . ? C113 C112 C111 119.79(15) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C114 C113 C112 120.48(15) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 120.02(14) . . ? C115 C114 H114 120 . . ? C113 C114 H114 120 . . ? C114 C115 C116 120.14(16) . . ? C114 C115 H115 119.9 . . ? C116 C115 H115 119.9 . . ? C115 C116 C111 120.45(15) . . ? C115 C116 H116 119.8 . . ? C111 C116 H116 119.8 . . ? C126 C121 C122 118.92(13) . . ? C126 C121 P1 123.32(11) . . ? # Attachment '2.br1429.cif' data_br1429 _database_code_depnum_ccdc_archive 'CCDC 754944' #TrackingRef '2.br1429.cif' _audit_creation_date 2008-09-05T17:02:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H31 Co3 Fe O8 P2' _chemical_formula_moiety 'C44 H31 Co3 Fe O8 P2' _chemical_formula_weight 982.27 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall P_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 14.3318(3) _cell_length_b 16.2488(3) _cell_length_c 51.1493(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11911.4(4) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9839 _cell_measurement_theta_min 2.5894 _cell_measurement_theta_max 67.1938 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5952 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.46669 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.1363 _diffrn_reflns_av_unetI/netI 0.1236 _diffrn_reflns_number 108494 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 67.3 _diffrn_reflns_theta_full 67.3 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 21075 _reflns_number_gt 12790 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0849P)^2^+0.0000P] 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_number_reflns 21075 _refine_ls_number_parameters 1556 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.098 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 0.82 _refine_ls_restrained_S_all 0.82 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.273(4) _refine_diff_density_max 0.502 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.42306(7) 0.63784(6) 0.169079(18) 0.0192(2) Uani 1 1 d . . . Co2 Co 0.59356(7) 0.63284(6) 0.163676(19) 0.0187(2) Uani 1 1 d . . . Co3 Co 0.51790(7) 0.75849(6) 0.18182(2) 0.0221(2) Uani 1 1 d . . . Co4 Co -0.10014(7) 0.37639(6) 0.336840(19) 0.0191(2) Uani 1 1 d . . . Co5 Co 0.07100(7) 0.36864(6) 0.332504(18) 0.0190(2) Uani 1 1 d . . . Co6 Co -0.01540(7) 0.25006(6) 0.351075(19) 0.0211(2) Uani 1 1 d . . . Co7 Co 0.55365(7) 0.63778(6) 0.505899(18) 0.0193(2) Uani 1 1 d . . . Co8 Co 0.38364(6) 0.63115(6) 0.49924(2) 0.0208(2) Uani 1 1 d . . . Co9 Co 0.45934(7) 0.76189(6) 0.51271(2) 0.0219(3) Uani 1 1 d . . . Fe1 Fe 0.46124(8) 0.64565(7) 0.275193(19) 0.0271(3) Uani 1 1 d . A . Fe2 Fe -0.06396(8) 0.35386(6) 0.443069(19) 0.0259(3) Uani 1 1 d . . . Fe3 Fe 0.52014(7) 0.63815(7) 0.608338(19) 0.0268(3) Uani 1 1 d . . . C11 C 0.3993(5) 0.6654(4) 0.13578(13) 0.0249(16) Uani 1 1 d . . . O11 O 0.3868(3) 0.6855(3) 0.11460(9) 0.0333(13) Uani 1 1 d . . . C12 C 0.3158(5) 0.6682(4) 0.18382(14) 0.0292(18) Uani 1 1 d . . . O12 O 0.2462(4) 0.6889(3) 0.19252(10) 0.0426(14) Uani 1 1 d . . . C21 C 0.6038(5) 0.6555(4) 0.12893(14) 0.0301(18) Uani 1 1 d . . . O21 O 0.6081(4) 0.6742(3) 0.10781(9) 0.0449(15) Uani 1 1 d . . . C22 C 0.7076(5) 0.6550(4) 0.17529(13) 0.0285(17) Uani 1 1 d . . . O22 O 0.7823(3) 0.6692(3) 0.18288(10) 0.0360(13) Uani 1 1 d . . . C31 C 0.5185(5) 0.8147(4) 0.15085(14) 0.0317(18) Uani 1 1 d . . . O31 O 0.5167(4) 0.8469(3) 0.13154(10) 0.0442(15) Uani 1 1 d . . . C32 C 0.4269(5) 0.8105(4) 0.19977(13) 0.0312(18) Uani 1 1 d . . . O32 O 0.3716(4) 0.8456(3) 0.21093(11) 0.0546(17) Uani 1 1 d . . . C33 C 0.6176(5) 0.7992(4) 0.19861(13) 0.0315(18) Uani 1 1 d . . . O33 O 0.6787(4) 0.8270(3) 0.20959(11) 0.0526(17) Uani 1 1 d . . . P1 P 0.40242(11) 0.50445(10) 0.17081(3) 0.0200(4) Uani 1 1 d . . . C111 C 0.3066(4) 0.4704(4) 0.19175(13) 0.0209(15) Uani 1 1 d . . . C112 C 0.3181(5) 0.4289(5) 0.21509(14) 0.036(2) Uani 1 1 d . . . H112 H 0.3792 0.4153 0.2208 0.043 Uiso 1 1 calc R . . C113 C 0.2430(5) 0.4068(5) 0.23015(15) 0.040(2) Uani 1 1 d . . . H113 H 0.2521 0.3769 0.2459 0.048 Uiso 1 1 calc R . . C114 C 0.1534(6) 0.4284(5) 0.22222(16) 0.046(2) Uani 1 1 d . . . H114 H 0.1011 0.4131 0.2325 0.056 Uiso 1 1 calc R . . C115 C 0.1409(5) 0.4719(5) 0.19935(16) 0.046(2) Uani 1 1 d . . . H115 H 0.0799 0.4878 0.1942 0.055 Uiso 1 1 calc R . . C116 C 0.2171(5) 0.4927(5) 0.18383(15) 0.038(2) Uani 1 1 d . . . H116 H 0.2081 0.5218 0.1679 0.045 Uiso 1 1 calc R . . C121 C 0.3813(5) 0.4424(4) 0.14136(13) 0.0292(17) Uani 1 1 d . . . C122 C 0.3373(5) 0.3666(5) 0.14410(16) 0.049(2) Uani 1 1 d . . . H122 H 0.3162 0.349 0.1608 0.059 Uiso 1 1 calc R . . C123 C 0.3243(6) 0.3167(6) 0.12226(19) 0.067(3) Uani 1 1 d . . . H123 H 0.2934 0.2652 0.124 0.08 Uiso 1 1 calc R . . C124 C 0.3557(7) 0.3415(6) 0.09871(19) 0.068(3) Uani 1 1 d . . . H124 H 0.3469 0.3069 0.0839 0.082 Uiso 1 1 calc R . . C125 C 0.4007(6) 0.4165(5) 0.09563(15) 0.056(3) Uani 1 1 d . . . H125 H 0.423 0.4328 0.0789 0.067 Uiso 1 1 calc R . . C126 C 0.4128(6) 0.4673(5) 0.11703(13) 0.043(2) Uani 1 1 d . . . H126 H 0.4427 0.5191 0.1151 0.051 Uiso 1 1 calc R . . C10 C 0.5060(4) 0.4557(4) 0.18469(12) 0.0206(15) Uani 1 1 d . . . H10A H 0.503 0.3953 0.1822 0.025 Uiso 1 1 calc R . . H10B H 0.5099 0.4673 0.2037 0.025 Uiso 1 1 calc R . . P2 P 0.60865(12) 0.49797(10) 0.16776(3) 0.0197(4) Uani 1 1 d . . . C211 C 0.7074(5) 0.4641(4) 0.18753(13) 0.0264(17) Uani 1 1 d . . . C212 C 0.6986(5) 0.4387(4) 0.21336(14) 0.0340(19) Uani 1 1 d . . . H212 H 0.6384 0.4362 0.2211 0.041 Uiso 1 1 calc R . . C213 C 0.7754(6) 0.4170(5) 0.22802(17) 0.047(2) Uani 1 1 d . . . H213 H 0.7679 0.399 0.2456 0.057 Uiso 1 1 calc R . . C214 C 0.8629(6) 0.4215(5) 0.21714(18) 0.056(3) Uani 1 1 d . . . H214 H 0.9161 0.4067 0.2272 0.067 Uiso 1 1 calc R . . C215 C 0.8738(6) 0.4478(6) 0.19141(19) 0.062(3) Uani 1 1 d . . . H215 H 0.9342 0.4514 0.1838 0.075 Uiso 1 1 calc R . . C216 C 0.7952(5) 0.4687(5) 0.17692(16) 0.044(2) Uani 1 1 d . . . H216 H 0.8024 0.4866 0.1593 0.053 Uiso 1 1 calc R . . C221 C 0.6247(5) 0.4330(4) 0.13873(12) 0.0246(16) Uani 1 1 d . . . C222 C 0.5988(5) 0.3512(4) 0.13854(13) 0.0324(18) Uani 1 1 d . . . H222 H 0.5716 0.3278 0.1537 0.039 Uiso 1 1 calc R . . C223 C 0.6117(5) 0.3025(4) 0.11645(14) 0.039(2) Uani 1 1 d . . . H223 H 0.5908 0.2471 0.1163 0.047 Uiso 1 1 calc R . . C224 C 0.6547(5) 0.3351(4) 0.09496(14) 0.037(2) Uani 1 1 d . . . H224 H 0.6651 0.3016 0.08 0.044 Uiso 1 1 calc R . . C225 C 0.6827(5) 0.4149(4) 0.09482(14) 0.0357(19) Uani 1 1 d . . . H225 H 0.7118 0.4373 0.0797 0.043 Uiso 1 1 calc R . . C226 C 0.6687(5) 0.4642(4) 0.11688(14) 0.037(2) Uani 1 1 d . . . H226 H 0.6896 0.5197 0.1168 0.044 Uiso 1 1 calc R . . C1 C 0.5191(4) 0.6456(4) 0.19461(12) 0.0197(14) Uani 1 1 d . A . C2 C 0.5507(5) 0.6213(4) 0.22056(12) 0.0251(16) Uani 1 1 d . . . O2 O 0.6339(3) 0.6233(3) 0.22612(9) 0.0394(14) Uani 1 1 d . A . C101 C 0.4841(5) 0.5894(4) 0.24036(13) 0.0269(17) Uani 1 1 d . A . C102 C 0.5138(6) 0.5376(4) 0.26213(13) 0.0348(19) Uani 1 1 d . A . H102 H 0.5753 0.5178 0.2651 0.042 Uiso 1 1 calc R . . C103 C 0.4353(6) 0.5221(5) 0.27808(14) 0.043(2) Uani 1 1 d . A . H103 H 0.4353 0.4897 0.2935 0.051 Uiso 1 1 calc R . . C104 C 0.3567(6) 0.5626(5) 0.26741(14) 0.046(2) Uani 1 1 d . . . H104 H 0.2954 0.5631 0.2745 0.055 Uiso 1 1 calc R A . C105 C 0.3865(5) 0.6026(5) 0.24400(13) 0.0355(19) Uani 1 1 d . A . H105 H 0.3474 0.6333 0.2326 0.043 Uiso 1 1 calc R . . C201 C 0.5492(9) 0.7451(7) 0.2753(3) 0.042(3) Uiso 0.638(10) 1 d P A 1 H201 H 0.5954 0.7562 0.2625 0.05 Uiso 0.638(10) 1 calc PR A 1 C202 C 0.5616(9) 0.6968(7) 0.2993(2) 0.037(3) Uiso 0.638(10) 1 d P A 1 H202 H 0.6167 0.6704 0.3053 0.044 Uiso 0.638(10) 1 calc PR A 1 C203 C 0.4740(10) 0.6984(8) 0.3112(3) 0.035(3) Uiso 0.638(10) 1 d P A 1 H203 H 0.4609 0.6722 0.3274 0.042 Uiso 0.638(10) 1 calc PR A 1 C204 C 0.4074(8) 0.7427(7) 0.2969(2) 0.027(3) Uiso 0.638(10) 1 d P A 1 H204 H 0.3435 0.7516 0.301 0.032 Uiso 0.638(10) 1 calc PR A 1 C205 C 0.4586(10) 0.7712(8) 0.2749(3) 0.039(3) Uiso 0.638(10) 1 d P A 1 H205 H 0.4327 0.8044 0.2614 0.047 Uiso 0.638(10) 1 calc PR A 1 C301 C 0.5007(16) 0.7626(13) 0.2710(4) 0.029(5) Uiso 0.362(10) 1 d P A 2 H301 H 0.5232 0.7872 0.2554 0.035 Uiso 0.362(10) 1 calc PR A 2 C302 C 0.5570(13) 0.7224(10) 0.2895(4) 0.016(4) Uiso 0.362(10) 1 d P A 2 H302 H 0.6229 0.7179 0.2882 0.019 Uiso 0.362(10) 1 calc PR A 2 C303 C 0.5018(18) 0.6882(15) 0.3112(5) 0.037(7) Uiso 0.362(10) 1 d P A 2 H303 H 0.5228 0.6575 0.3258 0.044 Uiso 0.362(10) 1 calc PR A 2 C304 C 0.4108(19) 0.7122(15) 0.3049(5) 0.047(7) Uiso 0.362(10) 1 d P A 2 H304 H 0.3568 0.7007 0.315 0.056 Uiso 0.362(10) 1 calc PR A 2 C305 C 0.4118(18) 0.7616(15) 0.2783(5) 0.046(6) Uiso 0.362(10) 1 d P A 2 H305 H 0.3601 0.7853 0.2695 0.055 Uiso 0.362(10) 1 calc PR A 2 C41 C -0.1141(5) 0.3527(4) 0.30273(12) 0.0271(16) Uani 1 1 d . . . O41 O -0.1207(4) 0.3357(3) 0.28115(9) 0.0382(14) Uani 1 1 d . . . C42 C -0.2128(5) 0.3543(4) 0.34941(13) 0.0283(17) Uani 1 1 d . . . O42 O -0.2857(3) 0.3381(3) 0.35668(10) 0.0423(15) Uani 1 1 d . . . C51 C 0.1802(5) 0.3412(4) 0.34660(12) 0.0255(17) Uani 1 1 d . . . O51 O 0.2512(3) 0.3227(3) 0.35544(10) 0.0347(13) Uani 1 1 d . . . C52 C 0.0926(5) 0.3403(4) 0.29861(13) 0.0280(17) Uani 1 1 d . . . O52 O 0.1040(4) 0.3209(3) 0.27753(9) 0.0386(14) Uani 1 1 d . . . C61 C -0.0137(5) 0.1936(4) 0.31999(14) 0.0287(17) Uani 1 1 d . . . O61 O -0.0099(4) 0.1581(3) 0.30124(10) 0.0466(15) Uani 1 1 d . . . C62 C 0.0778(5) 0.2034(4) 0.36919(13) 0.0271(17) Uani 1 1 d . . . O62 O 0.1360(4) 0.1754(3) 0.38137(11) 0.0490(16) Uani 1 1 d . . . C63 C -0.1124(5) 0.2033(4) 0.36705(14) 0.0327(18) Uani 1 1 d . . . O63 O -0.1732(4) 0.1720(3) 0.37743(12) 0.0590(18) Uani 1 1 d . . . P4 P -0.11210(11) 0.51079(10) 0.33986(3) 0.0189(4) Uani 1 1 d . . . C411 C -0.2021(5) 0.5505(4) 0.36206(13) 0.0259(17) Uani 1 1 d . . . C412 C -0.1842(5) 0.5822(4) 0.38646(12) 0.0275(17) Uani 1 1 d . . . H412 H -0.1219 0.5851 0.3927 0.033 Uiso 1 1 calc R . . C413 C -0.2582(5) 0.6103(4) 0.40209(14) 0.0358(19) Uani 1 1 d . . . H413 H -0.2453 0.6326 0.4189 0.043 Uiso 1 1 calc R . . C414 C -0.3483(5) 0.6061(5) 0.39357(14) 0.039(2) Uani 1 1 d . . . H414 H -0.3978 0.6257 0.4042 0.046 Uiso 1 1 calc R . . C415 C -0.3665(5) 0.5726(5) 0.36893(15) 0.044(2) Uani 1 1 d . . . H415 H -0.429 0.5686 0.3628 0.053 Uiso 1 1 calc R . . C416 C -0.2948(5) 0.5456(5) 0.35361(15) 0.040(2) Uani 1 1 d . . . H416 H -0.3081 0.523 0.3369 0.048 Uiso 1 1 calc R . . C421 C -0.1384(5) 0.5745(4) 0.31094(12) 0.0224(16) Uani 1 1 d . . . C422 C -0.1139(5) 0.6557(4) 0.31020(13) 0.0352(19) Uani 1 1 d . . . H422 H -0.0819 0.6797 0.3246 0.042 Uiso 1 1 calc R . . C423 C -0.1358(6) 0.7038(5) 0.28835(16) 0.052(2) Uani 1 1 d . . . H423 H -0.1158 0.7595 0.2875 0.062 Uiso 1 1 calc R . . C424 C -0.1864(5) 0.6700(5) 0.26814(15) 0.039(2) Uani 1 1 d . . . H424 H -0.2043 0.7036 0.2538 0.047 Uiso 1 1 calc R . . C425 C -0.2109(6) 0.5898(5) 0.26848(14) 0.041(2) Uani 1 1 d . . . H425 H -0.2439 0.5664 0.2542 0.049 Uiso 1 1 calc R . . C426 C -0.1872(5) 0.5412(4) 0.29021(14) 0.0316(18) Uani 1 1 d . . . H426 H -0.2049 0.4848 0.2906 0.038 Uiso 1 1 calc R . . C20 C -0.0016(4) 0.5525(4) 0.35232(12) 0.0207(15) Uani 1 1 d . . . H20A H 0.0008 0.6127 0.3495 0.025 Uiso 1 1 calc R . . H20B H 0.0039 0.5417 0.3713 0.025 Uiso 1 1 calc R . . P5 P 0.09330(11) 0.50228(10) 0.33476(3) 0.0192(4) Uani 1 1 d . . . C511 C 0.1981(5) 0.5329(4) 0.35249(13) 0.0225(16) Uani 1 1 d . . . C512 C 0.1954(5) 0.5740(4) 0.37648(13) 0.0277(17) Uani 1 1 d . . . H512 H 0.1373 0.5894 0.384 0.033 Uiso 1 1 calc R . . C513 C 0.2783(5) 0.5922(5) 0.38934(15) 0.041(2) Uani 1 1 d . . . H513 H 0.2765 0.6201 0.4057 0.049 Uiso 1 1 calc R . . C514 C 0.3627(5) 0.5706(5) 0.37875(15) 0.038(2) Uani 1 1 d . . . H514 H 0.4189 0.5829 0.3878 0.046 Uiso 1 1 calc R . . C515 C 0.3660(5) 0.5303(5) 0.35464(15) 0.040(2) Uani 1 1 d . . . H515 H 0.4242 0.5151 0.3472 0.048 Uiso 1 1 calc R . . C516 C 0.2831(5) 0.5127(4) 0.34173(15) 0.0323(18) Uani 1 1 d . . . H516 H 0.2851 0.4862 0.3252 0.039 Uiso 1 1 calc R . . C521 C 0.1016(5) 0.5654(4) 0.30507(13) 0.0272(17) Uani 1 1 d . . . C522 C 0.1404(5) 0.6434(4) 0.30645(15) 0.038(2) Uani 1 1 d . . . H522 H 0.1681 0.6619 0.3223 0.046 Uiso 1 1 calc R . . C523 C 0.1388(6) 0.6947(5) 0.28455(16) 0.049(2) Uani 1 1 d . . . H523 H 0.1637 0.7488 0.2855 0.059 Uiso 1 1 calc R . . C524 C 0.1011(7) 0.6663(5) 0.26183(15) 0.056(3) Uani 1 1 d . . . H524 H 0.1017 0.7005 0.2468 0.067 Uiso 1 1 calc R . . C525 C 0.0625(7) 0.5897(5) 0.26028(14) 0.052(2) Uani 1 1 d . . . H525 H 0.035 0.5714 0.2444 0.062 Uiso 1 1 calc R . . C526 C 0.0638(5) 0.5395(4) 0.28171(13) 0.0333(18) Uani 1 1 d . . . H526 H 0.0381 0.4858 0.2805 0.04 Uiso 1 1 calc R . . C3 C -0.0070(4) 0.3632(4) 0.36247(12) 0.0193(14) Uani 1 1 d . B . C4 C 0.0238(4) 0.3899(4) 0.38886(12) 0.0222(15) Uani 1 1 d . . . O4 O 0.1078(3) 0.3935(3) 0.39381(9) 0.0384(14) Uani 1 1 d . B . C401 C -0.0429(5) 0.4161(4) 0.40914(12) 0.0216(15) Uani 1 1 d . B . C402 C -0.0146(5) 0.4647(4) 0.43139(13) 0.0315(18) Uani 1 1 d . B . H402 H 0.0465 0.4854 0.4344 0.038 Uiso 1 1 calc R . . C403 C -0.0912(5) 0.4765(4) 0.44775(14) 0.0346(19) Uani 1 1 d . B . H403 H -0.0912 0.5059 0.4638 0.042 Uiso 1 1 calc R . . C404 C -0.1690(5) 0.4369(4) 0.43617(14) 0.0350(19) Uani 1 1 d . B . H404 H -0.2306 0.4355 0.4431 0.042 Uiso 1 1 calc R . . C405 C -0.1397(4) 0.4000(3) 0.41280(11) 0.0289(17) Uani 1 1 d . B . H405 H -0.1782 0.3692 0.4013 0.035 Uiso 1 1 calc R . . C501 C 0.0359(4) 0.2586(3) 0.44346(11) 0.025(3) Uiso 0.586(11) 1 d PRD B 1 H501 H 0.0879 0.2516 0.4322 0.03 Uiso 0.586(11) 1 d PR B 1 C502 C 0.0340(8) 0.3019(8) 0.4676(2) 0.033(3) Uiso 0.586(11) 1 d PD B 1 H502 H 0.0858 0.329 0.4754 0.04 Uiso 0.586(11) 1 calc PR B 1 C503 C -0.0597(9) 0.2984(7) 0.4786(2) 0.031(3) Uiso 0.586(11) 1 d PD B 1 H503 H -0.0803 0.3237 0.4943 0.037 Uiso 0.586(11) 1 calc PR B 1 C504 C -0.1142(8) 0.2498(8) 0.4613(2) 0.036(3) Uiso 0.586(11) 1 d PD B 1 H504 H -0.1777 0.2347 0.4636 0.043 Uiso 0.586(11) 1 calc PR B 1 C505 C -0.0558(8) 0.2282(6) 0.4401(2) 0.022(3) Uiso 0.586(11) 1 d PD B 1 H505 H -0.0757 0.1971 0.4254 0.027 Uiso 0.586(11) 1 calc PR B 1 C601 C -0.0011(10) 0.2423(10) 0.4390(3) 0.033(5) Uiso 0.414(11) 1 d PD B 2 H601 H 0.0303 0.222 0.424 0.04 Uiso 0.414(11) 1 calc PR B 2 C602 C 0.0405(11) 0.2860(13) 0.4599(4) 0.052(7) Uiso 0.414(11) 1 d PD B 2 H602 H 0.1042 0.302 0.4609 0.063 Uiso 0.414(11) 1 calc PR B 2 C603 C -0.0301(11) 0.3023(10) 0.4792(3) 0.022(4) Uiso 0.414(11) 1 d PD B 2 H603 H -0.0216 0.3289 0.4956 0.026 Uiso 0.414(11) 1 calc PR B 2 C604 C -0.1152(9) 0.2706(11) 0.4690(3) 0.029(5) Uiso 0.414(11) 1 d PD B 2 H604 H -0.1744 0.2737 0.4773 0.035 Uiso 0.414(11) 1 calc PR B 2 C605 C -0.0974(12) 0.2338(11) 0.4443(3) 0.044(5) Uiso 0.414(11) 1 d PD B 2 H605 H -0.1422 0.208 0.4334 0.053 Uiso 0.414(11) 1 calc PR B 2 C71 C 0.5870(5) 0.6670(4) 0.47290(13) 0.0245(16) Uani 1 1 d . . . O71 O 0.6037(3) 0.6880(3) 0.45255(9) 0.0316(12) Uani 1 1 d . . . C72 C 0.6553(5) 0.6645(4) 0.52414(13) 0.0263(17) Uani 1 1 d . . . O72 O 0.7199(4) 0.6829(3) 0.53590(10) 0.0415(14) Uani 1 1 d . . . C81 C 0.3829(5) 0.6480(4) 0.46459(13) 0.0267(16) Uani 1 1 d . . . O81 O 0.3860(4) 0.6613(3) 0.44259(9) 0.0422(15) Uani 1 1 d . . . C82 C 0.2670(5) 0.6535(4) 0.50935(13) 0.0261(17) Uani 1 1 d . . . O82 O 0.1924(4) 0.6652(3) 0.51602(11) 0.0465(15) Uani 1 1 d . . . C91 C 0.4689(5) 0.8128(4) 0.48058(15) 0.0334(19) Uani 1 1 d . . . O91 O 0.4737(4) 0.8461(3) 0.46138(10) 0.0458(15) Uani 1 1 d . . . C92 C 0.3575(5) 0.8108(4) 0.52551(14) 0.0303(18) Uani 1 1 d . . . O92 O 0.2941(3) 0.8473(3) 0.53287(10) 0.0406(14) Uani 1 1 d . . . C93 C 0.5451(5) 0.8162(4) 0.53137(14) 0.0314(18) Uani 1 1 d . . . O93 O 0.5989(4) 0.8507(3) 0.54365(11) 0.0496(15) Uani 1 1 d . . . P7 P 0.57326(11) 0.50377(10) 0.50480(3) 0.0190(4) Uani 1 1 d . . . C711 C 0.6737(5) 0.4663(4) 0.52308(12) 0.0230(16) Uani 1 1 d . . . C712 C 0.6681(5) 0.4162(4) 0.54518(13) 0.0281(17) Uani 1 1 d . . . H712 H 0.6091 0.398 0.5513 0.034 Uiso 1 1 calc R . . C713 C 0.7489(5) 0.3931(4) 0.55821(14) 0.0294(18) Uani 1 1 d . . . H713 H 0.7447 0.3592 0.5733 0.035 Uiso 1 1 calc R . . C714 C 0.8348(5) 0.4185(4) 0.54953(14) 0.0331(19) Uani 1 1 d . . . H714 H 0.8897 0.4022 0.5586 0.04 Uiso 1 1 calc R . . C715 C 0.8415(5) 0.4680(4) 0.52746(14) 0.0319(19) Uani 1 1 d . . . H715 H 0.901 0.4852 0.5213 0.038 Uiso 1 1 calc R . . C716 C 0.7617(5) 0.4924(4) 0.51440(14) 0.0281(17) Uani 1 1 d . . . H716 H 0.7665 0.527 0.4995 0.034 Uiso 1 1 calc R . . C721 C 0.5873(5) 0.4462(4) 0.47409(12) 0.0226(16) Uani 1 1 d . . . C722 C 0.6196(5) 0.3657(4) 0.47476(13) 0.0308(17) Uani 1 1 d . . . H722 H 0.6396 0.3421 0.4908 0.037 Uiso 1 1 calc R . . C723 C 0.6227(5) 0.3201(4) 0.45203(16) 0.041(2) Uani 1 1 d . . . H723 H 0.6469 0.2657 0.4525 0.049 Uiso 1 1 calc R . . C724 C 0.5914(6) 0.3517(5) 0.42873(14) 0.044(2) Uani 1 1 d . . . H724 H 0.5927 0.3191 0.4133 0.053 Uiso 1 1 calc R . . C725 C 0.5583(6) 0.4304(4) 0.42788(13) 0.0363(19) Uani 1 1 d . . . H725 H 0.5369 0.4529 0.4118 0.044 Uiso 1 1 calc R . . C726 C 0.5559(5) 0.4775(4) 0.45036(12) 0.0302(17) Uani 1 1 d . . . H726 H 0.5325 0.5321 0.4496 0.036 Uiso 1 1 calc R . . C30 C 0.4723(4) 0.4529(4) 0.51967(12) 0.0198(15) Uani 1 1 d . . . H30A H 0.471 0.4631 0.5387 0.024 Uiso 1 1 calc R . . H30B H 0.4752 0.3927 0.5167 0.024 Uiso 1 1 calc R . . P8 P 0.36756(11) 0.49672(10) 0.50403(3) 0.0200(4) Uani 1 1 d . . . C811 C 0.2725(5) 0.4612(4) 0.52547(13) 0.0243(16) Uani 1 1 d . . . C812 C 0.2852(5) 0.4485(4) 0.55167(13) 0.0292(18) Uani 1 1 d . . . H812 H 0.3446 0.4587 0.5592 0.035 Uiso 1 1 calc R . . C813 C 0.2125(5) 0.4211(5) 0.56742(15) 0.037(2) Uani 1 1 d . . . H813 H 0.2224 0.4122 0.5856 0.044 Uiso 1 1 calc R . . C814 C 0.1255(5) 0.4069(4) 0.55653(14) 0.0344(19) Uani 1 1 d . . . H814 H 0.0756 0.3874 0.5671 0.041 Uiso 1 1 calc R . . C815 C 0.1124(6) 0.4212(5) 0.53051(16) 0.047(2) Uani 1 1 d . . . H815 H 0.0524 0.4124 0.5231 0.056 Uiso 1 1 calc R . . C816 C 0.1847(5) 0.4482(5) 0.51450(15) 0.043(2) Uani 1 1 d . . . H816 H 0.1744 0.4578 0.4964 0.052 Uiso 1 1 calc R . . C821 C 0.3457(5) 0.4352(4) 0.47460(12) 0.0221(16) Uani 1 1 d . . . C822 C 0.3768(5) 0.3547(4) 0.47231(13) 0.0320(18) Uani 1 1 d . . . H822 H 0.4118 0.3304 0.4861 0.038 Uiso 1 1 calc R . . C823 C 0.3569(5) 0.3098(5) 0.45008(16) 0.042(2) Uani 1 1 d . . . H823 H 0.3805 0.2555 0.4483 0.05 Uiso 1 1 calc R . . C824 C 0.3024(6) 0.3437(5) 0.43026(14) 0.041(2) Uani 1 1 d . . . H824 H 0.2873 0.3122 0.4152 0.05 Uiso 1 1 calc R . . C825 C 0.2708(5) 0.4231(4) 0.43276(14) 0.0348(19) Uani 1 1 d . . . H825 H 0.2335 0.4464 0.4193 0.042 Uiso 1 1 calc R . . C826 C 0.2924(5) 0.4695(4) 0.45458(13) 0.0291(18) Uani 1 1 d . . . H826 H 0.2709 0.5247 0.4559 0.035 Uiso 1 1 calc R . . C5 C 0.4533(4) 0.6561(3) 0.52982(11) 0.0181(14) Uani 1 1 d . . . C6 C 0.4144(5) 0.6456(4) 0.55619(12) 0.0257(16) Uani 1 1 d . . . O6 O 0.3412(3) 0.6801(3) 0.56265(9) 0.0418(14) Uani 1 1 d . . . C701 C 0.4594(5) 0.5905(4) 0.57617(13) 0.0295(18) Uani 1 1 d . . . C702 C 0.4127(5) 0.5636(4) 0.59930(13) 0.0330(18) Uani 1 1 d . . . H702 H 0.349 0.5733 0.6035 0.04 Uiso 1 1 calc R . . C703 C 0.4770(6) 0.5204(4) 0.61489(14) 0.039(2) Uani 1 1 d . . . H703 H 0.4642 0.4963 0.6314 0.047 Uiso 1 1 calc R . . C704 C 0.5631(6) 0.5189(4) 0.60194(13) 0.0332(19) Uani 1 1 d . . . H704 H 0.6182 0.4927 0.608 0.04 Uiso 1 1 calc R . . C705 C 0.5539(5) 0.5641(4) 0.57763(12) 0.0260(16) Uani 1 1 d . . . H705 H 0.6016 0.5741 0.5651 0.031 Uiso 1 1 calc R . . C801 C 0.5099(6) 0.7612(4) 0.60373(15) 0.041(2) Uani 1 1 d . . . H801 H 0.4827 0.7883 0.5891 0.049 Uiso 1 1 calc R . . C802 C 0.6064(6) 0.7387(5) 0.60592(17) 0.048(2) Uani 1 1 d . . . H802 H 0.6546 0.748 0.5935 0.057 Uiso 1 1 calc R . . C803 C 0.6139(6) 0.6998(5) 0.63059(17) 0.058(3) Uani 1 1 d . . . H803 H 0.6698 0.6776 0.6376 0.07 Uiso 1 1 calc R . . C804 C 0.5272(6) 0.6988(5) 0.64304(15) 0.047(2) Uani 1 1 d . . . H804 H 0.5146 0.6763 0.6598 0.056 Uiso 1 1 calc R . . C805 C 0.4616(6) 0.7371(5) 0.62641(15) 0.049(2) Uani 1 1 d . . . H805 H 0.3971 0.7451 0.6299 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0180(5) 0.0187(5) 0.0208(5) 0.0002(4) -0.0014(4) 0.0012(5) Co2 0.0185(5) 0.0187(5) 0.0190(5) 0.0007(5) 0.0019(4) 0.0001(5) Co3 0.0248(5) 0.0181(5) 0.0233(5) -0.0014(5) -0.0021(5) 0.0009(5) Co4 0.0188(5) 0.0179(5) 0.0206(5) 0.0002(4) -0.0032(4) -0.0009(4) Co5 0.0190(5) 0.0172(5) 0.0208(5) -0.0005(4) -0.0008(4) 0.0000(5) Co6 0.0229(5) 0.0175(5) 0.0230(5) 0.0028(5) -0.0025(5) -0.0011(5) Co7 0.0190(5) 0.0182(5) 0.0209(5) 0.0005(5) -0.0003(4) -0.0011(4) Co8 0.0202(5) 0.0192(5) 0.0229(5) 0.0009(5) -0.0045(5) -0.0007(4) Co9 0.0223(6) 0.0185(5) 0.0248(6) -0.0022(5) 0.0012(5) -0.0009(4) Fe1 0.0353(6) 0.0255(6) 0.0204(5) -0.0046(5) 0.0037(5) -0.0026(5) Fe2 0.0348(6) 0.0228(5) 0.0201(5) 0.0030(5) 0.0017(5) 0.0039(5) Fe3 0.0342(6) 0.0240(6) 0.0223(5) -0.0053(5) -0.0045(5) 0.0037(5) C11 0.027(4) 0.016(3) 0.032(4) -0.004(3) 0.002(3) -0.006(3) O11 0.043(3) 0.031(3) 0.026(3) 0.001(2) -0.008(2) -0.005(2) C12 0.032(4) 0.021(4) 0.035(4) 0.000(3) 0.000(3) 0.000(3) O12 0.030(3) 0.042(3) 0.056(4) 0.001(3) 0.013(3) 0.009(3) C21 0.030(4) 0.027(4) 0.034(4) -0.009(3) 0.001(3) 0.010(3) O21 0.060(4) 0.051(3) 0.024(3) 0.011(2) 0.014(3) 0.018(3) C22 0.039(4) 0.018(4) 0.028(4) -0.003(3) 0.006(3) -0.001(3) O22 0.021(3) 0.045(3) 0.041(3) 0.002(2) -0.005(2) -0.008(2) C31 0.029(4) 0.026(4) 0.040(4) 0.004(3) -0.009(3) -0.003(3) O31 0.059(4) 0.039(3) 0.035(3) 0.013(3) -0.012(3) -0.007(3) C32 0.034(4) 0.029(4) 0.030(4) -0.007(3) -0.006(3) 0.001(3) O32 0.045(3) 0.052(4) 0.067(4) -0.022(3) 0.008(3) 0.014(3) C33 0.036(4) 0.028(4) 0.031(4) -0.006(3) 0.000(3) 0.004(3) O33 0.047(4) 0.052(4) 0.060(4) -0.022(3) -0.015(3) -0.003(3) P1 0.0189(8) 0.0191(9) 0.0219(8) -0.0008(7) -0.0017(7) -0.0003(7) C111 0.017(3) 0.015(3) 0.030(4) 0.000(3) -0.003(3) -0.002(3) C112 0.034(4) 0.038(5) 0.036(4) 0.002(4) 0.001(3) -0.010(4) C113 0.045(5) 0.042(5) 0.034(4) 0.010(4) 0.015(4) -0.002(4) C114 0.055(6) 0.032(4) 0.052(5) -0.010(4) 0.025(4) -0.012(4) C115 0.019(4) 0.046(5) 0.073(6) 0.003(5) 0.004(4) -0.003(4) C116 0.024(4) 0.040(5) 0.048(5) 0.006(4) 0.004(3) -0.010(3) C121 0.027(4) 0.024(4) 0.037(4) -0.013(3) -0.009(3) 0.008(3) C122 0.045(5) 0.054(5) 0.048(5) -0.028(4) 0.009(4) -0.011(4) C123 0.045(5) 0.068(6) 0.087(7) -0.053(6) 0.001(5) -0.015(5) C124 0.066(6) 0.067(6) 0.072(6) -0.048(5) -0.027(5) 0.028(5) C125 0.079(7) 0.057(5) 0.031(4) -0.010(4) -0.013(4) 0.038(5) C126 0.061(6) 0.041(4) 0.025(4) -0.003(3) -0.007(4) 0.020(4) C10 0.021(3) 0.024(3) 0.016(3) 0.000(3) 0.001(3) -0.001(3) P2 0.0197(9) 0.0180(8) 0.0213(8) 0.0004(7) 0.0011(7) 0.0013(7) C211 0.028(4) 0.020(4) 0.030(4) -0.002(3) -0.003(3) 0.000(3) C212 0.039(5) 0.027(4) 0.037(4) -0.001(3) -0.011(4) 0.006(3) C213 0.058(6) 0.037(5) 0.047(5) -0.006(4) -0.010(4) 0.004(4) C214 0.047(5) 0.038(5) 0.083(7) -0.017(5) -0.038(5) 0.017(4) C215 0.024(5) 0.083(7) 0.079(7) -0.011(6) -0.013(5) 0.016(5) C216 0.028(4) 0.050(5) 0.054(5) -0.007(4) -0.009(4) 0.007(4) C221 0.028(4) 0.022(4) 0.023(3) -0.002(3) 0.004(3) 0.007(3) C222 0.040(4) 0.029(4) 0.028(4) 0.001(3) 0.005(3) -0.001(3) C223 0.048(5) 0.027(4) 0.042(4) -0.007(3) 0.007(4) 0.008(4) C224 0.042(5) 0.039(4) 0.029(4) -0.009(3) 0.005(4) 0.011(4) C225 0.050(5) 0.029(4) 0.028(4) 0.003(3) 0.013(4) 0.012(3) C226 0.049(5) 0.025(4) 0.036(4) 0.000(3) 0.018(4) 0.004(3) C1 0.022(3) 0.012(3) 0.025(3) -0.003(3) 0.000(3) -0.005(3) C2 0.032(4) 0.019(3) 0.024(4) -0.001(3) 0.003(3) 0.004(3) O2 0.023(3) 0.066(4) 0.030(3) 0.010(3) -0.004(2) 0.005(3) C101 0.039(4) 0.020(3) 0.022(4) -0.007(3) 0.001(3) -0.005(3) C102 0.058(5) 0.016(3) 0.030(4) -0.006(3) 0.008(4) 0.005(3) C103 0.067(6) 0.037(4) 0.024(4) -0.003(3) 0.010(4) -0.013(4) C104 0.043(5) 0.065(6) 0.028(4) -0.013(4) 0.007(4) -0.030(4) C105 0.039(4) 0.049(5) 0.018(3) -0.006(3) 0.001(3) -0.013(4) C41 0.029(4) 0.026(4) 0.026(4) 0.002(3) -0.008(3) 0.003(3) O41 0.044(3) 0.047(3) 0.024(3) -0.009(2) -0.010(2) 0.010(3) C42 0.027(4) 0.027(4) 0.031(4) -0.003(3) -0.008(3) -0.004(3) O42 0.026(3) 0.047(3) 0.054(3) 0.006(3) 0.001(3) -0.011(2) C51 0.036(4) 0.021(4) 0.019(3) -0.007(3) 0.012(3) -0.005(3) O51 0.022(3) 0.038(3) 0.045(3) -0.006(2) -0.005(2) 0.005(2) C52 0.030(4) 0.029(4) 0.025(4) 0.001(3) 0.004(3) -0.009(3) O52 0.051(3) 0.043(3) 0.022(3) -0.003(2) 0.004(2) -0.002(3) C61 0.038(4) 0.012(3) 0.036(4) 0.004(3) -0.002(3) 0.003(3) O61 0.053(4) 0.049(4) 0.039(3) -0.011(3) -0.004(3) -0.006(3) C62 0.032(4) 0.018(3) 0.031(4) 0.006(3) -0.004(3) -0.005(3) O62 0.046(3) 0.045(3) 0.057(4) 0.014(3) -0.016(3) 0.007(3) C63 0.031(4) 0.037(4) 0.030(4) 0.006(3) -0.003(3) 0.006(3) O63 0.037(3) 0.059(4) 0.082(4) 0.031(3) 0.007(3) -0.013(3) P4 0.0173(8) 0.0185(8) 0.0208(8) 0.0007(7) -0.0018(7) 0.0010(7) C411 0.023(4) 0.024(4) 0.031(4) -0.002(3) 0.001(3) -0.002(3) C412 0.031(4) 0.028(4) 0.024(4) 0.003(3) 0.003(3) 0.001(3) C413 0.050(5) 0.035(4) 0.022(4) 0.003(3) 0.006(3) 0.008(4) C414 0.034(4) 0.046(5) 0.035(4) 0.002(4) 0.013(4) 0.007(4) C415 0.023(4) 0.066(6) 0.044(5) -0.002(4) 0.003(4) -0.004(4) C416 0.029(4) 0.057(5) 0.033(4) -0.017(4) 0.002(3) 0.000(4) C421 0.025(4) 0.026(4) 0.016(3) 0.005(3) 0.002(3) 0.006(3) C422 0.049(5) 0.026(4) 0.031(4) 0.001(3) -0.008(4) 0.001(3) C423 0.060(6) 0.036(5) 0.059(6) 0.023(4) -0.011(5) -0.005(4) C424 0.040(5) 0.035(4) 0.043(5) 0.017(4) -0.017(4) 0.002(4) C425 0.049(5) 0.047(5) 0.026(4) 0.004(4) -0.009(4) 0.004(4) C426 0.030(4) 0.024(4) 0.040(4) -0.003(3) -0.009(3) 0.009(3) C20 0.021(4) 0.019(3) 0.022(3) 0.000(3) -0.002(3) -0.004(3) P5 0.0183(9) 0.0183(8) 0.0210(8) 0.0008(7) -0.0007(7) -0.0020(7) C511 0.025(4) 0.018(3) 0.024(4) 0.009(3) -0.005(3) -0.004(3) C512 0.026(4) 0.025(4) 0.032(4) -0.004(3) -0.003(3) -0.002(3) C513 0.047(5) 0.039(5) 0.038(5) -0.012(4) -0.005(4) -0.008(4) C514 0.030(4) 0.041(5) 0.044(5) 0.007(4) -0.016(4) -0.003(4) C515 0.026(4) 0.038(4) 0.056(5) 0.003(4) -0.001(4) -0.009(3) C516 0.029(4) 0.030(4) 0.038(4) -0.004(3) 0.005(3) -0.001(3) C521 0.034(4) 0.022(4) 0.025(4) 0.008(3) 0.003(3) 0.008(3) C522 0.036(4) 0.031(4) 0.048(5) 0.006(4) 0.002(4) -0.004(4) C523 0.050(5) 0.037(5) 0.061(6) 0.030(4) -0.005(5) -0.004(4) C524 0.080(7) 0.057(6) 0.031(4) 0.025(4) 0.001(5) 0.017(5) C525 0.084(7) 0.047(5) 0.024(4) 0.008(4) 0.003(4) 0.015(5) C526 0.039(4) 0.032(4) 0.029(4) 0.001(3) -0.004(3) 0.011(3) C3 0.012(3) 0.016(3) 0.030(3) 0.004(3) -0.003(3) 0.000(3) C4 0.023(4) 0.023(3) 0.020(3) 0.006(3) -0.008(3) -0.004(3) O4 0.023(3) 0.068(4) 0.024(2) -0.016(2) 0.001(2) -0.005(2) C401 0.030(4) 0.020(3) 0.016(3) 0.003(3) 0.000(3) 0.004(3) C402 0.047(5) 0.017(3) 0.030(4) -0.001(3) -0.004(4) -0.008(3) C403 0.058(5) 0.016(3) 0.030(4) 0.001(3) 0.005(4) 0.008(3) C404 0.034(4) 0.031(4) 0.040(4) 0.009(4) 0.011(4) 0.018(3) C405 0.032(4) 0.027(4) 0.027(4) 0.008(3) 0.001(3) 0.002(3) C71 0.024(4) 0.018(3) 0.032(4) 0.001(3) 0.000(3) -0.001(3) O71 0.035(3) 0.039(3) 0.022(3) 0.000(2) 0.006(2) 0.002(2) C72 0.027(4) 0.019(4) 0.033(4) 0.003(3) 0.003(3) -0.001(3) O72 0.032(3) 0.043(3) 0.050(3) -0.004(3) -0.010(3) -0.003(2) C81 0.029(4) 0.020(4) 0.031(4) 0.002(3) -0.014(3) 0.001(3) O81 0.066(4) 0.040(3) 0.021(3) 0.003(2) -0.017(3) -0.016(3) C82 0.027(4) 0.022(4) 0.029(4) -0.004(3) -0.009(3) -0.005(3) O82 0.026(3) 0.046(3) 0.068(4) -0.009(3) -0.002(3) 0.003(2) C91 0.031(4) 0.032(4) 0.038(4) -0.005(4) 0.000(4) -0.001(3) O91 0.055(4) 0.040(3) 0.042(3) 0.012(3) 0.002(3) 0.004(3) C92 0.032(4) 0.025(4) 0.034(4) -0.002(3) -0.009(3) -0.013(3) O92 0.031(3) 0.039(3) 0.052(3) -0.006(3) 0.003(3) 0.011(2) C93 0.025(4) 0.034(4) 0.036(4) 0.000(3) -0.007(3) 0.006(3) O93 0.041(3) 0.047(3) 0.061(4) -0.016(3) -0.008(3) -0.005(3) P7 0.0202(8) 0.0177(8) 0.0191(8) -0.0008(7) -0.0011(7) 0.0002(7) C711 0.021(3) 0.028(4) 0.020(3) 0.000(3) -0.002(3) 0.001(3) C712 0.023(4) 0.025(4) 0.036(4) -0.004(3) 0.001(3) -0.001(3) C713 0.022(4) 0.037(4) 0.029(4) 0.005(3) -0.005(3) -0.001(3) C714 0.024(4) 0.033(4) 0.042(5) -0.004(4) -0.008(3) 0.010(3) C715 0.018(4) 0.031(4) 0.047(5) -0.002(4) 0.003(3) 0.000(3) C716 0.028(4) 0.026(4) 0.031(4) -0.001(3) -0.001(3) 0.001(3) C721 0.029(4) 0.020(3) 0.019(3) -0.004(3) 0.005(3) -0.003(3) C722 0.035(4) 0.031(4) 0.027(4) -0.005(3) 0.003(3) 0.000(3) C723 0.040(5) 0.023(4) 0.060(5) -0.015(4) -0.009(4) 0.005(3) C724 0.054(5) 0.043(5) 0.035(4) -0.016(4) -0.002(4) -0.017(4) C725 0.054(5) 0.031(4) 0.024(4) -0.004(3) 0.003(4) -0.019(4) C726 0.035(4) 0.034(4) 0.021(4) -0.004(3) 0.003(3) -0.001(3) C30 0.018(3) 0.016(3) 0.025(3) 0.007(3) -0.003(3) -0.002(3) P8 0.0182(8) 0.0183(8) 0.0236(9) 0.0004(7) -0.0029(7) -0.0008(7) C811 0.023(4) 0.021(4) 0.029(4) -0.004(3) 0.000(3) 0.000(3) C812 0.021(4) 0.036(4) 0.030(4) -0.001(3) -0.002(3) -0.005(3) C813 0.038(5) 0.039(5) 0.033(4) 0.002(4) 0.008(4) 0.000(4) C814 0.029(4) 0.033(4) 0.041(4) -0.001(4) 0.007(4) -0.006(3) C815 0.028(4) 0.058(5) 0.054(5) 0.000(4) 0.000(4) -0.013(4) C816 0.029(4) 0.068(6) 0.032(4) 0.002(4) -0.007(4) -0.008(4) C821 0.026(4) 0.014(3) 0.026(4) -0.003(3) 0.002(3) -0.009(3) C822 0.036(4) 0.027(4) 0.033(4) 0.000(3) -0.012(3) -0.003(3) C823 0.045(5) 0.025(4) 0.056(5) -0.017(4) -0.017(4) 0.001(4) C824 0.057(5) 0.037(5) 0.030(4) -0.009(4) -0.012(4) -0.014(4) C825 0.036(4) 0.033(4) 0.036(4) 0.001(4) -0.009(4) -0.012(3) C826 0.027(4) 0.025(4) 0.035(4) 0.003(3) -0.012(3) -0.003(3) C5 0.024(3) 0.012(3) 0.019(3) -0.002(2) -0.001(3) 0.000(3) C6 0.026(4) 0.026(4) 0.025(3) -0.003(3) -0.009(3) -0.001(3) O6 0.027(3) 0.069(4) 0.029(3) 0.005(3) 0.003(2) 0.013(3) C701 0.032(4) 0.028(4) 0.028(4) -0.013(3) -0.003(3) -0.003(3) C702 0.041(5) 0.026(4) 0.032(4) 0.000(3) -0.001(3) -0.010(3) C703 0.060(5) 0.029(4) 0.028(4) 0.002(3) -0.004(4) -0.004(4) C704 0.058(5) 0.016(3) 0.025(4) 0.001(3) -0.003(4) 0.007(3) C705 0.039(4) 0.019(3) 0.020(3) -0.004(3) 0.003(3) 0.001(3) C801 0.061(5) 0.017(4) 0.043(5) -0.014(3) -0.015(4) 0.003(4) C802 0.040(5) 0.035(5) 0.069(6) -0.009(4) 0.001(4) -0.011(4) C803 0.059(6) 0.051(5) 0.065(6) -0.024(5) -0.033(5) -0.001(5) C804 0.076(6) 0.040(5) 0.025(4) -0.021(3) 0.004(4) 0.013(4) C805 0.060(6) 0.040(5) 0.047(5) -0.025(4) -0.007(4) 0.011(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.782(7) . ? Co1 C11 1.793(7) . ? Co1 C1 1.902(6) . ? Co1 P1 2.1893(19) . ? Co1 Co2 2.4604(14) . ? Co1 Co3 2.4730(14) . ? Co2 C22 1.776(7) . ? Co2 C21 1.821(7) . ? Co2 C1 1.920(6) . ? Co2 P2 2.2120(19) . ? Co2 Co3 2.4911(14) . ? Co3 C33 1.794(7) . ? Co3 C32 1.805(7) . ? Co3 C31 1.828(7) . ? Co3 C1 1.947(6) . ? Co4 C42 1.775(7) . ? Co4 C41 1.798(6) . ? Co4 C3 1.884(6) . ? Co4 P4 2.1960(19) . ? Co4 Co5 2.4660(14) . ? Co4 Co6 2.4937(14) . ? Co5 C51 1.780(7) . ? Co5 C52 1.820(7) . ? Co5 C3 1.899(6) . ? Co5 P5 2.1980(19) . ? Co5 Co6 2.4795(14) . ? Co6 C63 1.783(7) . ? Co6 C62 1.793(7) . ? Co6 C61 1.836(7) . ? Co6 C3 1.932(6) . ? Co7 C72 1.784(7) . ? Co7 C71 1.817(7) . ? Co7 C5 1.912(6) . ? Co7 P7 2.1964(19) . ? Co7 Co9 2.4526(14) . ? Co7 Co8 2.4626(13) . ? Co8 C82 1.787(7) . ? Co8 C81 1.793(7) . ? Co8 C5 1.900(6) . ? Co8 P8 2.2100(19) . ? Co8 Co9 2.4830(14) . ? Co9 C92 1.786(8) . ? Co9 C93 1.789(7) . ? Co9 C91 1.845(8) . ? Co9 C5 1.931(6) . ? Fe1 C302 1.994(17) . ? Fe1 C301 1.99(2) . ? Fe1 C304 2.00(2) . ? Fe1 C305 2.02(2) . ? Fe1 C102 2.024(7) . ? Fe1 C101 2.029(6) . ? Fe1 C205 2.040(13) . ? Fe1 C203 2.042(14) . ? Fe1 C105 2.045(7) . ? Fe1 C103 2.047(7) . ? Fe1 C201 2.049(12) . ? Fe1 C303 2.05(3) . ? Fe2 C605 2.010(18) . ? Fe2 C402 2.026(7) . ? Fe2 C503 2.029(12) . ? Fe2 C401 2.031(6) . ? Fe2 C604 2.032(16) . ? Fe2 C405 2.034(6) . ? Fe2 C601 2.035(16) . ? Fe2 C403 2.045(6) . ? Fe2 C602 2.05(2) . ? Fe2 C505 2.051(11) . ? Fe2 C404 2.052(7) . ? Fe2 C504 2.061(12) . ? Fe3 C702 2.013(7) . ? Fe3 C701 2.016(7) . ? Fe3 C801 2.018(7) . ? Fe3 C803 2.026(8) . ? Fe3 C804 2.033(7) . ? Fe3 C805 2.036(7) . ? Fe3 C705 2.037(6) . ? Fe3 C703 2.038(7) . ? Fe3 C802 2.053(8) . ? Fe3 C704 2.060(7) . ? C11 O11 1.146(8) . ? C12 O12 1.142(8) . ? C21 O21 1.123(8) . ? C22 O22 1.161(8) . ? C31 O31 1.119(8) . ? C32 O32 1.130(8) . ? C33 O33 1.134(9) . ? P1 C10 1.826(6) . ? P1 C111 1.827(7) . ? P1 C121 1.838(7) . ? C111 C112 1.382(9) . ? C111 C116 1.392(9) . ? C112 C113 1.371(10) . ? C112 H112 0.95 . ? C113 C114 1.391(11) . ? C113 H113 0.95 . ? C114 C115 1.379(11) . ? C114 H114 0.95 . ? C115 C116 1.392(10) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.384(10) . ? C121 C122 1.390(10) . ? C122 C123 1.393(11) . ? C122 H122 0.95 . ? C123 C124 1.347(13) . ? C123 H123 0.95 . ? C124 C125 1.388(12) . ? C124 H124 0.95 . ? C125 C126 1.382(10) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 P2 1.840(6) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? P2 C211 1.825(7) . ? P2 C221 1.836(6) . ? C211 C216 1.373(10) . ? C211 C212 1.390(9) . ? C212 C213 1.377(10) . ? C212 H212 0.95 . ? C213 C214 1.374(12) . ? C213 H213 0.95 . ? C214 C215 1.392(12) . ? C214 H214 0.95 . ? C215 C216 1.391(11) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.379(9) . ? C221 C222 1.380(9) . ? C222 C223 1.392(9) . ? C222 H222 0.95 . ? C223 C224 1.366(10) . ? C223 H223 0.95 . ? C224 C225 1.358(10) . ? C224 H224 0.95 . ? C225 C226 1.398(9) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C1 C2 1.457(8) . ? C2 O2 1.226(8) . ? C2 C101 1.485(9) . ? C101 C105 1.428(10) . ? C101 C102 1.459(9) . ? C102 C103 1.413(10) . ? C102 H102 0.95 . ? C103 C104 1.414(11) . ? C103 H103 0.95 . ? C104 C105 1.428(10) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C201 C205 1.366(19) . ? C201 C202 1.469(16) . ? C201 H201 0.95 . ? C202 C203 1.395(19) . ? C202 H202 0.95 . ? C203 C204 1.403(17) . ? C203 H203 0.95 . ? C204 C205 1.422(17) . ? C204 H204 0.95 . ? C205 H205 0.95 . ? C301 C305 1.33(3) . ? C301 C302 1.40(3) . ? C301 H301 0.95 . ? C302 C303 1.47(3) . ? C302 H302 0.95 . ? C303 C304 1.40(4) . ? C303 H303 0.95 . ? C304 C305 1.58(3) . ? C304 H304 0.95 . ? C305 H305 0.95 . ? C41 O41 1.142(7) . ? C42 O42 1.140(8) . ? C51 O51 1.154(8) . ? C52 O52 1.135(8) . ? C61 O61 1.120(8) . ? C62 O62 1.137(8) . ? C63 O63 1.139(9) . ? P4 C411 1.836(7) . ? P4 C20 1.837(6) . ? P4 C421 1.845(6) . ? C411 C412 1.375(9) . ? C411 C416 1.399(9) . ? C412 C413 1.404(10) . ? C412 H412 0.95 . ? C413 C414 1.365(10) . ? C413 H413 0.95 . ? C414 C415 1.397(10) . ? C414 H414 0.95 . ? C415 C416 1.365(10) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C422 1.366(9) . ? C421 C426 1.381(9) . ? C422 C423 1.399(10) . ? C422 H422 0.95 . ? C423 C424 1.377(11) . ? C423 H423 0.95 . ? C424 C425 1.351(10) . ? C424 H424 0.95 . ? C425 C426 1.405(10) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C20 P5 1.823(6) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P5 C511 1.824(7) . ? P5 C521 1.836(6) . ? C511 C516 1.376(9) . ? C511 C512 1.398(9) . ? C512 C513 1.390(10) . ? C512 H512 0.95 . ? C513 C514 1.371(11) . ? C513 H513 0.95 . ? C514 C515 1.397(10) . ? C514 H514 0.95 . ? C515 C516 1.390(10) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C526 1.377(9) . ? C521 C522 1.387(10) . ? C522 C523 1.396(10) . ? C522 H522 0.95 . ? C523 C524 1.363(11) . ? C523 H523 0.95 . ? C524 C525 1.364(11) . ? C524 H524 0.95 . ? C525 C526 1.366(9) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? C3 C4 1.485(8) . ? C4 O4 1.232(8) . ? C4 C401 1.473(9) . ? C401 C405 1.425(9) . ? C401 C402 1.444(9) . ? C402 C403 1.393(10) . ? C402 H402 0.95 . ? C403 C404 1.418(10) . ? C403 H403 0.95 . ? C404 C405 1.402(9) . ? C404 H404 0.95 . ? C405 H405 0.95 . ? C501 C505 1.415(12) . ? C501 C502 1.422(13) . ? C501 H501 0.95 . ? C502 C503 1.456(14) . ? C502 H502 0.95 . ? C503 C504 1.418(14) . ? C503 H503 0.95 . ? C504 C505 1.416(14) . ? C504 H504 0.95 . ? C505 H505 0.95 . ? C601 C605 1.414(17) . ? C601 C602 1.414(18) . ? C601 H601 0.95 . ? C602 C603 1.440(17) . ? C602 H602 0.95 . ? C603 C604 1.423(16) . ? C603 H603 0.95 . ? C604 C605 1.421(17) . ? C604 H604 0.95 . ? C605 H605 0.95 . ? C71 O71 1.121(7) . ? C72 O72 1.144(8) . ? C81 O81 1.146(8) . ? C82 O82 1.139(8) . ? C91 O91 1.124(8) . ? C92 O92 1.149(8) . ? C93 O93 1.142(8) . ? P7 C711 1.821(7) . ? P7 C30 1.832(6) . ? P7 C721 1.839(6) . ? C711 C712 1.395(9) . ? C711 C716 1.403(9) . ? C712 C713 1.388(9) . ? C712 H712 0.95 . ? C713 C714 1.373(10) . ? C713 H713 0.95 . ? C714 C715 1.390(10) . ? C714 H714 0.95 . ? C715 C716 1.382(9) . ? C715 H715 0.95 . ? C716 H716 0.95 . ? C721 C722 1.388(9) . ? C721 C726 1.390(9) . ? C722 C723 1.380(9) . ? C722 H722 0.95 . ? C723 C724 1.373(10) . ? C723 H723 0.95 . ? C724 C725 1.365(10) . ? C724 H724 0.95 . ? C725 C726 1.382(9) . ? C725 H725 0.95 . ? C726 H726 0.95 . ? C30 P8 1.844(6) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? P8 C821 1.834(6) . ? P8 C811 1.842(7) . ? C811 C812 1.368(9) . ? C811 C816 1.394(10) . ? C812 C813 1.390(9) . ? C812 H812 0.95 . ? C813 C814 1.384(10) . ? C813 H813 0.95 . ? C814 C815 1.364(10) . ? C814 H814 0.95 . ? C815 C816 1.392(10) . ? C815 H815 0.95 . ? C816 H816 0.95 . ? C821 C822 1.386(9) . ? C821 C826 1.395(9) . ? C822 C823 1.381(10) . ? C822 H822 0.95 . ? C823 C824 1.392(10) . ? C823 H823 0.95 . ? C824 C825 1.374(10) . ? C824 H824 0.95 . ? C825 C826 1.383(9) . ? C825 H825 0.95 . ? C826 H826 0.95 . ? C5 C6 1.470(8) . ? C6 O6 1.234(8) . ? C6 C701 1.505(9) . ? C701 C705 1.422(10) . ? C701 C702 1.428(9) . ? C702 C703 1.407(10) . ? C702 H702 0.95 . ? C703 C704 1.401(11) . ? C703 H703 0.95 . ? C704 C705 1.450(9) . ? C704 H704 0.95 . ? C705 H705 0.95 . ? C801 C805 1.407(11) . ? C801 C802 1.434(11) . ? C801 H801 0.95 . ? C802 C803 1.416(11) . ? C802 H802 0.95 . ? C803 C804 1.396(12) . ? C803 H803 0.95 . ? C804 C805 1.413(11) . ? C804 H804 0.95 . ? C805 H805 0.95 . ? 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 C12 Co1 C11 99.7(3) . . ? C12 Co1 C1 108.4(3) . . ? C11 Co1 C1 140.6(3) . . ? C12 Co1 P1 98.1(2) . . ? C11 Co1 P1 105.0(2) . . ? C1 Co1 P1 97.80(19) . . ? C12 Co1 Co2 156.0(2) . . ? C11 Co1 Co2 95.2(2) . . ? C1 Co1 Co2 50.24(18) . . ? P1 Co1 Co2 96.09(6) . . ? C12 Co1 Co3 98.2(2) . . ? C11 Co1 Co3 99.0(2) . . ? C1 Co1 Co3 50.83(18) . . ? P1 Co1 Co3 148.04(7) . . ? Co2 Co1 Co3 60.65(4) . . ? C22 Co2 C21 102.2(3) . . ? C22 Co2 C1 102.4(3) . . ? C21 Co2 C1 145.8(3) . . ? C22 Co2 P2 94.5(2) . . ? C21 Co2 P2 106.5(2) . . ? C1 Co2 P2 94.80(19) . . ? C22 Co2 Co1 150.4(2) . . ? C21 Co2 Co1 100.5(2) . . ? C1 Co2 Co1 49.61(18) . . ? P2 Co2 Co1 96.85(6) . . ? C22 Co2 Co3 96.3(2) . . ? C21 Co2 Co3 103.5(2) . . ? C1 Co2 Co3 50.38(18) . . ? P2 Co2 Co3 145.02(7) . . ? Co1 Co2 Co3 59.92(4) . . ? C33 Co3 C32 99.2(3) . . ? C33 Co3 C31 103.1(3) . . ? C32 Co3 C31 102.1(3) . . ? C33 Co3 C1 100.3(3) . . ? C32 Co3 C1 106.1(3) . . ? C31 Co3 C1 139.6(3) . . ? C33 Co3 Co1 148.9(2) . . ? C32 Co3 Co1 96.2(2) . . ? C31 Co3 Co1 99.8(2) . . ? C1 Co3 Co1 49.22(18) . . ? C33 Co3 Co2 97.7(2) . . ? C32 Co3 Co2 152.6(2) . . ? C31 Co3 Co2 94.8(2) . . ? C1 Co3 Co2 49.41(18) . . ? Co1 Co3 Co2 59.42(4) . . ? C42 Co4 C41 101.9(3) . . ? C42 Co4 C3 111.7(3) . . ? C41 Co4 C3 136.9(3) . . ? C42 Co4 P4 96.0(2) . . ? C41 Co4 P4 105.8(2) . . ? C3 Co4 P4 96.9(2) . . ? C42 Co4 Co5 158.0(2) . . ? C41 Co4 Co5 90.7(2) . . ? C3 Co4 Co5 49.58(19) . . ? P4 Co4 Co5 97.75(6) . . ? C42 Co4 Co6 99.8(2) . . ? C41 Co4 Co6 99.3(2) . . ? C3 Co4 Co6 50.03(19) . . ? P4 Co4 Co6 146.73(7) . . ? Co5 Co4 Co6 59.99(4) . . ? C51 Co5 C52 100.0(3) . . ? C51 Co5 C3 100.3(3) . . ? C52 Co5 C3 149.0(3) . . ? C51 Co5 P5 95.6(2) . . ? C52 Co5 P5 106.0(2) . . ? C3 Co5 P5 95.14(19) . . ? C51 Co5 Co4 148.3(2) . . ? C52 Co5 Co4 105.5(2) . . ? C3 Co5 Co4 49.04(18) . . ? P5 Co5 Co4 95.13(6) . . ? C51 Co5 Co6 95.1(2) . . ? C52 Co5 Co6 104.7(2) . . ? C3 Co5 Co6 50.24(19) . . ? P5 Co5 Co6 145.11(7) . . ? Co4 Co5 Co6 60.56(4) . . ? C63 Co6 C62 99.4(3) . . ? C63 Co6 C61 101.2(3) . . ? C62 Co6 C61 103.1(3) . . ? C63 Co6 C3 108.4(3) . . ? C62 Co6 C3 101.5(3) . . ? C61 Co6 C3 137.4(3) . . ? C63 Co6 Co5 153.7(2) . . ? C62 Co6 Co5 98.9(2) . . ? C61 Co6 Co5 92.9(2) . . ? C3 Co6 Co5 49.09(18) . . ? C63 Co6 Co4 96.0(2) . . ? C62 Co6 Co4 149.5(2) . . ? C61 Co6 Co4 99.5(2) . . ? C3 Co6 Co4 48.35(17) . . ? Co5 Co6 Co4 59.45(4) . . ? C72 Co7 C71 102.0(3) . . ? C72 Co7 C5 104.0(3) . . ? C71 Co7 C5 138.7(3) . . ? C72 Co7 P7 98.7(2) . . ? C71 Co7 P7 101.6(2) . . ? C5 Co7 P7 105.50(18) . . ? C72 Co7 Co9 100.1(2) . . ? C71 Co7 Co9 93.6(2) . . ? C5 Co7 Co9 50.67(17) . . ? P7 Co7 Co9 152.80(7) . . ? C72 Co7 Co8 153.0(2) . . ? C71 Co7 Co8 98.2(2) . . ? C5 Co7 Co8 49.53(18) . . ? P7 Co7 Co8 94.57(6) . . ? Co9 Co7 Co8 60.69(4) . . ? C82 Co8 C81 104.4(3) . . ? C82 Co8 C5 102.1(3) . . ? C81 Co8 C5 141.7(3) . . ? C82 Co8 P8 94.1(2) . . ? C81 Co8 P8 105.0(2) . . ? C5 Co8 P8 100.05(18) . . ? C82 Co8 Co7 151.2(2) . . ? C81 Co8 Co7 97.8(2) . . ? C5 Co8 Co7 49.97(19) . . ? P8 Co8 Co7 97.53(6) . . ? C82 Co8 Co9 98.9(2) . . ? C81 Co8 Co9 98.4(2) . . ? C5 Co8 Co9 50.14(17) . . ? P8 Co8 Co9 149.36(7) . . ? Co7 Co8 Co9 59.46(4) . . ? C92 Co9 C93 98.4(3) . . ? C92 Co9 C91 100.8(3) . . ? C93 Co9 C91 101.7(3) . . ? C92 Co9 C5 101.1(3) . . ? C93 Co9 C5 103.2(3) . . ? C91 Co9 C5 143.7(3) . . ? C92 Co9 Co7 150.3(2) . . ? C93 Co9 Co7 95.9(2) . . ? C91 Co9 Co7 101.6(2) . . ? C5 Co9 Co7 50.00(18) . . ? C92 Co9 Co8 97.2(2) . . ? C93 Co9 Co8 150.5(2) . . ? C91 Co9 Co8 99.7(2) . . ? C5 Co9 Co8 49.04(18) . . ? Co7 Co9 Co8 59.86(4) . . ? C302 Fe1 C301 41.2(8) . . ? C302 Fe1 C304 68.4(9) . . ? C301 Fe1 C304 70.7(10) . . ? C302 Fe1 C305 68.2(9) . . ? C301 Fe1 C305 38.6(9) . . ? C304 Fe1 C305 46.3(9) . . ? C302 Fe1 C102 114.1(6) . . ? C301 Fe1 C102 133.3(7) . . ? C304 Fe1 C102 148.7(8) . . ? C305 Fe1 C102 165.0(7) . . ? C302 Fe1 C101 119.5(6) . . ? C301 Fe1 C101 106.8(6) . . ? C304 Fe1 C101 165.7(8) . . ? C305 Fe1 C101 123.1(7) . . ? C102 Fe1 C101 42.2(3) . . ? C302 Fe1 C205 52.4(6) . . ? C301 Fe1 C205 18.5(6) . . ? C304 Fe1 C205 57.2(8) . . ? C305 Fe1 C205 20.1(7) . . ? C102 Fe1 C205 150.6(4) . . ? C101 Fe1 C205 116.5(4) . . ? C302 Fe1 C203 49.0(6) . . ? C301 Fe1 C203 70.9(7) . . ? C304 Fe1 C203 28.3(7) . . ? C305 Fe1 C203 64.4(8) . . ? C102 Fe1 C203 129.0(4) . . ? C101 Fe1 C203 165.4(4) . . ? C205 Fe1 C203 65.8(5) . . ? C302 Fe1 C105 149.4(6) . . ? C301 Fe1 C105 113.0(6) . . ? C304 Fe1 C105 126.0(8) . . ? C305 Fe1 C105 101.3(7) . . ? C102 Fe1 C105 69.0(3) . . ? C101 Fe1 C105 41.0(3) . . ? C205 Fe1 C105 109.0(4) . . ? C203 Fe1 C105 153.5(4) . . ? C302 Fe1 C103 135.4(6) . . ? C301 Fe1 C103 173.6(7) . . ? C304 Fe1 C103 114.2(8) . . ? C305 Fe1 C103 147.7(8) . . ? C102 Fe1 C103 40.6(3) . . ? C101 Fe1 C103 69.6(3) . . ? C205 Fe1 C103 167.9(5) . . ? C203 Fe1 C103 111.3(4) . . ? C105 Fe1 C103 68.0(3) . . ? C302 Fe1 C201 23.4(5) . . ? C301 Fe1 C201 22.2(6) . . ? C304 Fe1 C201 78.1(8) . . ? C305 Fe1 C201 58.6(8) . . ? C102 Fe1 C201 117.1(4) . . ? C101 Fe1 C201 105.0(4) . . ? C205 Fe1 C201 39.0(5) . . ? C203 Fe1 C201 67.1(5) . . ? C105 Fe1 C201 126.4(4) . . ? C103 Fe1 C201 152.2(5) . . ? C302 Fe1 C303 42.6(9) . . ? C301 Fe1 C303 72.2(9) . . ? C304 Fe1 C303 40.4(10) . . ? C305 Fe1 C303 73.4(10) . . ? C102 Fe1 C303 118.9(7) . . ? C101 Fe1 C303 153.4(7) . . ? C205 Fe1 C303 71.1(8) . . ? C203 Fe1 C303 12.1(8) . . ? C105 Fe1 C303 164.6(7) . . ? C103 Fe1 C303 108.5(8) . . ? C201 Fe1 C303 63.7(8) . . ? C605 Fe2 C402 162.9(5) . . ? C605 Fe2 C503 63.1(6) . . ? C402 Fe2 C503 130.4(4) . . ? C605 Fe2 C401 123.1(5) . . ? C402 Fe2 C401 41.7(3) . . ? C503 Fe2 C401 169.0(4) . . ? C605 Fe2 C604 41.1(5) . . ? C402 Fe2 C604 155.6(5) . . ? C503 Fe2 C604 29.6(5) . . ? C401 Fe2 C604 160.6(5) . . ? C605 Fe2 C405 104.7(5) . . ? C402 Fe2 C405 68.6(3) . . ? C503 Fe2 C405 149.5(4) . . ? C401 Fe2 C405 41.0(2) . . ? C604 Fe2 C405 123.3(4) . . ? C605 Fe2 C601 40.9(5) . . ? C402 Fe2 C601 127.4(5) . . ? C503 Fe2 C601 71.5(5) . . ? C401 Fe2 C601 106.9(5) . . ? C604 Fe2 C601 68.5(6) . . ? C405 Fe2 C601 119.1(5) . . ? C605 Fe2 C403 153.7(6) . . ? C402 Fe2 C403 40.0(3) . . ? C503 Fe2 C403 109.5(4) . . ? C401 Fe2 C403 69.1(3) . . ? C604 Fe2 C403 120.2(5) . . ? C405 Fe2 C403 68.2(3) . . ? C601 Fe2 C403 164.7(5) . . ? C605 Fe2 C602 68.8(7) . . ? C402 Fe2 C602 110.3(6) . . ? C503 Fe2 C602 50.4(6) . . ? C401 Fe2 C602 121.2(5) . . ? C604 Fe2 C602 68.4(6) . . ? C405 Fe2 C602 155.2(5) . . ? C601 Fe2 C602 40.5(5) . . ? C403 Fe2 C602 127.9(6) . . ? C605 Fe2 C505 18.1(5) . . ? C402 Fe2 C505 147.5(4) . . ? C503 Fe2 C505 67.8(4) . . ? C401 Fe2 C505 115.0(3) . . ? C604 Fe2 C505 53.6(6) . . ? C405 Fe2 C505 109.9(3) . . ? C601 Fe2 C505 23.1(5) . . ? C403 Fe2 C505 171.9(4) . . ? C602 Fe2 C505 56.9(6) . . ? C605 Fe2 C404 117.9(6) . . ? C402 Fe2 C404 67.7(3) . . ? C503 Fe2 C404 117.9(4) . . ? C401 Fe2 C404 68.6(3) . . ? C604 Fe2 C404 106.5(5) . . ? C405 Fe2 C404 40.1(2) . . ? C601 Fe2 C404 153.2(5) . . ? C403 Fe2 C404 40.5(3) . . ? C602 Fe2 C404 164.2(5) . . ? C505 Fe2 C404 133.1(4) . . ? C605 Fe2 C504 26.6(5) . . ? C402 Fe2 C504 170.1(4) . . ? C503 Fe2 C504 40.6(4) . . ? C401 Fe2 C504 147.9(4) . . ? C604 Fe2 C504 14.5(5) . . ? C405 Fe2 C504 117.4(4) . . ? C601 Fe2 C504 58.0(5) . . ? C403 Fe2 C504 132.8(4) . . ? C602 Fe2 C504 67.9(6) . . ? C505 Fe2 C504 40.3(4) . . ? C404 Fe2 C504 111.2(4) . . ? C702 Fe3 C701 41.5(3) . . ? C702 Fe3 C801 120.9(3) . . ? C701 Fe3 C801 104.7(3) . . ? C702 Fe3 C803 159.1(3) . . ? C701 Fe3 C803 159.2(4) . . ? C801 Fe3 C803 67.9(3) . . ? C702 Fe3 C804 122.0(3) . . ? C701 Fe3 C804 157.0(3) . . ? C801 Fe3 C804 68.0(3) . . ? C803 Fe3 C804 40.2(3) . . ? C702 Fe3 C805 105.3(3) . . ? C701 Fe3 C805 119.8(3) . . ? C801 Fe3 C805 40.6(3) . . ? C803 Fe3 C805 68.2(3) . . ? C804 Fe3 C805 40.6(3) . . ? C702 Fe3 C705 69.5(3) . . ? C701 Fe3 C705 41.1(3) . . ? C801 Fe3 C705 120.8(3) . . ? C803 Fe3 C705 124.6(3) . . ? C804 Fe3 C705 161.4(3) . . ? C805 Fe3 C705 156.2(3) . . ? C702 Fe3 C703 40.6(3) . . ? C701 Fe3 C703 69.0(3) . . ? C801 Fe3 C703 158.0(3) . . ? C803 Fe3 C703 125.0(3) . . ? C804 Fe3 C703 109.1(3) . . ? C805 Fe3 C703 122.8(3) . . ? C705 Fe3 C703 69.2(3) . . ? C702 Fe3 C802 157.8(3) . . ? C701 Fe3 C802 121.1(3) . . ? C801 Fe3 C802 41.2(3) . . ? C803 Fe3 C802 40.6(3) . . ? C804 Fe3 C802 68.7(3) . . ? C805 Fe3 C802 69.3(3) . . ? C705 Fe3 C802 106.3(3) . . ? C703 Fe3 C802 160.0(3) . . ? C702 Fe3 C704 68.1(3) . . ? C701 Fe3 C704 68.8(3) . . ? C801 Fe3 C704 159.2(3) . . ? C803 Fe3 C704 110.8(3) . . ? C804 Fe3 C704 125.5(3) . . ? C805 Fe3 C704 159.8(3) . . ? C705 Fe3 C704 41.5(2) . . ? C703 Fe3 C704 40.0(3) . . ? C802 Fe3 C704 124.0(3) . . ? O11 C11 Co1 177.2(6) . . ? O12 C12 Co1 177.8(7) . . ? O21 C21 Co2 175.8(6) . . ? O22 C22 Co2 179.8(8) . . ? O31 C31 Co3 177.4(7) . . ? O32 C32 Co3 177.6(7) . . ? O33 C33 Co3 177.6(7) . . ? C10 P1 C111 104.6(3) . . ? C10 P1 C121 102.4(3) . . ? C111 P1 C121 101.0(3) . . ? C10 P1 Co1 109.6(2) . . ? C111 P1 Co1 115.1(2) . . ? C121 P1 Co1 122.2(2) . . ? C112 C111 C116 119.2(7) . . ? C112 C111 P1 124.4(5) . . ? C116 C111 P1 116.3(5) . . ? C113 C112 C111 121.3(7) . . ? C113 C112 H112 119.3 . . ? C111 C112 H112 119.3 . . ? C112 C113 C114 119.6(7) . . ? C112 C113 H113 120.2 . . ? C114 C113 H113 120.2 . . ? C115 C114 C113 119.8(7) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 120.4(8) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 119.6(7) . . ? C115 C116 H116 120.2 . . ? C111 C116 H116 120.2 . . ? C126 C121 C122 119.8(7) . . ? C126 C121 P1 121.5(6) . . ? C122 C121 P1 118.5(6) . . ? C121 C122 C123 119.7(8) . . ? C121 C122 H122 120.2 . . ? C123 C122 H122 120.2 . . ? C124 C123 C122 119.9(9) . . ? C124 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? C123 C124 C125 121.3(8) . . ? C123 C124 H124 119.4 . . ? C125 C124 H124 119.4 . . ? C126 C125 C124 119.5(8) . . ? C126 C125 H125 120.2 . . ? C124 C125 H125 120.2 . . ? C125 C126 C121 119.8(8) . . ? C125 C126 H126 120.1 . . ? C121 C126 H126 120.1 . . ? P1 C10 P2 107.8(3) . . ? P1 C10 H10A 110.2 . . ? P2 C10 H10A 110.2 . . ? P1 C10 H10B 110.2 . . ? P2 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C211 P2 C221 100.2(3) . . ? C211 P2 C10 104.3(3) . . ? C221 P2 C10 105.4(3) . . ? C211 P2 Co2 115.3(2) . . ? C221 P2 Co2 120.4(2) . . ? C10 P2 Co2 109.6(2) . . ? C216 C211 C212 118.4(7) . . ? C216 C211 P2 118.4(6) . . ? C212 C211 P2 123.1(6) . . ? C213 C212 C211 121.4(8) . . ? C213 C212 H212 119.3 . . ? C211 C212 H212 119.3 . . ? C214 C213 C212 119.7(8) . . ? C214 C213 H213 120.2 . . ? C212 C213 H213 120.2 . . ? C213 C214 C215 120.1(8) . . ? C213 C214 H214 119.9 . . ? C215 C214 H214 119.9 . . ? C216 C215 C214 119.2(8) . . ? C216 C215 H215 120.4 . . ? C214 C215 H215 120.4 . . ? C211 C216 C215 121.2(8) . . ? C211 C216 H216 119.4 . . ? C215 C216 H216 119.4 . . ? C226 C221 C222 118.1(6) . . ? C226 C221 P2 120.1(5) . . ? C222 C221 P2 121.7(5) . . ? C221 C222 C223 121.1(7) . . ? C221 C222 H222 119.4 . . ? C223 C222 H222 119.4 . . ? C224 C223 C222 119.6(7) . . ? C224 C223 H223 120.2 . . ? C222 C223 H223 120.2 . . ? C225 C224 C223 120.5(7) . . ? C225 C224 H224 119.8 . . ? C223 C224 H224 119.8 . . ? C224 C225 C226 120.1(7) . . ? C224 C225 H225 120 . . ? C226 C225 H225 120 . . ? C221 C226 C225 120.6(7) . . ? C221 C226 H226 119.7 . . ? C225 C226 H226 119.7 . . ? C2 C1 Co1 146.4(5) . . ? C2 C1 Co2 123.3(5) . . ? Co1 C1 Co2 80.2(2) . . ? C2 C1 Co3 124.3(4) . . ? Co1 C1 Co3 79.9(2) . . ? Co2 C1 Co3 80.2(2) . . ? O2 C2 C1 120.4(6) . . ? O2 C2 C101 118.4(6) . . ? C1 C2 C101 121.1(6) . . ? C105 C101 C102 105.9(6) . . ? C105 C101 C2 131.8(6) . . ? C102 C101 C2 122.3(6) . . ? C105 C101 Fe1 70.1(4) . . ? C102 C101 Fe1 68.7(4) . . ? C2 C101 Fe1 123.0(4) . . ? C103 C102 C101 108.1(7) . . ? C103 C102 Fe1 70.6(4) . . ? C101 C102 Fe1 69.1(4) . . ? C103 C102 H102 126 . . ? C101 C102 H102 126 . . ? Fe1 C102 H102 126 . . ? C102 C103 C104 109.2(7) . . ? C102 C103 Fe1 68.8(4) . . ? C104 C103 Fe1 70.2(4) . . ? C102 C103 H103 125.4 . . ? C104 C103 H103 125.4 . . ? Fe1 C103 H103 127.2 . . ? C103 C104 C105 107.3(7) . . ? C103 C104 Fe1 69.5(4) . . ? C105 C104 Fe1 69.2(4) . . ? C103 C104 H104 126.4 . . ? C105 C104 H104 126.4 . . ? Fe1 C104 H104 126.5 . . ? C101 C105 C104 109.5(7) . . ? C101 C105 Fe1 68.9(4) . . ? C104 C105 Fe1 70.0(4) . . ? C101 C105 H105 125.3 . . ? C104 C105 H105 125.3 . . ? Fe1 C105 H105 127.5 . . ? C205 C201 C202 107.1(11) . . ? C205 C201 Fe1 70.1(7) . . ? C202 C201 Fe1 69.8(7) . . ? C205 C201 H201 126.4 . . ? C202 C201 H201 126.4 . . ? Fe1 C201 H201 125.2 . . ? C203 C202 C201 104.3(11) . . ? C203 C202 Fe1 69.1(8) . . ? C201 C202 Fe1 68.4(7) . . ? C203 C202 H202 127.9 . . ? C201 C202 H202 127.8 . . ? Fe1 C202 H202 126.2 . . ? C202 C203 C204 113.1(12) . . ? C202 C203 Fe1 71.2(7) . . ? C204 C203 Fe1 71.5(7) . . ? C202 C203 H203 123.4 . . ? C204 C203 H203 123.5 . . ? Fe1 C203 H203 125.5 . . ? C203 C204 C205 103.4(11) . . ? C203 C204 Fe1 68.7(7) . . ? C205 C204 Fe1 68.4(7) . . ? C203 C204 H204 128.3 . . ? C205 C204 H204 128.3 . . ? Fe1 C204 H204 126.1 . . ? C201 C205 C204 112.1(12) . . ? C201 C205 Fe1 70.8(7) . . ? C204 C205 Fe1 71.2(7) . . ? C201 C205 H205 124 . . ? C204 C205 H205 124 . . ? Fe1 C205 H205 125.6 . . ? C305 C301 C302 110.8(19) . . ? C305 C301 Fe1 71.6(14) . . ? C302 C301 Fe1 69.3(11) . . ? C305 C301 H301 124.6 . . ? C302 C301 H301 124.6 . . ? Fe1 C301 H301 126 . . ? C301 C302 C303 112.0(18) . . ? C301 C302 Fe1 69.4(11) . . ? C303 C302 Fe1 70.8(12) . . ? C301 C302 H302 124 . . ? C303 C302 H302 124 . . ? Fe1 C302 H302 127.5 . . ? C304 C303 C302 103(2) . . ? C304 C303 Fe1 67.9(14) . . ? C302 C303 Fe1 66.6(12) . . ? C304 C303 H303 128.6 . . ? C302 C303 H303 128.6 . . ? Fe1 C303 H303 128.3 . . ? C303 C304 C305 109(2) . . ? C303 C304 Fe1 71.7(14) . . ? C305 C304 Fe1 67.5(12) . . ? C303 C304 H304 125.3 . . ? C305 C304 H304 125.4 . . ? Fe1 C304 H304 127 . . ? C301 C305 C304 105(2) . . ? C301 C305 Fe1 69.7(14) . . ? C304 C305 Fe1 66.3(12) . . ? C301 C305 H305 127.5 . . ? C304 C305 H305 127.5 . . ? Fe1 C305 H305 128 . . ? O41 C41 Co4 177.7(6) . . ? O42 C42 Co4 177.4(7) . . ? O51 C51 Co5 179.0(6) . . ? O52 C52 Co5 178.0(6) . . ? O61 C61 Co6 177.7(7) . . ? O62 C62 Co6 177.8(7) . . ? O63 C63 Co6 178.6(7) . . ? C411 P4 C20 105.2(3) . . ? C411 P4 C421 98.9(3) . . ? C20 P4 C421 104.3(3) . . ? C411 P4 Co4 116.6(2) . . ? C20 P4 Co4 108.9(2) . . ? C421 P4 Co4 121.2(2) . . ? C412 C411 C416 118.7(7) . . ? C412 C411 P4 124.2(5) . . ? C416 C411 P4 117.1(5) . . ? C411 C412 C413 119.8(7) . . ? C411 C412 H412 120.1 . . ? C413 C412 H412 120.1 . . ? C414 C413 C412 121.1(7) . . ? C414 C413 H413 119.5 . . ? C412 C413 H413 119.5 . . ? C413 C414 C415 119.0(7) . . ? C413 C414 H414 120.5 . . ? C415 C414 H414 120.5 . . ? C416 C415 C414 120.1(7) . . ? C416 C415 H415 119.9 . . ? C414 C415 H415 119.9 . . ? C415 C416 C411 121.3(7) . . ? C415 C416 H416 119.4 . . ? C411 C416 H416 119.4 . . ? C422 C421 C426 119.2(6) . . ? C422 C421 P4 120.8(5) . . ? C426 C421 P4 119.9(5) . . ? C421 C422 C423 120.2(7) . . ? C421 C422 H422 119.9 . . ? C423 C422 H422 119.9 . . ? C424 C423 C422 119.7(7) . . ? C424 C423 H423 120.2 . . ? C422 C423 H423 120.2 . . ? C425 C424 C423 120.8(7) . . ? C425 C424 H424 119.6 . . ? C423 C424 H424 119.6 . . ? C424 C425 C426 119.3(7) . . ? C424 C425 H425 120.3 . . ? C426 C425 H425 120.3 . . ? C421 C426 C425 120.6(7) . . ? C421 C426 H426 119.7 . . ? C425 C426 H426 119.7 . . ? P5 C20 P4 107.9(3) . . ? P5 C20 H20A 110.1 . . ? P4 C20 H20A 110.1 . . ? P5 C20 H20B 110.1 . . ? P4 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? C20 P5 C511 104.3(3) . . ? C20 P5 C521 101.9(3) . . ? C511 P5 C521 101.9(3) . . ? C20 P5 Co5 111.1(2) . . ? C511 P5 Co5 114.5(2) . . ? C521 P5 Co5 121.2(2) . . ? C516 C511 C512 119.3(6) . . ? C516 C511 P5 117.7(5) . . ? C512 C511 P5 122.9(5) . . ? C513 C512 C511 119.5(7) . . ? C513 C512 H512 120.2 . . ? C511 C512 H512 120.2 . . ? C514 C513 C512 120.8(7) . . ? C514 C513 H513 119.6 . . ? C512 C513 H513 119.6 . . ? C513 C514 C515 119.9(7) . . ? C513 C514 H514 120 . . ? C515 C514 H514 120 . . ? C516 C515 C514 119.1(7) . . ? C516 C515 H515 120.4 . . ? C514 C515 H515 120.4 . . ? C511 C516 C515 121.2(7) . . ? C511 C516 H516 119.4 . . ? C515 C516 H516 119.4 . . ? C526 C521 C522 118.8(6) . . ? C526 C521 P5 121.4(5) . . ? C522 C521 P5 119.6(5) . . ? C521 C522 C523 119.9(7) . . ? C521 C522 H522 120.1 . . ? C523 C522 H522 120.1 . . ? C524 C523 C522 119.2(8) . . ? C524 C523 H523 120.4 . . ? C522 C523 H523 120.4 . . ? C523 C524 C525 121.3(7) . . ? C523 C524 H524 119.3 . . ? C525 C524 H524 119.3 . . ? C524 C525 C526 119.5(8) . . ? C524 C525 H525 120.3 . . ? C526 C525 H525 120.3 . . ? C525 C526 C521 121.3(7) . . ? C525 C526 H526 119.4 . . ? C521 C526 H526 119.4 . . ? C4 C3 Co4 144.1(5) . . ? C4 C3 Co5 123.1(4) . . ? Co4 C3 Co5 81.4(2) . . ? C4 C3 Co6 124.8(4) . . ? Co4 C3 Co6 81.6(2) . . ? Co5 C3 Co6 80.7(2) . . ? O4 C4 C401 118.4(6) . . ? O4 C4 C3 119.4(6) . . ? C401 C4 C3 122.1(6) . . ? C405 C401 C402 105.7(6) . . ? C405 C401 C4 132.2(6) . . ? C402 C401 C4 122.1(6) . . ? C405 C401 Fe2 69.6(3) . . ? C402 C401 Fe2 69.0(4) . . ? C4 C401 Fe2 123.7(4) . . ? C403 C402 C401 109.1(6) . . ? C403 C402 Fe2 70.7(4) . . ? C401 C402 Fe2 69.3(4) . . ? C403 C402 H402 125.4 . . ? C401 C402 H402 125.4 . . ? Fe2 C402 H402 126.1 . . ? C402 C403 C404 107.8(6) . . ? C402 C403 Fe2 69.2(4) . . ? C404 C403 Fe2 70.0(4) . . ? C402 C403 H403 126.1 . . ? C404 C403 H403 126.1 . . ? Fe2 C403 H403 126.2 . . ? C405 C404 C403 108.3(6) . . ? C405 C404 Fe2 69.2(4) . . ? C403 C404 Fe2 69.5(4) . . ? C405 C404 H404 125.8 . . ? C403 C404 H404 125.8 . . ? Fe2 C404 H404 127 . . ? C404 C405 C401 109.0(6) . . ? C404 C405 Fe2 70.6(4) . . ? C401 C405 Fe2 69.4(3) . . ? C404 C405 H405 125.5 . . ? C401 C405 H405 125.5 . . ? Fe2 C405 H405 126.1 . . ? C505 C501 C502 105.2(7) . . ? C505 C501 Fe2 68.0(5) . . ? C502 C501 Fe2 68.4(5) . . ? C505 C501 H501 127.7 . . ? C502 C501 H501 127.1 . . ? Fe2 C501 H501 127.9 . . ? C501 C502 C503 109.5(9) . . ? C501 C502 Fe2 71.8(5) . . ? C503 C502 Fe2 67.9(7) . . ? C501 C502 H502 125.3 . . ? C503 C502 H502 125.3 . . ? Fe2 C502 H502 126.6 . . ? C504 C503 C502 106.8(9) . . ? C504 C503 Fe2 70.9(7) . . ? C502 C503 Fe2 70.4(7) . . ? C504 C503 H503 126.6 . . ? C502 C503 H503 126.6 . . ? Fe2 C503 H503 123.7 . . ? C505 C504 C503 106.9(9) . . ? C505 C504 Fe2 69.5(6) . . ? C503 C504 Fe2 68.5(7) . . ? C505 C504 H504 126.5 . . ? C503 C504 H504 126.6 . . ? Fe2 C504 H504 127 . . ? C501 C505 C504 111.6(8) . . ? C501 C505 Fe2 72.3(5) . . ? C504 C505 Fe2 70.2(7) . . ? C501 C505 H505 124.2 . . ? C504 C505 H505 124.2 . . ? Fe2 C505 H505 124.9 . . ? C605 C601 C602 108.4(12) . . ? C605 C601 Fe2 68.6(10) . . ? C602 C601 Fe2 70.2(11) . . ? C605 C601 H601 125.8 . . ? C602 C601 H601 125.8 . . ? Fe2 C601 H601 126.9 . . ? C601 C602 C603 108.3(12) . . ? C601 C602 Fe2 69.3(10) . . ? C603 C602 Fe2 71.1(10) . . ? C601 C602 H602 125.8 . . ? C603 C602 H602 125.8 . . ? Fe2 C602 H602 125.4 . . ? C604 C603 C602 106.5(12) . . ? C604 C603 Fe2 67.7(9) . . ? C602 C603 Fe2 68.2(10) . . ? C604 C603 H603 126.7 . . ? C602 C603 H603 126.7 . . ? Fe2 C603 H603 128.8 . . ? C605 C604 C603 108.9(12) . . ? C605 C604 Fe2 68.6(10) . . ? C603 C604 Fe2 71.9(9) . . ? C605 C604 H604 125.5 . . ? C603 C604 H604 125.6 . . ? Fe2 C604 H604 125.5 . . ? C601 C605 C604 107.8(12) . . ? C601 C605 Fe2 70.5(10) . . ? C604 C605 Fe2 70.2(10) . . ? C601 C605 H605 126.1 . . ? C604 C605 H605 126.1 . . ? Fe2 C605 H605 124.8 . . ? O71 C71 Co7 176.3(6) . . ? O72 C72 Co7 178.9(7) . . ? O81 C81 Co8 176.6(6) . . ? O82 C82 Co8 177.8(7) . . ? O91 C91 Co9 177.8(7) . . ? O92 C92 Co9 175.1(7) . . ? O93 C93 Co9 178.9(7) . . ? C711 P7 C30 105.1(3) . . ? C711 P7 C721 100.5(3) . . ? C30 P7 C721 102.2(3) . . ? C711 P7 Co7 114.8(2) . . ? C30 P7 Co7 109.6(2) . . ? C721 P7 Co7 122.7(2) . . ? C712 C711 C716 118.9(6) . . ? C712 C711 P7 124.5(5) . . ? C716 C711 P7 116.6(5) . . ? C713 C712 C711 120.0(6) . . ? C713 C712 H712 120 . . ? C711 C712 H712 120 . . ? C714 C713 C712 120.8(7) . . ? C714 C713 H713 119.6 . . ? C712 C713 H713 119.6 . . ? C713 C714 C715 119.9(7) . . ? C713 C714 H714 120 . . ? C715 C714 H714 120 . . ? C716 C715 C714 120.1(7) . . ? C716 C715 H715 119.9 . . ? C714 C715 H715 119.9 . . ? C715 C716 C711 120.3(7) . . ? C715 C716 H716 119.9 . . ? C711 C716 H716 119.9 . . ? C722 C721 C726 118.3(6) . . ? C722 C721 P7 119.6(5) . . ? C726 C721 P7 121.6(5) . . ? C723 C722 C721 119.8(7) . . ? C723 C722 H722 120.1 . . ? C721 C722 H722 120.1 . . ? C724 C723 C722 121.3(7) . . ? C724 C723 H723 119.3 . . ? C722 C723 H723 119.3 . . ? C725 C724 C723 119.5(7) . . ? C725 C724 H724 120.3 . . ? C723 C724 H724 120.3 . . ? C724 C725 C726 120.1(7) . . ? C724 C725 H725 120 . . ? C726 C725 H725 120 . . ? C725 C726 C721 121.1(7) . . ? C725 C726 H726 119.5 . . ? C721 C726 H726 119.5 . . ? P7 C30 P8 106.8(3) . . ? P7 C30 H30A 110.4 . . ? P8 C30 H30A 110.4 . . ? P7 C30 H30B 110.4 . . ? P8 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? C821 P8 C811 101.0(3) . . ? C821 P8 C30 106.5(3) . . ? C811 P8 C30 102.9(3) . . ? C821 P8 Co8 117.7(2) . . ? C811 P8 Co8 117.0(2) . . ? C30 P8 Co8 110.2(2) . . ? C812 C811 C816 119.4(7) . . ? C812 C811 P8 122.2(5) . . ? C816 C811 P8 118.4(5) . . ? C811 C812 C813 121.1(7) . . ? C811 C812 H812 119.5 . . ? C813 C812 H812 119.5 . . ? C814 C813 C812 119.7(7) . . ? C814 C813 H813 120.2 . . ? C812 C813 H813 120.2 . . ? C815 C814 C813 119.2(7) . . ? C815 C814 H814 120.4 . . ? C813 C814 H814 120.4 . . ? C814 C815 C816 121.7(7) . . ? C814 C815 H815 119.2 . . ? C816 C815 H815 119.2 . . ? C815 C816 C811 118.9(7) . . ? C815 C816 H816 120.6 . . ? C811 C816 H816 120.6 . . ? C822 C821 C826 119.4(6) . . ? C822 C821 P8 121.9(5) . . ? C826 C821 P8 118.6(5) . . ? C823 C822 C821 120.1(7) . . ? C823 C822 H822 119.9 . . ? C821 C822 H822 119.9 . . ? C822 C823 C824 120.4(7) . . ? C822 C823 H823 119.8 . . ? C824 C823 H823 119.8 . . ? C825 C824 C823 119.2(7) . . ? C825 C824 H824 120.4 . . ? C823 C824 H824 120.4 . . ? C824 C825 C826 120.9(7) . . ? C824 C825 H825 119.5 . . ? C826 C825 H825 119.5 . . ? C825 C826 C821 119.8(7) . . ? C825 C826 H826 120.1 . . ? C821 C826 H826 120.1 . . ? C6 C5 Co8 122.1(5) . . ? C6 C5 Co7 148.7(5) . . ? Co8 C5 Co7 80.5(2) . . ? C6 C5 Co9 122.5(4) . . ? Co8 C5 Co9 80.8(2) . . ? Co7 C5 Co9 79.3(2) . . ? O6 C6 C5 121.0(6) . . ? O6 C6 C701 117.0(6) . . ? C5 C6 C701 122.0(6) . . ? C705 C701 C702 108.2(6) . . ? C705 C701 C6 128.6(6) . . ? C702 C701 C6 122.9(6) . . ? C705 C701 Fe3 70.3(4) . . ? C702 C701 Fe3 69.1(4) . . ? C6 C701 Fe3 120.7(5) . . ? C703 C702 C701 108.3(7) . . ? C703 C702 Fe3 70.7(4) . . ? C701 C702 Fe3 69.4(4) . . ? C703 C702 H702 125.8 . . ? C701 C702 H702 125.8 . . ? Fe3 C702 H702 125.7 . . ? C704 C703 C702 108.6(6) . . ? #===END # Attachment '6.br1437.cif' data_br1437 _database_code_depnum_ccdc_archive 'CCDC 754945' #TrackingRef '6.br1437.cif' _audit_creation_date 2008-10-12T10:06:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C72 H48 Cl4 Co6 O16 P4' _chemical_formula_moiety 'C70 H44 Co6 O16 P4, 2(C H2 Cl2)' _chemical_formula_weight 1788.36 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 13.1351(11) _cell_length_b 22.3563(9) _cell_length_c 13.8275(9) _cell_angle_alpha 90 _cell_angle_beta 116.671(9) _cell_angle_gamma 90 _cell_volume 3628.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3587 _cell_measurement_theta_min 3.3948 _cell_measurement_theta_max 32.2047 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.91 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0135241138 _diffrn_orient_matrix_ub_12 0.0303362919 _diffrn_orient_matrix_ub_13 -0.0150471996 _diffrn_orient_matrix_ub_21 -0.0513765435 _diffrn_orient_matrix_ub_22 -0.0090326118 _diffrn_orient_matrix_ub_23 -0.0445145133 _diffrn_orient_matrix_ub_31 -0.028557292 _diffrn_orient_matrix_ub_32 0.0016870092 _diffrn_orient_matrix_ub_33 0.032879459 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_unetI/netI 0.1066 _diffrn_reflns_number 37240 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 29 _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 9628 _reflns_number_gt 5783 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0599P)^2^+0.0000P] 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_number_reflns 9628 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.646 _refine_diff_density_min -1.746 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cl Cl 0.1484 0.1585 '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' 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 0.42020(4) 0.57571(2) 0.28572(4) 0.01420(12) Uani 1 1 d . . . Co2 Co 0.55230(4) 0.63085(2) 0.23215(4) 0.01221(11) Uani 1 1 d . . . Co3 Co 0.59051(4) 0.52547(2) 0.29329(4) 0.01559(12) Uani 1 1 d . . . C11 C 0.4670(3) 0.58191(17) 0.4298(3) 0.0227(9) Uani 1 1 d . . . O11 O 0.4981(3) 0.58274(13) 0.5210(2) 0.0358(7) Uani 1 1 d . . . C12 C 0.3219(3) 0.51510(18) 0.2474(3) 0.0243(9) Uani 1 1 d . . . O12 O 0.2597(3) 0.47614(13) 0.2184(3) 0.0353(7) Uani 1 1 d . . . C21 C 0.6261(3) 0.66323(16) 0.3645(3) 0.0174(8) Uani 1 1 d . . . O21 O 0.6703(2) 0.68191(12) 0.4503(2) 0.0259(6) Uani 1 1 d . . . C22 C 0.6430(3) 0.63722(16) 0.1681(3) 0.0177(8) Uani 1 1 d . . . O22 O 0.6996(2) 0.64125(13) 0.1252(2) 0.0294(7) Uani 1 1 d . . . C31 C 0.6763(3) 0.52874(17) 0.4396(3) 0.0236(9) Uani 1 1 d . . . O31 O 0.7291(3) 0.52994(14) 0.5312(2) 0.0382(8) Uani 1 1 d . . . C32 C 0.5292(4) 0.45237(18) 0.2709(3) 0.0261(9) Uani 1 1 d . . . O32 O 0.4840(3) 0.40789(13) 0.2499(3) 0.0416(8) Uani 1 1 d . . . C33 C 0.7007(3) 0.51394(17) 0.2516(3) 0.0224(8) Uani 1 1 d . . . O33 O 0.7712(2) 0.50614(13) 0.2274(2) 0.0313(7) Uani 1 1 d . . . P1 P 0.28648(8) 0.64404(4) 0.22365(7) 0.0142(2) Uani 1 1 d . . . C111 C 0.1433(3) 0.61371(16) 0.1731(3) 0.0172(8) Uani 1 1 d . . . C112 C 0.0771(3) 0.60019(17) 0.0650(3) 0.0208(8) Uani 1 1 d . . . H112 H 0.1031 0.6104 0.0132 0.025 Uiso 1 1 calc R . . C113 C -0.0272(3) 0.57185(17) 0.0320(3) 0.0271(9) Uani 1 1 d . . . H113 H -0.072 0.5628 -0.0424 0.033 Uiso 1 1 calc R . . C114 C -0.0664(3) 0.55684(16) 0.1053(3) 0.0214(8) Uani 1 1 d . . . H114 H -0.1382 0.5378 0.082 0.026 Uiso 1 1 calc R . . C115 C -0.0008(3) 0.56954(19) 0.2128(3) 0.0312(10) Uani 1 1 d . . . H115 H -0.0275 0.5591 0.264 0.037 Uiso 1 1 calc R . . C116 C 0.1038(4) 0.5975(2) 0.2476(3) 0.0333(11) Uani 1 1 d . . . H116 H 0.1487 0.6055 0.3223 0.04 Uiso 1 1 calc R . . C121 C 0.2866(3) 0.70458(16) 0.3126(3) 0.0160(7) Uani 1 1 d . . . C122 C 0.3873(3) 0.72095(16) 0.4019(3) 0.0195(8) Uani 1 1 d . . . H122 H 0.4552 0.699 0.4191 0.023 Uiso 1 1 calc R . . C123 C 0.3891(4) 0.76900(18) 0.4657(3) 0.0291(10) Uani 1 1 d . . . H123 H 0.4583 0.7802 0.526 0.035 Uiso 1 1 calc R . . C124 C 0.2907(4) 0.80052(19) 0.4419(4) 0.0307(10) Uani 1 1 d . . . H124 H 0.2917 0.8333 0.4859 0.037 Uiso 1 1 calc R . . C125 C 0.1920(4) 0.78467(19) 0.3553(4) 0.0345(11) Uani 1 1 d . . . H125 H 0.1243 0.8065 0.3394 0.041 Uiso 1 1 calc R . . C126 C 0.1888(3) 0.73696(18) 0.2896(3) 0.0268(9) Uani 1 1 d . . . H126 H 0.1194 0.7266 0.2289 0.032 Uiso 1 1 calc R . . C0 C 0.2887(3) 0.68317(16) 0.1080(3) 0.0164(8) Uani 1 1 d . . . H0A H 0.2404 0.7194 0.0909 0.02 Uiso 1 1 calc R . . H0B H 0.2579 0.6568 0.0437 0.02 Uiso 1 1 calc R . . P2 P 0.43594(7) 0.70426(4) 0.14173(7) 0.01317(19) Uani 1 1 d . . . C211 C 0.4218(3) 0.72472(17) 0.0076(3) 0.0171(8) Uani 1 1 d . . . C212 C 0.4111(3) 0.67983(18) -0.0656(3) 0.0253(9) Uani 1 1 d . . . H212 H 0.4171 0.6391 -0.0439 0.03 Uiso 1 1 calc R . . C213 C 0.3916(4) 0.6938(2) -0.1702(3) 0.0302(10) Uani 1 1 d . . . H213 H 0.3831 0.6625 -0.2198 0.036 Uiso 1 1 calc R . . C214 C 0.3845(3) 0.7524(2) -0.2033(3) 0.0294(10) Uani 1 1 d . . . H214 H 0.3711 0.7617 -0.2751 0.035 Uiso 1 1 calc R . . C215 C 0.3972(4) 0.7971(2) -0.1308(4) 0.0367(11) Uani 1 1 d . . . H215 H 0.3937 0.8377 -0.1523 0.044 Uiso 1 1 calc R . . C216 C 0.4152(3) 0.78363(18) -0.0253(3) 0.0269(9) Uani 1 1 d . . . H216 H 0.4229 0.815 0.0238 0.032 Uiso 1 1 calc R . . C221 C 0.4634(3) 0.77700(15) 0.2081(3) 0.0154(7) Uani 1 1 d . . . C222 C 0.5771(3) 0.79670(17) 0.2604(3) 0.0203(8) Uani 1 1 d . . . H222 H 0.6371 0.7703 0.2686 0.024 Uiso 1 1 calc R . . C223 C 0.6017(4) 0.85456(16) 0.2999(3) 0.0255(9) Uani 1 1 d . . . H223 H 0.6786 0.8678 0.3346 0.031 Uiso 1 1 calc R . . C224 C 0.5157(4) 0.89291(17) 0.2891(3) 0.0296(10) Uani 1 1 d . . . H224 H 0.533 0.9328 0.3152 0.036 Uiso 1 1 calc R . . C225 C 0.4039(4) 0.87346(18) 0.2401(3) 0.0277(9) Uani 1 1 d . . . H225 H 0.3447 0.8998 0.2344 0.033 Uiso 1 1 calc R . . C226 C 0.3773(3) 0.81577(17) 0.1991(3) 0.0215(8) Uani 1 1 d . . . H226 H 0.3001 0.8029 0.165 0.026 Uiso 1 1 calc R . . C1 C 0.4628(3) 0.56201(15) 0.1747(3) 0.0159(7) Uani 1 1 d . . . C2 C 0.4007(3) 0.54153(15) 0.0619(3) 0.0169(8) Uani 1 1 d . . . O2 O 0.2985(2) 0.54821(12) 0.0048(2) 0.0254(6) Uani 1 1 d . . . C3 C 0.4717(3) 0.51216(15) 0.0182(3) 0.0166(8) Uani 1 1 d . . . Cl1 Cl 0.92828(15) 0.42904(8) 0.48593(14) 0.0790(5) Uani 1 1 d . A 1 Cl2 Cl 0.73225(18) 0.35882(9) 0.45568(13) 0.0890(6) Uani 1 1 d . A 1 C01 C 0.8400(8) 0.3732(5) 0.4256(8) 0.131(3) Uiso 1 1 d . A 1 H01A H 0.8863 0.3363 0.4404 0.157 Uiso 1 1 calc R A 1 H01B H 0.8065 0.3804 0.3467 0.157 Uiso 1 1 calc R A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0169(3) 0.0138(2) 0.0154(3) -0.0018(2) 0.0104(2) -0.0015(2) Co2 0.0123(2) 0.0127(2) 0.0120(2) -0.0015(2) 0.00582(19) -0.00153(19) Co3 0.0192(3) 0.0142(2) 0.0155(3) 0.0001(2) 0.0097(2) 0.0018(2) C11 0.024(2) 0.019(2) 0.028(2) 0.0026(18) 0.0146(18) 0.0016(16) O11 0.0445(19) 0.0459(19) 0.0201(16) 0.0082(15) 0.0174(14) 0.0143(16) C12 0.029(2) 0.024(2) 0.030(2) 0.0004(18) 0.0223(19) 0.0033(18) O12 0.0406(18) 0.0234(15) 0.050(2) -0.0103(15) 0.0275(16) -0.0160(14) C21 0.0151(19) 0.0181(18) 0.019(2) 0.0009(16) 0.0076(16) 0.0003(15) O21 0.0268(16) 0.0291(15) 0.0171(14) -0.0059(13) 0.0057(12) -0.0013(12) C22 0.0174(19) 0.0159(18) 0.0163(18) 0.0009(15) 0.0045(15) 0.0002(15) O22 0.0312(17) 0.0370(17) 0.0309(16) 0.0027(13) 0.0235(14) 0.0008(13) C31 0.026(2) 0.0199(19) 0.027(2) 0.0051(18) 0.0140(18) 0.0090(17) O31 0.0395(19) 0.050(2) 0.0178(16) 0.0014(15) 0.0067(14) 0.0113(16) C32 0.037(3) 0.022(2) 0.028(2) 0.0003(18) 0.022(2) 0.0028(19) O32 0.060(2) 0.0197(16) 0.059(2) -0.0091(16) 0.0383(19) -0.0071(15) C33 0.022(2) 0.026(2) 0.0181(19) 0.0022(17) 0.0084(17) 0.0042(17) O33 0.0226(16) 0.0453(18) 0.0289(16) 0.0042(14) 0.0142(13) 0.0082(14) P1 0.0133(5) 0.0169(5) 0.0133(5) -0.0029(4) 0.0068(4) -0.0027(4) C111 0.0131(19) 0.0180(18) 0.0214(19) -0.0020(16) 0.0085(16) -0.0011(14) C112 0.0138(19) 0.026(2) 0.020(2) 0.0040(17) 0.0055(16) -0.0042(16) C113 0.019(2) 0.027(2) 0.023(2) 0.0009(18) -0.0014(17) -0.0057(17) C114 0.0136(19) 0.0175(18) 0.032(2) -0.0034(17) 0.0087(17) -0.0044(15) C115 0.031(2) 0.043(3) 0.031(2) -0.012(2) 0.024(2) -0.020(2) C116 0.028(2) 0.052(3) 0.024(2) -0.012(2) 0.0159(19) -0.018(2) C121 0.0183(19) 0.0156(17) 0.0173(18) -0.0026(15) 0.0108(16) -0.0003(15) C122 0.020(2) 0.0206(19) 0.0192(19) -0.0014(16) 0.0094(16) 0.0004(16) C123 0.029(2) 0.029(2) 0.026(2) -0.0134(19) 0.0088(19) -0.0060(18) C124 0.035(3) 0.028(2) 0.038(3) -0.016(2) 0.024(2) -0.0065(19) C125 0.024(2) 0.029(2) 0.054(3) -0.016(2) 0.021(2) 0.0044(18) C126 0.019(2) 0.027(2) 0.034(2) -0.0076(19) 0.0112(19) -0.0033(17) C0 0.0159(19) 0.0195(18) 0.0150(18) -0.0032(15) 0.0081(15) -0.0025(15) P2 0.0122(5) 0.0140(4) 0.0130(4) -0.0006(4) 0.0054(4) -0.0014(4) C211 0.0114(18) 0.026(2) 0.0157(18) 0.0029(16) 0.0073(15) -0.0010(15) C212 0.031(2) 0.026(2) 0.022(2) 0.0017(18) 0.0145(18) 0.0073(18) C213 0.034(2) 0.042(3) 0.019(2) -0.0015(19) 0.0165(19) 0.012(2) C214 0.026(2) 0.045(3) 0.020(2) 0.008(2) 0.0133(18) 0.008(2) C215 0.049(3) 0.034(3) 0.028(2) 0.011(2) 0.018(2) -0.002(2) C216 0.034(2) 0.026(2) 0.021(2) 0.0035(18) 0.0129(19) -0.0009(18) C221 0.021(2) 0.0129(17) 0.0117(17) 0.0009(14) 0.0063(15) -0.0017(14) C222 0.020(2) 0.0189(19) 0.022(2) 0.0000(16) 0.0087(16) -0.0016(15) C223 0.028(2) 0.018(2) 0.026(2) 0.0000(17) 0.0080(18) -0.0077(17) C224 0.053(3) 0.0120(19) 0.023(2) -0.0045(17) 0.016(2) -0.0047(19) C225 0.042(3) 0.021(2) 0.022(2) 0.0011(18) 0.0163(19) 0.0123(19) C226 0.024(2) 0.023(2) 0.0169(19) 0.0005(16) 0.0086(17) 0.0029(16) C1 0.020(2) 0.0141(17) 0.0163(18) 0.0010(15) 0.0104(16) 0.0002(14) C2 0.019(2) 0.0146(18) 0.0196(19) -0.0028(15) 0.0112(16) -0.0041(15) O2 0.0152(15) 0.0348(16) 0.0232(15) -0.0102(12) 0.0059(12) -0.0022(12) C3 0.0148(19) 0.0172(19) 0.0135(18) -0.0032(15) 0.0027(14) -0.0046(14) Cl1 0.0787(12) 0.0975(13) 0.0650(11) 0.0256(10) 0.0361(9) 0.0216(10) Cl2 0.1254(16) 0.1056(15) 0.0473(9) -0.0152(9) 0.0487(10) -0.0420(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.780(4) . ? Co1 C11 1.807(4) . ? Co1 C1 1.879(4) . ? Co1 P1 2.1914(11) . ? Co1 Co3 2.4631(7) . ? Co1 Co2 2.4965(7) . ? Co2 C22 1.781(4) . ? Co2 C21 1.795(4) . ? Co2 C1 1.883(4) . ? Co2 P2 2.2084(10) . ? Co2 Co3 2.4769(7) . ? Co3 C32 1.786(4) . ? Co3 C33 1.800(4) . ? Co3 C31 1.822(4) . ? Co3 C1 1.924(4) . ? C11 O11 1.138(4) . ? C12 O12 1.137(4) . ? C21 O21 1.140(4) . ? C22 O22 1.144(4) . ? C31 O31 1.139(4) . ? C32 O32 1.128(5) . ? C33 O33 1.131(4) . ? P1 C111 1.818(4) . ? P1 C121 1.828(4) . ? P1 C0 1.834(4) . ? C111 C112 1.384(5) . ? C111 C116 1.393(5) . ? C112 C113 1.387(5) . ? C112 H112 0.95 . ? C113 C114 1.368(6) . ? C113 H113 0.95 . ? C114 C115 1.373(5) . ? C114 H114 0.95 . ? C115 C116 1.384(5) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.382(5) . ? C121 C122 1.393(5) . ? C122 C123 1.384(5) . ? C122 H122 0.95 . ? C123 C124 1.376(6) . ? C123 H123 0.95 . ? C124 C125 1.358(6) . ? C124 H124 0.95 . ? C125 C126 1.389(6) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C0 P2 1.836(3) . ? C0 H0A 0.99 . ? C0 H0B 0.99 . ? P2 C221 1.822(4) . ? P2 C211 1.837(4) . ? C211 C216 1.383(5) . ? C211 C212 1.387(5) . ? C212 C213 1.387(5) . ? C212 H212 0.95 . ? C213 C214 1.376(6) . ? C213 H213 0.95 . ? C214 C215 1.373(6) . ? C214 H214 0.95 . ? C215 C216 1.402(6) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.386(5) . ? C221 C222 1.406(5) . ? C222 C223 1.385(5) . ? C222 H222 0.95 . ? C223 C224 1.372(6) . ? C223 H223 0.95 . ? C224 C225 1.383(6) . ? C224 H224 0.95 . ? C225 C226 1.389(5) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C1 C2 1.472(5) . ? C2 O2 1.223(4) . ? C2 C3 1.473(5) . ? C3 C3 1.199(7) 3_665 ? Cl1 C01 1.653(9) . ? Cl2 C01 1.675(9) . ? C01 H01A 0.99 . ? C01 H01B 0.99 . ? 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 C12 Co1 C11 103.23(18) . . ? C12 Co1 C1 94.28(16) . . ? C11 Co1 C1 146.52(17) . . ? C12 Co1 P1 93.87(13) . . ? C11 Co1 P1 101.21(12) . . ? C1 Co1 P1 105.88(11) . . ? C12 Co1 Co3 100.89(12) . . ? C11 Co1 Co3 97.77(12) . . ? C1 Co1 Co3 50.43(11) . . ? P1 Co1 Co3 152.57(4) . . ? C12 Co1 Co2 142.67(12) . . ? C11 Co1 Co2 110.58(12) . . ? C1 Co1 Co2 48.48(11) . . ? P1 Co1 Co2 94.66(3) . . ? Co3 Co1 Co2 59.919(19) . . ? C22 Co2 C21 107.42(16) . . ? C22 Co2 C1 106.64(16) . . ? C21 Co2 C1 135.17(16) . . ? C22 Co2 P2 96.11(12) . . ? C21 Co2 P2 101.38(12) . . ? C1 Co2 P2 103.07(11) . . ? C22 Co2 Co3 99.65(11) . . ? C21 Co2 Co3 95.83(12) . . ? C1 Co2 Co3 50.13(11) . . ? P2 Co2 Co3 151.98(3) . . ? C22 Co2 Co1 153.67(12) . . ? C21 Co2 Co1 91.48(12) . . ? C1 Co2 Co1 48.37(11) . . ? P2 Co2 Co1 97.95(3) . . ? Co3 Co2 Co1 59.370(19) . . ? C32 Co3 C33 100.24(18) . . ? C32 Co3 C31 103.59(18) . . ? C33 Co3 C31 100.13(17) . . ? C32 Co3 C1 95.04(17) . . ? C33 Co3 C1 107.88(16) . . ? C31 Co3 C1 142.85(16) . . ? C32 Co3 Co1 94.58(13) . . ? C33 Co3 Co1 153.76(12) . . ? C31 Co3 Co1 97.24(12) . . ? C1 Co3 Co1 48.85(11) . . ? C32 Co3 Co2 143.56(14) . . ? C33 Co3 Co2 95.50(12) . . ? C31 Co3 Co2 105.69(12) . . ? C1 Co3 Co2 48.68(10) . . ? Co1 Co3 Co2 60.711(19) . . ? O11 C11 Co1 176.4(4) . . ? O12 C12 Co1 176.7(4) . . ? O21 C21 Co2 176.7(3) . . ? O22 C22 Co2 178.8(3) . . ? O31 C31 Co3 178.9(4) . . ? O32 C32 Co3 174.8(4) . . ? O33 C33 Co3 178.6(4) . . ? C111 P1 C121 102.91(16) . . ? C111 P1 C0 105.14(16) . . ? C121 P1 C0 103.75(17) . . ? C111 P1 Co1 113.54(12) . . ? C121 P1 Co1 119.61(12) . . ? C0 P1 Co1 110.51(12) . . ? C112 C111 C116 118.6(3) . . ? C112 C111 P1 122.5(3) . . ? C116 C111 P1 118.5(3) . . ? C111 C112 C113 120.3(4) . . ? C111 C112 H112 119.9 . . ? C113 C112 H112 119.9 . . ? C114 C113 C112 120.8(4) . . ? C114 C113 H113 119.6 . . ? C112 C113 H113 119.6 . . ? C113 C114 C115 119.3(4) . . ? C113 C114 H114 120.3 . . ? C115 C114 H114 120.3 . . ? C114 C115 C116 120.8(4) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? C115 C116 C111 120.2(4) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C126 C121 C122 118.7(3) . . ? C126 C121 P1 120.9(3) . . ? C122 C121 P1 120.3(3) . . ? C123 C122 C121 120.5(4) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C124 C123 C122 119.9(4) . . ? C124 C123 H123 120 . . ? C122 C123 H123 120 . . ? C125 C124 C123 120.0(4) . . ? C125 C124 H124 120 . . ? C123 C124 H124 120 . . ? C124 C125 C126 120.9(4) . . ? C124 C125 H125 119.6 . . ? C126 C125 H125 119.6 . . ? C121 C126 C125 120.0(4) . . ? C121 C126 H126 120 . . ? C125 C126 H126 120 . . ? P1 C0 P2 109.17(18) . . ? P1 C0 H0A 109.8 . . ? P2 C0 H0A 109.8 . . ? P1 C0 H0B 109.8 . . ? P2 C0 H0B 109.8 . . ? H0A C0 H0B 108.3 . . ? C221 P2 C0 107.73(17) . . ? C221 P2 C211 101.17(17) . . ? data_br1438 _database_code_depnum_ccdc_archive 'CCDC 754946' #TrackingRef '8.br1438.cif' _audit_creation_date 2008-11-05T15:33:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C80 H48 Co6 O14 P4' _chemical_formula_moiety 'C80 H48 Co6 O14 P4' _chemical_formula_weight 1710.64 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 12.4783(4) _cell_length_b 24.8382(5) _cell_length_c 13.2345(3) _cell_angle_alpha 90 _cell_angle_beta 112.622(3) _cell_angle_gamma 90 _cell_volume 3786.29(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9730 _cell_measurement_theta_min 2.8545 _cell_measurement_theta_max 31.7926 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.5 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max .89 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0421142376 _diffrn_orient_matrix_ub_12 0.0179028548 _diffrn_orient_matrix_ub_13 -0.0051589594 _diffrn_orient_matrix_ub_21 0.0384481594 _diffrn_orient_matrix_ub_22 -0.0220653094 _diffrn_orient_matrix_ub_23 0.0062755947 _diffrn_orient_matrix_ub_31 -0.0235706723 _diffrn_orient_matrix_ub_32 -0.0040221365 _diffrn_orient_matrix_ub_33 -0.0575986956 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_unetI/netI 0.0736 _diffrn_reflns_number 29608 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 8689 _reflns_number_gt 6065 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0507P)^2^+0.0000P] 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_number_reflns 8689 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.846 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.79030(4) 0.409337(17) 0.32529(3) 0.01842(11) Uani 1 1 d . . . Co2 Co 0.72238(4) 0.366787(17) 0.45914(3) 0.01861(11) Uani 1 1 d . . . Co3 Co 0.77013(4) 0.464140(18) 0.47531(3) 0.02191(12) Uani 1 1 d . . . C11 C 0.9459(3) 0.39912(13) 0.3757(3) 0.0251(8) Uani 1 1 d . . . O11 O 1.0440(2) 0.39497(11) 0.4064(2) 0.0392(7) Uani 1 1 d . . . C12 C 0.7681(3) 0.46272(14) 0.2287(3) 0.0259(8) Uani 1 1 d . . . O12 O 0.7485(2) 0.49712(10) 0.1678(2) 0.0400(7) Uani 1 1 d . . . C21 C 0.8584(3) 0.33300(14) 0.5244(3) 0.0248(8) Uani 1 1 d . . . O21 O 0.9452(2) 0.31124(11) 0.5649(2) 0.0381(6) Uani 1 1 d . . . C22 C 0.6647(3) 0.36512(15) 0.5628(3) 0.0303(8) Uani 1 1 d . . . O22 O 0.6304(3) 0.36329(12) 0.6304(2) 0.0478(8) Uani 1 1 d . . . C31 C 0.9172(3) 0.45729(14) 0.5766(3) 0.0280(8) Uani 1 1 d . . . O31 O 1.0085(2) 0.45230(11) 0.6411(2) 0.0429(7) Uani 1 1 d . . . C32 C 0.7606(3) 0.52877(16) 0.4121(3) 0.0324(9) Uani 1 1 d . . . O32 O 0.7486(3) 0.56992(11) 0.3711(2) 0.0470(7) Uani 1 1 d . . . C33 C 0.6842(3) 0.48145(16) 0.5514(3) 0.0359(9) Uani 1 1 d . . . O33 O 0.6254(3) 0.49269(14) 0.5960(3) 0.0658(10) Uani 1 1 d . . . P1 P 0.71785(7) 0.34515(3) 0.20300(6) 0.01873(18) Uani 1 1 d . . . C111 C 0.6689(3) 0.36944(12) 0.0622(2) 0.0222(7) Uani 1 1 d . . . C112 C 0.5633(3) 0.39551(15) 0.0142(3) 0.0310(8) Uani 1 1 d . . . H112 H 0.5128 0.398 0.0525 0.037 Uiso 1 1 calc R . . C113 C 0.5304(4) 0.41811(15) -0.0893(3) 0.0359(9) Uani 1 1 d . . . H113 H 0.4574 0.4355 -0.1222 0.043 Uiso 1 1 calc R . . C114 C 0.6041(4) 0.41513(14) -0.1442(3) 0.0373(10) Uani 1 1 d . . . H114 H 0.5817 0.4303 -0.2152 0.045 Uiso 1 1 calc R . . C115 C 0.7096(4) 0.39036(16) -0.0968(3) 0.0378(10) Uani 1 1 d . . . H115 H 0.7603 0.3887 -0.135 0.045 Uiso 1 1 calc R . . C116 C 0.7429(3) 0.36785(15) 0.0060(3) 0.0323(8) Uani 1 1 d . . . H116 H 0.8168 0.3511 0.0386 0.039 Uiso 1 1 calc R . . C121 C 0.8007(3) 0.28480(13) 0.2016(3) 0.0225(7) Uani 1 1 d . . . C122 C 0.8985(3) 0.27012(14) 0.2914(3) 0.0258(8) Uani 1 1 d . . . H122 H 0.9277 0.2933 0.3532 0.031 Uiso 1 1 calc R . . C123 C 0.9541(3) 0.22151(14) 0.2915(3) 0.0332(9) Uani 1 1 d . . . H123 H 1.0216 0.2117 0.3529 0.04 Uiso 1 1 calc R . . C124 C 0.9114(4) 0.18775(15) 0.2026(3) 0.0366(9) Uani 1 1 d . . . H124 H 0.9496 0.1546 0.2027 0.044 Uiso 1 1 calc R . . C125 C 0.8141(4) 0.20165(15) 0.1138(3) 0.0410(10) Uani 1 1 d . . . H125 H 0.785 0.1781 0.0528 0.049 Uiso 1 1 calc R . . C126 C 0.7580(4) 0.24973(14) 0.1125(3) 0.0336(9) Uani 1 1 d . . . H126 H 0.6902 0.259 0.0509 0.04 Uiso 1 1 calc R . . C0 C 0.5862(3) 0.31642(13) 0.2122(2) 0.0199(7) Uani 1 1 d . . . H0A H 0.5205 0.3417 0.1798 0.024 Uiso 1 1 calc R . . H0B H 0.5661 0.2823 0.1704 0.024 Uiso 1 1 calc R . . P2 P 0.61016(7) 0.30365(3) 0.35597(6) 0.01946(19) Uani 1 1 d . . . C211 C 0.4600(3) 0.29900(14) 0.3475(2) 0.0235(7) Uani 1 1 d . . . C212 C 0.4060(3) 0.34439(15) 0.3660(3) 0.0298(8) Uani 1 1 d . . . H212 H 0.45 0.3763 0.3919 0.036 Uiso 1 1 calc R . . C213 C 0.2890(3) 0.34403(17) 0.3474(3) 0.0372(9) Uani 1 1 d . . . H213 H 0.2526 0.3758 0.3584 0.045 Uiso 1 1 calc R . . C214 C 0.2258(3) 0.29768(18) 0.3131(3) 0.0410(10) Uani 1 1 d . . . H214 H 0.1456 0.2972 0.3005 0.049 Uiso 1 1 calc R . . C215 C 0.2793(3) 0.25158(17) 0.2968(3) 0.0390(10) Uani 1 1 d . . . H215 H 0.2357 0.2193 0.274 0.047 Uiso 1 1 calc R . . C216 C 0.3960(3) 0.25199(16) 0.3134(3) 0.0322(9) Uani 1 1 d . . . H216 H 0.432 0.2203 0.3015 0.039 Uiso 1 1 calc R . . C221 C 0.6648(3) 0.23494(13) 0.3877(3) 0.0232(7) Uani 1 1 d . . . C222 C 0.7084(3) 0.21968(14) 0.4980(3) 0.0290(8) Uani 1 1 d . . . H222 H 0.708 0.2446 0.5523 0.035 Uiso 1 1 calc R . . C223 C 0.7520(3) 0.16867(15) 0.5279(3) 0.0354(9) Uani 1 1 d . . . H223 H 0.7809 0.1584 0.6028 0.043 Uiso 1 1 calc R . . C224 C 0.7542(3) 0.13244(15) 0.4502(3) 0.0340(9) Uani 1 1 d . . . H224 H 0.7859 0.0975 0.4715 0.041 Uiso 1 1 calc R . . C225 C 0.7101(3) 0.14686(14) 0.3413(3) 0.0315(9) Uani 1 1 d . . . H225 H 0.7104 0.1216 0.2874 0.038 Uiso 1 1 calc R . . C226 C 0.6656(3) 0.19772(14) 0.3102(3) 0.0266(8) Uani 1 1 d . . . H226 H 0.6352 0.2073 0.235 0.032 Uiso 1 1 calc R . . C1 C 0.6579(3) 0.42361(13) 0.3583(2) 0.0194(7) Uani 1 1 d . . . C2 C 0.5466(3) 0.43909(13) 0.2897(2) 0.0214(7) Uani 1 1 d . . . C3 C 0.4469(3) 0.44955(14) 0.2299(3) 0.0260(8) Uani 1 1 d . . . C4 C 0.3332(3) 0.46045(14) 0.1699(3) 0.0283(8) Uani 1 1 d . . . C5 C 0.2331(3) 0.47066(15) 0.1179(3) 0.0322(9) Uani 1 1 d . . . C6 C 0.1148(3) 0.48497(15) 0.0583(3) 0.0302(8) Uani 1 1 d . . . C7 C 0.0527(4) 0.5083(2) 0.1102(3) 0.0596(14) Uani 1 1 d . . . H7 H 0.0879 0.5141 0.187 0.072 Uiso 1 1 calc R . . C8 C 0.0617(4) 0.4759(2) -0.0538(3) 0.0618(15) Uani 1 1 d . . . H8 H 0.1035 0.459 -0.0917 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0160(2) 0.0185(2) 0.0192(2) -0.00205(18) 0.00499(18) 0.00075(19) Co2 0.0161(2) 0.0221(2) 0.0151(2) -0.00201(18) 0.00311(17) 0.00030(19) Co3 0.0197(2) 0.0214(2) 0.0214(2) -0.00599(19) 0.00437(18) 0.0016(2) C11 0.026(2) 0.0210(18) 0.0281(18) -0.0047(15) 0.0096(15) -0.0016(16) O11 0.0165(14) 0.0440(17) 0.0532(17) -0.0103(13) 0.0091(12) -0.0018(13) C12 0.0259(19) 0.0222(18) 0.0278(18) -0.0030(16) 0.0084(15) -0.0014(16) O12 0.0543(19) 0.0249(14) 0.0373(15) 0.0045(12) 0.0139(13) -0.0016(13) C21 0.0233(19) 0.0282(19) 0.0203(16) 0.0001(15) 0.0056(15) -0.0028(16) O21 0.0247(14) 0.0437(17) 0.0369(14) 0.0086(12) 0.0018(12) 0.0095(13) C22 0.028(2) 0.035(2) 0.0274(19) -0.0048(16) 0.0100(16) -0.0016(17) O22 0.0552(19) 0.064(2) 0.0329(15) -0.0057(14) 0.0264(14) -0.0034(16) C31 0.029(2) 0.027(2) 0.0277(18) -0.0075(15) 0.0104(16) -0.0036(17) O31 0.0264(15) 0.0496(18) 0.0383(15) -0.0072(13) -0.0036(12) -0.0024(14) C32 0.035(2) 0.032(2) 0.0245(18) -0.0086(16) 0.0046(16) 0.0015(18) O32 0.065(2) 0.0267(15) 0.0456(16) 0.0016(13) 0.0178(15) 0.0060(15) C33 0.034(2) 0.041(2) 0.0298(19) -0.0148(17) 0.0087(17) 0.0009(18) O33 0.060(2) 0.088(3) 0.061(2) -0.0265(19) 0.0361(18) 0.010(2) P1 0.0198(4) 0.0184(4) 0.0165(4) -0.0011(3) 0.0054(3) 0.0019(4) C111 0.033(2) 0.0161(16) 0.0135(15) -0.0017(13) 0.0044(14) 0.0005(15) C112 0.038(2) 0.031(2) 0.0244(18) 0.0019(15) 0.0129(16) 0.0046(18) C113 0.042(2) 0.033(2) 0.0274(19) 0.0083(16) 0.0076(17) 0.0077(18) C114 0.062(3) 0.026(2) 0.0202(17) 0.0024(15) 0.0117(18) -0.004(2) C115 0.053(3) 0.037(2) 0.031(2) 0.0019(17) 0.0246(19) 0.000(2) C116 0.036(2) 0.033(2) 0.0301(19) 0.0039(17) 0.0156(16) 0.0041(18) C121 0.0269(19) 0.0180(17) 0.0248(17) 0.0015(14) 0.0121(15) 0.0020(15) C122 0.0208(18) 0.0256(19) 0.0309(18) 0.0006(15) 0.0101(15) 0.0004(15) C123 0.024(2) 0.026(2) 0.050(2) 0.0068(18) 0.0149(18) 0.0055(17) C124 0.048(3) 0.025(2) 0.050(2) 0.0036(18) 0.032(2) 0.0109(19) C125 0.069(3) 0.027(2) 0.031(2) -0.0021(17) 0.024(2) 0.010(2) C126 0.048(2) 0.028(2) 0.0234(18) 0.0003(15) 0.0125(17) 0.0106(18) C0 0.0193(17) 0.0214(17) 0.0150(15) -0.0015(13) 0.0023(13) 0.0005(14) P2 0.0168(4) 0.0229(5) 0.0158(4) -0.0001(3) 0.0031(3) -0.0004(4) C211 0.0191(17) 0.034(2) 0.0156(15) 0.0014(14) 0.0045(13) -0.0059(16) C212 0.0225(19) 0.039(2) 0.0286(18) 0.0028(16) 0.0099(15) -0.0027(17) C213 0.026(2) 0.049(3) 0.038(2) 0.0066(19) 0.0124(17) 0.0016(19) C214 0.020(2) 0.068(3) 0.035(2) 0.009(2) 0.0104(17) -0.004(2) C215 0.033(2) 0.050(3) 0.032(2) -0.0017(18) 0.0095(17) -0.022(2) C216 0.031(2) 0.037(2) 0.0265(18) 0.0013(16) 0.0098(16) -0.0078(18) C221 0.0193(18) 0.0233(18) 0.0214(16) 0.0017(14) 0.0016(14) -0.0039(15) C222 0.036(2) 0.0263(19) 0.0198(16) -0.0017(14) 0.0049(15) -0.0018(17) C223 0.041(2) 0.032(2) 0.0234(18) 0.0068(16) 0.0010(17) 0.0012(18) C224 0.035(2) 0.025(2) 0.039(2) 0.0068(17) 0.0101(18) 0.0034(18) C225 0.037(2) 0.025(2) 0.0305(19) -0.0037(15) 0.0110(17) -0.0017(17) C226 0.028(2) 0.0260(19) 0.0223(17) 0.0001(15) 0.0056(15) -0.0027(16) C1 0.0180(17) 0.0223(18) 0.0175(15) -0.0028(13) 0.0062(13) 0.0002(14) C2 0.0222(18) 0.0219(18) 0.0206(16) -0.0044(14) 0.0088(14) 0.0001(15) C3 0.0237(19) 0.0255(19) 0.0254(17) -0.0052(14) 0.0057(15) 0.0032(16) C4 0.0197(19) 0.031(2) 0.0280(18) -0.0035(15) 0.0029(15) 0.0065(16) C5 0.024(2) 0.032(2) 0.035(2) -0.0025(17) 0.0051(16) 0.0049(17) C6 0.0193(18) 0.032(2) 0.0310(19) -0.0031(16) 0.0008(15) 0.0043(16) C7 0.035(3) 0.104(4) 0.030(2) -0.001(2) 0.0008(19) 0.029(3) C8 0.039(3) 0.102(4) 0.041(2) 0.004(3) 0.011(2) 0.034(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.787(4) . ? Co1 C11 1.812(4) . ? Co1 C1 1.898(3) . ? Co1 P1 2.2029(9) . ? Co1 Co2 2.4756(6) . ? Co1 Co3 2.4985(6) . ? Co2 C22 1.778(4) . ? Co2 C21 1.790(4) . ? Co2 C1 1.896(3) . ? Co2 P2 2.1939(9) . ? Co2 Co3 2.4799(6) . ? Co3 C33 1.783(4) . ? Co3 C32 1.793(4) . ? Co3 C31 1.817(4) . ? Co3 C1 1.925(3) . ? C11 O11 1.136(4) . ? C12 O12 1.136(4) . ? C21 O21 1.143(4) . ? C22 O22 1.131(4) . ? C31 O31 1.137(4) . ? C32 O32 1.140(4) . ? C33 O33 1.139(4) . ? P1 C121 1.825(3) . ? P1 C111 1.826(3) . ? P1 C0 1.838(3) . ? C111 C112 1.384(5) . ? C111 C116 1.391(5) . ? C112 C113 1.389(5) . ? C112 H112 0.95 . ? C113 C114 1.375(5) . ? C113 H113 0.95 . ? C114 C115 1.367(6) . ? C114 H114 0.95 . ? C115 C116 1.379(5) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.386(5) . ? C121 C126 1.396(5) . ? C122 C123 1.392(5) . ? C122 H122 0.95 . ? C123 C124 1.374(5) . ? C123 H123 0.95 . ? C124 C125 1.370(5) . ? C124 H124 0.95 . ? C125 C126 1.381(5) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C0 P2 1.836(3) . ? C0 H0A 0.99 . ? C0 H0B 0.99 . ? P2 C221 1.826(3) . ? P2 C211 1.837(3) . ? C211 C212 1.382(5) . ? C211 C216 1.388(5) . ? C212 C213 1.385(5) . ? C212 H212 0.95 . ? C213 C214 1.370(6) . ? C213 H213 0.95 . ? C214 C215 1.384(6) . ? C214 H214 0.95 . ? C215 C216 1.386(5) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.383(5) . ? C221 C222 1.399(4) . ? C222 C223 1.376(5) . ? C222 H222 0.95 . ? C223 C224 1.374(5) . ? C223 H223 0.95 . ? C224 C225 1.378(5) . ? C224 H224 0.95 . ? C225 C226 1.378(5) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C1 C2 1.390(4) . ? C2 C3 1.218(5) . ? C3 C4 1.361(5) . ? C4 C5 1.198(5) . ? C5 C6 1.426(5) . ? C6 C7 1.348(5) . ? C6 C8 1.391(5) . ? C7 C8 1.388(6) 3_565 ? C7 H7 0.95 . ? C8 C7 1.388(6) 3_565 ? C8 H8 0.95 . ? 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 C12 Co1 C11 102.51(16) . . ? C12 Co1 C1 96.68(15) . . ? C11 Co1 C1 147.79(14) . . ? C12 Co1 P1 96.01(11) . . ? C11 Co1 P1 104.35(10) . . ? C1 Co1 P1 99.02(10) . . ? C12 Co1 Co2 145.73(12) . . ? C11 Co1 Co2 106.89(11) . . ? C1 Co1 Co2 49.23(9) . . ? P1 Co1 Co2 93.44(3) . . ? C12 Co1 Co3 97.38(11) . . ? C11 Co1 Co3 101.84(10) . . ? C1 Co1 Co3 49.65(9) . . ? P1 Co1 Co3 147.12(3) . . ? Co2 Co1 Co3 59.806(17) . . ? C22 Co2 C21 101.95(16) . . ? C22 Co2 C1 111.86(15) . . ? C21 Co2 C1 139.08(15) . . ? C22 Co2 P2 96.46(12) . . ? C21 Co2 P2 103.00(11) . . ? C1 Co2 P2 95.60(10) . . ? C22 Co2 Co1 156.02(12) . . ? C21 Co2 Co1 91.35(11) . . ? C1 Co2 Co1 49.29(10) . . ? P2 Co2 Co1 99.90(3) . . ? C22 Co2 Co3 96.39(12) . . ? C21 Co2 Co3 105.29(11) . . ? C1 Co2 Co3 50.03(9) . . ? P2 Co2 Co3 145.62(3) . . ? Co1 Co2 Co3 60.556(17) . . ? C33 Co3 C32 95.82(18) . . ? C33 Co3 C31 105.18(16) . . ? C32 Co3 C31 107.16(17) . . ? C33 Co3 C1 99.84(15) . . ? C32 Co3 C1 101.29(14) . . ? C31 Co3 C1 139.51(14) . . ? C33 Co3 Co2 96.15(13) . . ? C32 Co3 Co2 149.57(11) . . ? C31 Co3 Co2 96.51(11) . . ? C1 Co3 Co2 49.02(9) . . ? C33 Co3 Co1 147.82(12) . . ? C32 Co3 Co1 97.23(11) . . ? C31 Co3 Co1 98.84(11) . . ? C1 Co3 Co1 48.71(9) . . ? Co2 Co3 Co1 59.638(17) . . ? O11 C11 Co1 177.1(3) . . ? O12 C12 Co1 176.4(3) . . ? O21 C21 Co2 179.2(3) . . ? O22 C22 Co2 178.2(4) . . ? O31 C31 Co3 178.7(4) . . ? O32 C32 Co3 176.4(4) . . ? O33 C33 Co3 177.2(4) . . ? C121 P1 C111 103.24(15) . . ? C121 P1 C0 101.89(15) . . ? C111 P1 C0 103.86(15) . . ? C121 P1 Co1 121.88(11) . . ? C111 P1 Co1 113.10(11) . . ? C0 P1 Co1 110.92(10) . . ? C112 C111 C116 118.6(3) . . ? C112 C111 P1 120.5(3) . . ? C116 C111 P1 120.4(3) . . ? C111 C112 C113 120.6(3) . . ? C111 C112 H112 119.7 . . ? C113 C112 H112 119.7 . . ? C114 C113 C112 119.7(4) . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.2 . . ? C115 C114 C113 120.3(3) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C114 C115 C116 120.4(4) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 120.5(4) . . ? C115 C116 H116 119.8 . . ? C111 C116 H116 119.8 . . ? C122 C121 C126 119.0(3) . . ? C122 C121 P1 121.5(2) . . ? C126 C121 P1 119.2(3) . . ? C121 C122 C123 120.2(3) . . ? C121 C122 H122 119.9 . . ? C123 C122 H122 119.9 . . ? C124 C123 C122 120.0(3) . . ? C124 C123 H123 120 . . ? C122 C123 H123 120 . . ? C125 C124 C123 120.3(3) . . ? C125 C124 H124 119.9 . . ? C123 C124 H124 119.9 . . ? C124 C125 C126 120.4(4) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 120.1(4) . . ? C125 C126 H126 119.9 . . ? C121 C126 H126 119.9 . . ? P2 C0 P1 110.01(16) . . ? P2 C0 H0A 109.7 . . ? P1 C0 H0A 109.7 . . ? P2 C0 H0B 109.7 . . ? P1 C0 H0B 109.7 . . ? H0A C0 H0B 108.2 . . ? C221 P2 C0 107.30(15) . . ? C221 P2 C211 103.73(16) . . ? C0 P2 C211 101.04(14) . . ? C221 P2 Co2 115.62(11) . . ? C0 P2 Co2 109.39(11) . . ? C211 P2 Co2 118.35(11) . . ? C212 C211 C216 119.0(3) . . ? C212 C211 P2 119.5(3) . . ? C216 C211 P2 121.2(3) . . ? C211 C212 C213 121.0(4) . . ? C211 C212 H212 119.5 . . ? C213 C212 H212 119.5 . . ? C214 C213 C212 119.8(4) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C213 C214 C215 119.8(4) . . ? C213 C214 H214 120.1 . . ? C215 C214 H214 120.1 . . ? C214 C215 C216 120.6(4) . . ? C214 C215 H215 119.7 . . ? C216 C215 H215 119.7 . . ? C215 C216 C211 119.7(4) . . ? C215 C216 H216 120.2 . . ? C211 C216 H216 120.2 . . ? C226 C221 C222 118.8(3) . . ? C226 C221 P2 124.2(2) . . ? C222 C221 P2 117.0(3) . . ? C223 C222 C221 120.1(3) . . ? C223 C222 H222 119.9 . . ? C221 C222 H222 119.9 . . ? C224 C223 C222 120.5(3) . . ? C224 C223 H223 119.8 . . ? C222 C223 H223 119.8 . . ? C223 C224 C225 119.8(3) . . ? C223 C224 H224 120.1 . . ? C225 C224 H224 120.1 . . ? C226 C225 C224 120.2(3) . . ? C226 C225 H225 119.9 . . ? C224 C225 H225 119.9 . . ? C225 C226 C221 120.6(3) . . ? C225 C226 H226 119.7 . . ? C221 C226 H226 119.7 . . ? C2 C1 Co2 135.4(3) . . ? C2 C1 Co1 129.9(2) . . ? Co2 C1 Co1 81.48(13) . . ? C2 C1 Co3 128.0(2) . . ? Co2 C1 Co3 80.94(12) . . ? Co1 C1 Co3 81.64(13) . . ? C3 C2 C1 176.1(4) . . ? C2 C3 C4 175.4(4) . . ? C5 C4 C3 179.1(4) . . ? C4 C5 C6 177.6(4) . . ? C7 C6 C8 118.8(3) . . ? C7 C6 C5 120.1(3) . . ? C8 C6 C5 121.1(3) . . ? C6 C7 C8 121.4(4) . 3_565 ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 3_565 . ? C7 C8 C6 119.8(4) 3_565 . ? C7 C8 H8 120.1 3_565 . ? C6 C8 H8 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Co1 Co2 C22 -36.5(3) . . . . ? C11 Co1 Co2 C22 111.5(3) . . . . ? C1 Co1 Co2 C22 -43.5(3) . . . . ? P1 Co1 Co2 C22 -142.4(3) . . . . ? Co3 Co1 Co2 C22 17.4(3) . . . . ? C12 Co1 Co2 C21 -160.7(2) . . . . ? C11 Co1 Co2 C21 -12.74(15) . . . . ? C1 Co1 Co2 C21 -167.68(16) . . . . ? P1 Co1 Co2 C21 93.38(11) . . . . ? Co3 Co1 Co2 C21 -106.84(11) . . . . ? C12 Co1 Co2 C1 7.0(2) . . . . ? C11 Co1 Co2 C1 154.93(16) . . . . ? P1 Co1 Co2 C1 -98.94(12) . . . . ? Co3 Co1 Co2 C1 60.83(12) . . . . ? C12 Co1 Co2 P2 95.87(19) . . . . ? C11 Co1 Co2 P2 -116.19(11) . . . . ? C1 Co1 Co2 P2 88.88(12) . . . . ? P1 Co1 Co2 P2 -10.06(4) . . . . ? Co3 Co1 Co2 P2 149.71(3) . . . . ? C12 Co1 Co2 Co3 -53.84(19) . . . . ? C11 Co1 Co2 Co3 94.10(11) . . . . ? C1 Co1 Co2 Co3 -60.83(12) . . . . ? P1 Co1 Co2 Co3 -159.77(3) . . . . ? C22 Co2 Co3 C33 -15.55(17) . . . . ? C21 Co2 Co3 C33 -119.83(16) . . . . ? C1 Co2 Co3 C33 97.71(17) . . . . ? P2 Co2 Co3 C33 95.81(13) . . . . ? Co1 Co2 Co3 C33 157.44(12) . . . . ? C22 Co2 Co3 C32 -128.2(3) . . . . ? C21 Co2 Co3 C32 127.6(3) . . . . ? C1 Co2 Co3 C32 -14.9(3) . . . . ? P2 Co2 Co3 C32 -16.8(3) . . . . ? Co1 Co2 Co3 C32 44.8(2) . . . . ? C22 Co2 Co3 C31 90.55(16) . . . . ? C21 Co2 Co3 C31 -13.72(15) . . . . ? C1 Co2 Co3 C31 -156.18(16) . . . . ? P2 Co2 Co3 C31 -158.08(12) . . . . ? Co1 Co2 Co3 C31 -96.46(11) . . . . ? C22 Co2 Co3 C1 -113.26(17) . . . . ? C21 Co2 Co3 C1 142.46(16) . . . . ? P2 Co2 Co3 C1 -1.90(13) . . . . ? Co1 Co2 Co3 C1 59.73(12) . . . . ? C22 Co2 Co3 Co1 -172.99(12) . . . . ? C21 Co2 Co3 Co1 82.74(11) . . . . ? C1 Co2 Co3 Co1 -59.73(12) . . . . ? P2 Co2 Co3 Co1 -61.63(6) . . . . ? C12 Co1 Co3 C33 107.0(3) . . . . ? C11 Co1 Co3 C33 -148.5(3) . . . . ? C1 Co1 Co3 C33 14.5(3) . . . . ? P1 Co1 Co3 C33 -6.3(3) . . . . ? Co2 Co1 Co3 C33 -45.7(2) . . . . ? C12 Co1 Co3 C32 -6.18(17) . . . . ? C11 Co1 Co3 C32 98.31(17) . . . . ? C1 Co1 Co3 C32 -98.70(18) . . . . ? P1 Co1 Co3 C32 -119.44(13) . . . . ? Co2 Co1 Co3 C32 -158.90(13) . . . . ? C12 Co1 Co3 C31 -114.89(16) . . . . ? C11 Co1 Co3 C31 -10.39(16) . . . . ? C1 Co1 Co3 C31 152.59(17) . . . . ? P1 Co1 Co3 C31 131.86(13) . . . . ? Co2 Co1 Co3 C31 92.39(12) . . . . ? C12 Co1 Co3 C1 92.52(17) . . . . ? C11 Co1 Co3 C1 -162.99(17) . . . . ? P1 Co1 Co3 C1 -20.73(13) . . . . ? Co2 Co1 Co3 C1 -60.20(12) . . . . ? C12 Co1 Co3 Co2 152.72(11) . . . . ? C11 Co1 Co3 Co2 -102.79(11) . . . . ? C1 Co1 Co3 Co2 60.20(12) . . . . ? P1 Co1 Co3 Co2 39.47(6) . . . . ? C12 Co1 C11 O11 29(6) . . . . ? C1 Co1 C11 O11 -96(6) . . . . ? P1 Co1 C11 O11 129(6) . . . . ? Co2 Co1 C11 O11 -133(6) . . . . ? Co3 Co1 C11 O11 -71(6) . . . . ? C11 Co1 C12 O12 -161(5) . . . . ? C1 Co1 C12 O12 -7(5) . . . . ? P1 Co1 C12 O12 93(5) . . . . ? Co2 Co1 C12 O12 -12(5) . . . . ? Co3 Co1 C12 O12 -57(5) . . . . ? C22 Co2 C21 O21 15E1(10) . . . . ? C1 Co2 C21 O21 -6E1(2) . . . . ? P2 Co2 C21 O21 6E1(2) . . . . ? Co1 Co2 C21 O21 -5E1(2) . . . . ? Co3 Co2 C21 O21 -11E1(2) . . . . ? C21 Co2 C22 O22 -4(12) . . . . ? C1 Co2 C22 O22 -160(12) . . . . ? P2 Co2 C22 O22 101(12) . . . . ? Co1 Co2 C22 O22 -126(12) . . . . ? Co3 Co2 C22 O22 -111(12) . . . . ? C33 Co3 C31 O31 56(17) . . . . ? C32 Co3 C31 O31 157(17) . . . . ? C1 Co3 C31 O31 -70(17) . . . . ? Co2 Co3 C31 O31 -42(17) . . . . ? Co1 Co3 C31 O31 -102(17) . . . . ? C33 Co3 C32 O32 -42(5) . . . . ? C31 Co3 C32 O32 -150(5) . . . . ? C1 Co3 C32 O32 59(5) . . . . ? Co2 Co3 C32 O32 71(5) . . . . ? Co1 Co3 C32 O32 109(5) . . . . ? C32 Co3 C33 O33 67(8) . . . . ? C31 Co3 C33 O33 18E1(10) . . . . ? C1 Co3 C33 O33 -36(8) . . . . ? Co2 Co3 C33 O33 -85(8) . . . . ? Co1 Co3 C33 O33 -47(8) . . . . ? C12 Co1 P1 C121 124.59(17) . . . . ? C11 Co1 P1 C121 20.01(17) . . . . ? C1 Co1 P1 C121 -137.64(16) . . . . ? Co2 Co1 P1 C121 -88.39(13) . . . . ? Co3 Co1 P1 C121 -121.78(13) . . . . ? C12 Co1 P1 C111 0.64(17) . . . . ? C11 Co1 P1 C111 -103.93(17) . . . . ? C1 Co1 P1 C111 98.41(16) . . . . ? Co2 Co1 P1 C111 147.66(13) . . . . ? Co3 Co1 P1 C111 114.27(13) . . . . ? C12 Co1 P1 C0 -115.58(16) . . . . ? C11 Co1 P1 C0 139.84(15) . . . . ? C1 Co1 P1 C0 -17.81(15) . . . . ? Co2 Co1 P1 C0 31.44(11) . . . . ? Co3 Co1 P1 C0 -1.96(13) . . . . ? C121 P1 C111 C112 147.4(3) . . . . ? C0 P1 C111 C112 41.4(3) . . . . ? Co1 P1 C111 C112 -79.0(3) . . . . ? C121 P1 C111 C116 -40.3(3) . . . . ? C0 P1 C111 C116 -146.4(3) . . . . ? Co1 P1 C111 C116 93.3(3) . . . . ? C116 C111 C112 C113 2.0(5) . . . . ? P1 C111 C112 C113 174.4(3) . . . . ? C111 C112 C113 C114 -0.8(6) . . . . ? C112 C113 C114 C115 -0.4(6) . . . . ? C113 C114 C115 C116 0.4(6) . . . . ? C114 C115 C116 C111 0.8(6) . . . . ? C112 C111 C116 C115 -2.0(5) . . . . ? P1 C111 C116 C115 -174.4(3) . . . . ? C111 P1 C121 C122 145.2(3) . . . . ? C0 P1 C121 C122 -107.3(3) . . . . ? Co1 P1 C121 C122 16.8(3) . . . . ? C111 P1 C121 C126 -41.5(3) . . . . ? C0 P1 C121 C126 66.0(3) . . . . ? Co1 P1 C121 C126 -169.9(2) . . . . ? C126 C121 C122 C123 1.2(5) . . . . ? P1 C121 C122 C123 174.5(3) . . . . ? C121 C122 C123 C124 -0.6(5) . . . . ? C122 C123 C124 C125 -0.1(6) . . . . ? C123 C124 C125 C126 0.1(6) . . . . ? C124 C125 C126 C121 0.5(6) . . . . ? C122 C121 C126 C125 -1.1(5) . . . . ? P1 C121 C126 C125 -174.6(3) . . . . ? C121 P1 C0 P2 85.71(18) . . . . ? C111 P1 C0 P2 -167.25(16) . . . . ? Co1 P1 C0 P2 -45.45(18) . . . . ? P1 C0 P2 C221 -90.77(19) . . . . ? P1 C0 P2 C211 160.93(17) . . . . ? P1 C0 P2 Co2 35.36(18) . . . . ? C22 Co2 P2 C221 -88.62(17) . . . . ? C21 Co2 P2 C221 15.26(17) . . . . ? C1 Co2 P2 C221 158.57(15) . . . . ? Co1 Co2 P2 C221 108.98(12) . . . . ? Co3 Co2 P2 C221 160.04(12) . . . . ? C22 Co2 P2 C0 150.15(17) . . . . ? C21 Co2 P2 C0 -105.96(16) . . . . ? C1 Co2 P2 C0 37.35(15) . . . . ? Co1 Co2 P2 C0 -12.25(12) . . . . ? Co3 Co2 P2 C0 38.81(13) . . . . ? C22 Co2 P2 C211 35.28(17) . . . . ? C21 Co2 P2 C211 139.17(16) . . . . ? C1 Co2 P2 C211 -77.52(15) . . . . ? Co1 Co2 P2 C211 -127.12(12) . . . . ? Co3 Co2 P2 C211 -76.06(13) . . . . ? C221 P2 C211 C212 155.4(3) . . . . ? C0 P2 C211 C212 -93.5(3) . . . . ? Co2 P2 C211 C212 25.8(3) . . . . ? C221 P2 C211 C216 -30.3(3) . . . . ? # Attachment '5.br1493.cif' data_br1493 _database_code_depnum_ccdc_archive 'CCDC 766034' #TrackingRef '5.br1493.cif' _audit_creation_date 2009-10-21T11:34:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C69 H44 Co6 O15 P4' _chemical_formula_moiety 'C69 H44 Co6 O15 P4' _chemical_formula_weight 1590.5 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9662(6) _cell_length_b 14.5377(7) _cell_length_c 19.1896(9) _cell_angle_alpha 111.300(4) _cell_angle_beta 98.819(4) _cell_angle_gamma 100.393(4) _cell_volume 3218.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13727 _cell_measurement_theta_min 3.569 _cell_measurement_theta_max 36.4422 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.0269 0 -1 0 0.1114 1 -1 1 0.181 -1 1 -1 0.1146 -1 1 1 0.0352 1 -1 -1 0.0551 -4 -19 6 0.1603 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.678 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 0.893 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0515683679 _diffrn_orient_matrix_ub_12 -0.0100918443 _diffrn_orient_matrix_ub_13 0.000800952 _diffrn_orient_matrix_ub_21 -0.0230204844 _diffrn_orient_matrix_ub_22 -0.0467767373 _diffrn_orient_matrix_ub_23 -0.0325812936 _diffrn_orient_matrix_ub_31 0.0094436778 _diffrn_orient_matrix_ub_32 0.0253330401 _diffrn_orient_matrix_ub_33 -0.0245870114 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_unetI/netI 0.129 _diffrn_reflns_number 51534 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 35 _diffrn_reflns_theta_full 35 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 28302 _reflns_number_gt 15333 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0228P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 28302 _refine_ls_number_parameters 847 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.804 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.695 _refine_diff_density_min -1.473 _refine_diff_density_rms 0.105 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.191977(19) 0.200844(19) 0.043953(14) 0.01241(5) Uani 1 1 d . . . Co2 Co 0.327148(19) 0.340561(19) 0.038508(14) 0.01131(5) Uani 1 1 d . . . Co3 Co 0.13311(2) 0.31258(2) -0.017847(15) 0.01484(6) Uani 1 1 d . . . Co4 Co 0.073550(19) 0.674287(19) 0.314583(14) 0.01166(5) Uani 1 1 d . . . Co5 Co 0.102702(19) 0.635081(19) 0.430815(14) 0.01072(5) Uani 1 1 d . . . Co6 Co -0.02950(2) 0.51146(2) 0.310627(15) 0.01727(6) Uani 1 1 d . . . C11 C 0.20584(16) 0.09642(16) -0.03874(12) 0.0191(4) Uani 1 1 d . . . O11 O 0.21157(13) 0.03285(11) -0.09338(9) 0.0283(4) Uani 1 1 d . . . C12 C 0.06232(16) 0.14670(16) 0.05339(12) 0.0216(4) Uani 1 1 d . . . O12 O -0.02081(12) 0.11290(13) 0.05898(10) 0.0376(4) Uani 1 1 d . . . C21 C 0.36663(15) 0.26434(15) -0.04514(11) 0.0161(4) Uani 1 1 d . . . O21 O 0.38745(11) 0.21684(12) -0.10085(8) 0.0251(3) Uani 1 1 d . . . C22 C 0.37438(15) 0.46406(15) 0.03895(11) 0.0171(4) Uani 1 1 d . . . O22 O 0.40435(12) 0.54115(11) 0.03648(9) 0.0262(3) Uani 1 1 d . . . C31 C 0.13098(15) 0.23630(16) -0.11692(12) 0.0202(4) Uani 1 1 d . . . O31 O 0.12980(12) 0.18623(12) -0.17857(9) 0.0311(4) Uani 1 1 d . . . C32 C -0.00731(17) 0.27741(18) -0.01847(12) 0.0248(5) Uani 1 1 d . . . O32 O -0.09618(12) 0.25403(15) -0.01948(10) 0.0415(5) Uani 1 1 d . . . C33 C 0.13978(17) 0.44137(18) -0.01104(12) 0.0247(5) Uani 1 1 d . . . O33 O 0.14377(14) 0.52268(13) -0.00403(10) 0.0390(4) Uani 1 1 d . . . C41 C -0.02570(15) 0.74668(16) 0.33102(11) 0.0177(4) Uani 1 1 d . . . O41 O -0.09035(11) 0.79070(12) 0.34066(8) 0.0255(3) Uani 1 1 d . . . C42 C 0.06838(15) 0.64283(15) 0.21444(11) 0.0164(4) Uani 1 1 d . . . O42 O 0.06644(12) 0.62388(11) 0.15096(8) 0.0260(3) Uani 1 1 d . . . C51 C 0.01703(15) 0.70588(15) 0.48114(11) 0.0161(4) Uani 1 1 d . . . O51 O -0.04047(12) 0.75008(12) 0.50974(9) 0.0271(3) Uani 1 1 d . . . C52 C 0.11395(15) 0.53991(15) 0.46672(11) 0.0169(4) Uani 1 1 d . . . O52 O 0.12063(12) 0.47522(11) 0.48612(8) 0.0264(4) Uani 1 1 d . . . C61 C -0.14572(18) 0.54863(17) 0.34161(13) 0.0273(5) Uani 1 1 d . . . O61 O -0.21862(13) 0.57234(14) 0.36420(11) 0.0412(5) Uani 1 1 d . . . C62 C -0.0704(2) 0.45882(19) 0.20776(14) 0.0383(7) Uani 1 1 d . . . O62 O -0.09605(19) 0.42552(16) 0.14223(11) 0.0808(9) Uani 1 1 d . . . C63 C -0.04405(16) 0.39348(17) 0.32291(12) 0.0239(5) Uani 1 1 d . . . O63 O -0.05830(13) 0.31857(12) 0.33016(10) 0.0381(4) Uani 1 1 d . . . P1 P 0.28582(4) 0.19714(4) 0.14876(3) 0.01141(9) Uani 1 1 d . . . C111 C 0.20760(14) 0.17683(14) 0.21580(11) 0.0140(4) Uani 1 1 d . . . C112 C 0.21045(14) 0.25194(15) 0.28657(11) 0.0161(4) Uani 1 1 d . . . H112 H 0.2528 0.3196 0.3015 0.019 Uiso 1 1 calc R . . C113 C 0.15200(16) 0.22899(17) 0.33567(12) 0.0231(4) Uani 1 1 d . . . H113 H 0.1552 0.2805 0.3843 0.028 Uiso 1 1 calc R . . C114 C 0.08898(16) 0.13056(18) 0.31349(13) 0.0251(5) Uani 1 1 d . . . H114 H 0.0493 0.1147 0.3472 0.03 Uiso 1 1 calc R . . C115 C 0.08366(17) 0.05589(17) 0.24300(13) 0.0255(5) Uani 1 1 d . . . H115 H 0.0396 -0.0111 0.228 0.031 Uiso 1 1 calc R . . C116 C 0.14247(16) 0.07772(15) 0.19338(12) 0.0208(4) Uani 1 1 d . . . H116 H 0.1385 0.0259 0.1447 0.025 Uiso 1 1 calc R . . C121 C 0.37279(14) 0.11113(14) 0.14867(11) 0.0135(4) Uani 1 1 d . . . C122 C 0.42559(15) 0.11691(15) 0.22032(11) 0.0172(4) Uani 1 1 d . . . H122 H 0.4073 0.157 0.2658 0.021 Uiso 1 1 calc R . . C123 C 0.50365(16) 0.06503(15) 0.22530(12) 0.0203(4) Uani 1 1 d . . . H123 H 0.5403 0.0709 0.2741 0.024 Uiso 1 1 calc R . . C124 C 0.52871(16) 0.00385(15) 0.15833(12) 0.0198(4) Uani 1 1 d . . . H124 H 0.5833 -0.0311 0.1617 0.024 Uiso 1 1 calc R . . C125 C 0.47427(15) -0.00585(15) 0.08741(12) 0.0200(4) Uani 1 1 d . . . H125 H 0.4894 -0.0495 0.0418 0.024 Uiso 1 1 calc R . . C126 C 0.39683(15) 0.04851(14) 0.08258(11) 0.0162(4) Uani 1 1 d . . . H126 H 0.3604 0.0425 0.0336 0.019 Uiso 1 1 calc R . . C10 C 0.38432(13) 0.32072(14) 0.20524(10) 0.0112(3) Uani 1 1 d . . . H10A H 0.3473 0.3721 0.2322 0.013 Uiso 1 1 calc R . . H10B H 0.4386 0.3143 0.2443 0.013 Uiso 1 1 calc R . . P2 P 0.45062(4) 0.36122(4) 0.13982(3) 0.01135(9) Uani 1 1 d . . . C211 C 0.52810(14) 0.49328(14) 0.20067(10) 0.0130(4) Uani 1 1 d . . . C212 C 0.60955(15) 0.53775(15) 0.17316(11) 0.0197(4) Uani 1 1 d . . . H212 H 0.6228 0.4995 0.125 0.024 Uiso 1 1 calc R . . C213 C 0.67010(16) 0.63708(16) 0.21626(12) 0.0224(5) Uani 1 1 d . . . H213 H 0.7244 0.6669 0.1972 0.027 Uiso 1 1 calc R . . C214 C 0.65280(15) 0.69327(15) 0.28645(12) 0.0193(4) Uani 1 1 d . . . H214 H 0.6956 0.7612 0.3159 0.023 Uiso 1 1 calc R . . C215 C 0.57323(15) 0.65084(15) 0.31396(11) 0.0181(4) Uani 1 1 d . . . H215 H 0.5614 0.6897 0.3625 0.022 Uiso 1 1 calc R . . C216 C 0.50975(14) 0.55093(14) 0.27104(11) 0.0144(4) Uani 1 1 d . . . H216 H 0.4542 0.5225 0.29 0.017 Uiso 1 1 calc R . . C221 C 0.56045(14) 0.29855(14) 0.12750(11) 0.0151(4) Uani 1 1 d . . . C222 C 0.61248(15) 0.27288(15) 0.18450(12) 0.0192(4) Uani 1 1 d . . . H222 H 0.588 0.2852 0.2305 0.023 Uiso 1 1 calc R . . C223 C 0.69863(15) 0.22995(16) 0.17526(13) 0.0244(5) Uani 1 1 d . . . H223 H 0.7318 0.2118 0.2143 0.029 Uiso 1 1 calc R . . C224 C 0.73710(16) 0.21318(16) 0.10955(13) 0.0258(5) Uani 1 1 d . . . H224 H 0.796 0.1829 0.1032 0.031 Uiso 1 1 calc R . . C225 C 0.68940(16) 0.24062(18) 0.05316(12) 0.0273(5) Uani 1 1 d . . . H225 H 0.7167 0.2311 0.0085 0.033 Uiso 1 1 calc R . . C226 C 0.60122(15) 0.28232(16) 0.06199(11) 0.0205(4) Uani 1 1 d . . . H226 H 0.5681 0.3001 0.0227 0.025 Uiso 1 1 calc R . . C1 C 0.20767(14) 0.34456(14) 0.08543(10) 0.0134(4) Uani 1 1 d . . . C2 C 0.19438(14) 0.40888(15) 0.15634(11) 0.0151(4) Uani 1 1 d . . . C3 C 0.18951(15) 0.46178(14) 0.22149(11) 0.0147(4) Uani 1 1 d . . . C4 C 0.20532(15) 0.51648(14) 0.30328(11) 0.0153(4) Uani 1 1 d . . . O4 O 0.28926(11) 0.51886(11) 0.34656(8) 0.0219(3) Uani 1 1 d . . . C5 C 0.12434(15) 0.56787(14) 0.33188(10) 0.0136(4) Uani 1 1 d . . . P4 P 0.22417(4) 0.79422(4) 0.35607(3) 0.01075(9) Uani 1 1 d . . . C411 C 0.28813(14) 0.79893(14) 0.27890(10) 0.0127(4) Uani 1 1 d . . . C412 C 0.35789(15) 0.73885(15) 0.25558(11) 0.0174(4) Uani 1 1 d . . . H412 H 0.3777 0.6998 0.2833 0.021 Uiso 1 1 calc R . . C413 C 0.39982(16) 0.73443(17) 0.19209(11) 0.0223(4) Uani 1 1 d . . . H413 H 0.4487 0.6937 0.1771 0.027 Uiso 1 1 calc R . . C414 C 0.36922(16) 0.78998(17) 0.15141(12) 0.0235(5) Uani 1 1 d . . . H414 H 0.3972 0.7876 0.108 0.028 Uiso 1 1 calc R . . C415 C 0.29819(17) 0.84909(16) 0.17315(12) 0.0237(5) Uani 1 1 d . . . H415 H 0.2775 0.8869 0.1445 0.028 Uiso 1 1 calc R . . C416 C 0.25687(16) 0.85374(15) 0.23632(11) 0.0186(4) Uani 1 1 d . . . H416 H 0.2074 0.894 0.2507 0.022 Uiso 1 1 calc R . . C421 C 0.22579(14) 0.92671(14) 0.41165(10) 0.0129(4) Uani 1 1 d . . . C422 C 0.15189(15) 0.94833(15) 0.45666(11) 0.0171(4) Uani 1 1 d . . . H422 H 0.0984 0.8938 0.4561 0.021 Uiso 1 1 calc R . . C423 C 0.15497(16) 1.04879(16) 0.50265(12) 0.0243(5) Uani 1 1 d . . . H423 H 0.105 1.0625 0.5341 0.029 Uiso 1 1 calc R . . C424 C 0.23118(18) 1.12838(16) 0.50224(12) 0.0272(5) Uani 1 1 d . . . H424 H 0.2326 1.197 0.5324 0.033 Uiso 1 1 calc R . . C425 C 0.30506(18) 1.10790(16) 0.45802(13) 0.0268(5) Uani 1 1 d . . . H425 H 0.3575 1.1627 0.458 0.032 Uiso 1 1 calc R . . C426 C 0.30363(16) 1.00829(15) 0.41360(11) 0.0199(4) Uani 1 1 d . . . H426 H 0.356 0.9952 0.3842 0.024 Uiso 1 1 calc R . . C20 C 0.32710(14) 0.76930(14) 0.41897(10) 0.0123(3) Uani 1 1 d . . . H20A H 0.3546 0.7124 0.3879 0.015 Uiso 1 1 calc R . . H20B H 0.3885 0.8307 0.4457 0.015 Uiso 1 1 calc R . . P5 P 0.26667(4) 0.73610(4) 0.48980(3) 0.01111(9) Uani 1 1 d . . . C511 C 0.36669(14) 0.68347(14) 0.53051(10) 0.0136(4) Uani 1 1 d . . . C512 C 0.46418(15) 0.68029(15) 0.50918(11) 0.0175(4) Uani 1 1 d . . . H512 H 0.4812 0.7075 0.473 0.021 Uiso 1 1 calc R . . C513 C 0.53715(15) 0.63775(15) 0.54024(11) 0.0196(4) Uani 1 1 d . . . H513 H 0.6043 0.6376 0.5262 0.024 Uiso 1 1 calc R . . C514 C 0.51180(16) 0.59564(15) 0.59154(11) 0.0199(4) Uani 1 1 d . . . H514 H 0.5606 0.5651 0.6119 0.024 Uiso 1 1 calc R . . C515 C 0.41522(16) 0.59834(15) 0.61298(11) 0.0199(4) Uani 1 1 d . . . H515 H 0.3977 0.5691 0.6479 0.024 Uiso 1 1 calc R . . C516 C 0.34310(15) 0.64344(15) 0.58398(11) 0.0174(4) Uani 1 1 d . . . H516 H 0.278 0.647 0.6005 0.021 Uiso 1 1 calc R . . C521 C 0.28273(14) 0.85802(14) 0.57104(10) 0.0141(4) Uani 1 1 d . . . C522 C 0.21664(16) 0.86226(16) 0.62246(11) 0.0195(4) Uani 1 1 d . . . H522 H 0.1638 0.8025 0.6144 0.023 Uiso 1 1 calc R . . C523 C 0.22685(17) 0.95241(17) 0.68526(12) 0.0241(5) Uani 1 1 d . . . H523 H 0.1816 0.9538 0.7199 0.029 Uiso 1 1 calc R . . C524 C 0.30273(18) 1.04016(16) 0.69742(12) 0.0256(5) Uani 1 1 d . . . H524 H 0.3086 1.1023 0.7396 0.031 Uiso 1 1 calc R . . C525 C 0.36990(18) 1.03663(16) 0.64769(12) 0.0247(5) Uani 1 1 d . . . H525 H 0.4229 1.0965 0.6563 0.03 Uiso 1 1 calc R . . C526 C 0.36070(16) 0.94661(15) 0.58536(11) 0.0189(4) Uani 1 1 d . . . H526 H 0.408 0.9452 0.552 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01146(12) 0.01274(12) 0.01278(12) 0.00540(10) 0.00271(9) 0.00206(10) Co2 0.01269(12) 0.01184(12) 0.00934(11) 0.00411(10) 0.00368(9) 0.00243(10) Co3 0.01421(12) 0.01920(14) 0.01352(13) 0.00829(11) 0.00347(10) 0.00629(11) Co4 0.01334(12) 0.01106(12) 0.01035(12) 0.00482(10) 0.00240(9) 0.00185(10) Co5 0.01148(12) 0.01155(12) 0.00992(11) 0.00478(10) 0.00376(9) 0.00280(10) Co6 0.01761(13) 0.01568(14) 0.01500(13) 0.00748(11) -0.00071(10) -0.00303(11) C11 0.0196(10) 0.0172(10) 0.0190(10) 0.0089(9) 0.0016(8) 0.0002(8) O11 0.0405(9) 0.0182(8) 0.0205(8) 0.0013(7) 0.0080(7) 0.0073(7) C12 0.0195(10) 0.0226(11) 0.0243(11) 0.0120(9) 0.0034(8) 0.0054(9) O12 0.0190(8) 0.0454(11) 0.0582(12) 0.0329(10) 0.0113(8) 0.0040(8) C21 0.0138(9) 0.0177(10) 0.0140(9) 0.0059(8) 0.0014(7) 0.0002(8) O21 0.0238(8) 0.0279(9) 0.0182(8) 0.0018(7) 0.0076(6) 0.0078(7) C22 0.0202(10) 0.0214(10) 0.0103(9) 0.0057(8) 0.0055(7) 0.0066(8) O22 0.0357(9) 0.0182(8) 0.0271(8) 0.0117(7) 0.0105(7) 0.0041(7) C31 0.0175(10) 0.0244(11) 0.0191(10) 0.0121(9) 0.0027(8) 0.0008(8) O31 0.0357(9) 0.0328(9) 0.0169(8) 0.0063(7) 0.0047(7) -0.0011(8) C32 0.0218(11) 0.0357(13) 0.0213(11) 0.0150(10) 0.0049(9) 0.0110(10) O32 0.0190(8) 0.0691(14) 0.0502(12) 0.0370(11) 0.0119(8) 0.0132(9) C33 0.0266(11) 0.0307(13) 0.0188(10) 0.0124(10) 0.0006(9) 0.0111(10) O33 0.0532(11) 0.0265(9) 0.0395(10) 0.0163(8) 0.0012(9) 0.0172(9) C41 0.0163(9) 0.0206(10) 0.0154(9) 0.0087(8) 0.0020(8) 0.0011(8) O41 0.0190(7) 0.0286(9) 0.0270(8) 0.0084(7) 0.0032(6) 0.0095(7) C42 0.0168(9) 0.0139(9) 0.0167(9) 0.0063(8) 0.0012(7) 0.0016(8) O42 0.0335(8) 0.0291(9) 0.0147(7) 0.0105(7) 0.0035(6) 0.0044(7) C51 0.0170(9) 0.0198(10) 0.0127(9) 0.0080(8) 0.0041(7) 0.0042(8) O51 0.0272(8) 0.0369(10) 0.0271(8) 0.0150(8) 0.0153(7) 0.0197(7) C52 0.0165(9) 0.0185(10) 0.0130(9) 0.0050(8) 0.0043(7) 0.0007(8) O52 0.0337(9) 0.0214(8) 0.0276(8) 0.0163(7) 0.0044(7) 0.0042(7) C61 0.0252(12) 0.0245(12) 0.0349(13) 0.0217(11) -0.0028(10) 0.0000(10) O61 0.0225(9) 0.0500(12) 0.0699(13) 0.0414(11) 0.0133(9) 0.0152(9) C62 0.0421(14) 0.0316(13) 0.0266(13) 0.0146(11) -0.0058(11) -0.0198(12) O62 0.1066(18) 0.0681(15) 0.0236(10) 0.0207(11) -0.0205(11) -0.0573(14) C63 0.0183(10) 0.0234(12) 0.0258(11) 0.0089(10) 0.0034(9) -0.0006(9) O63 0.0339(9) 0.0246(9) 0.0564(12) 0.0239(9) 0.0029(8) -0.0004(8) P1 0.0120(2) 0.0112(2) 0.0120(2) 0.00511(19) 0.00414(18) 0.00322(18) C111 0.0139(9) 0.0150(9) 0.0172(9) 0.0096(8) 0.0057(7) 0.0054(7) C112 0.0130(9) 0.0191(10) 0.0177(9) 0.0084(8) 0.0053(7) 0.0037(8) C113 0.0247(11) 0.0292(12) 0.0178(10) 0.0095(9) 0.0112(8) 0.0076(9) C114 0.0206(10) 0.0361(13) 0.0286(12) 0.0223(11) 0.0119(9) 0.0060(10) C115 0.0237(11) 0.0241(12) 0.0333(13) 0.0165(10) 0.0117(9) 0.0023(9) C116 0.0242(11) 0.0166(10) 0.0196(10) 0.0069(9) 0.0062(8) 0.0008(8) C121 0.0144(9) 0.0120(9) 0.0164(9) 0.0067(8) 0.0061(7) 0.0048(7) C122 0.0213(10) 0.0148(10) 0.0174(10) 0.0070(8) 0.0060(8) 0.0068(8) C123 0.0242(11) 0.0184(10) 0.0209(10) 0.0102(9) 0.0033(8) 0.0089(9) C124 0.0181(10) 0.0158(10) 0.0273(11) 0.0092(9) 0.0062(8) 0.0069(8) C125 0.0230(10) 0.0163(10) 0.0219(10) 0.0062(9) 0.0101(8) 0.0074(8) C126 0.0171(9) 0.0159(10) 0.0164(9) 0.0074(8) 0.0042(7) 0.0040(8) C10 0.0116(8) 0.0123(9) 0.0105(8) 0.0042(7) 0.0034(7) 0.0049(7) P2 0.0118(2) 0.0118(2) 0.0105(2) 0.00440(19) 0.00364(17) 0.00220(18) C211 0.0138(9) 0.0128(9) 0.0128(9) 0.0066(7) 0.0011(7) 0.0027(7) C212 0.0209(10) 0.0185(10) 0.0164(10) 0.0059(8) 0.0044(8) -0.0003(8) C213 0.0187(10) 0.0214(11) 0.0268(11) 0.0128(10) 0.0037(9) -0.0011(9) C214 0.0172(10) 0.0113(9) 0.0236(11) 0.0049(8) -0.0019(8) 0.0002(8) C215 0.0160(9) 0.0155(10) 0.0189(10) 0.0033(8) 0.0006(8) 0.0058(8) C216 0.0136(9) 0.0139(9) 0.0155(9) 0.0057(8) 0.0023(7) 0.0042(7) C221 0.0126(9) 0.0117(9) 0.0179(9) 0.0034(8) 0.0042(7) 0.0007(7) C222 0.0166(9) 0.0214(11) 0.0220(10) 0.0106(9) 0.0069(8) 0.0048(8) C223 0.0146(10) 0.0241(11) 0.0363(13) 0.0155(10) 0.0036(9) 0.0040(9) C224 0.0098(9) 0.0202(11) 0.0377(13) 0.0008(10) 0.0050(9) 0.0042(8) C225 0.0162(10) 0.0345(13) 0.0211(11) -0.0001(10) 0.0068(8) 0.0044(9) C226 0.0154(9) 0.0254(11) 0.0169(10) 0.0043(9) 0.0052(8) 0.0044(8) C1 0.0158(9) 0.0133(9) 0.0129(9) 0.0059(7) 0.0049(7) 0.0056(7) C2 0.0141(9) 0.0166(10) 0.0171(9) 0.0096(8) 0.0022(7) 0.0055(7) C3 0.0169(9) 0.0144(9) 0.0153(9) 0.0071(8) 0.0039(7) 0.0070(7) C4 0.0179(9) 0.0108(9) 0.0166(9) 0.0054(8) 0.0041(7) 0.0020(7) O4 0.0212(7) 0.0257(8) 0.0184(7) 0.0068(6) 0.0024(6) 0.0114(6) C5 0.0198(9) 0.0089(8) 0.0104(8) 0.0035(7) 0.0029(7) 0.0012(7) P4 0.0121(2) 0.0104(2) 0.0111(2) 0.00495(19) 0.00427(17) 0.00339(18) C411 0.0134(8) 0.0123(9) 0.0114(8) 0.0046(7) 0.0046(7) 0.0004(7) C412 0.0185(10) 0.0211(10) 0.0144(9) 0.0080(8) 0.0048(8) 0.0070(8) C413 0.0198(10) 0.0293(12) 0.0177(10) 0.0068(9) 0.0085(8) 0.0084(9) C414 0.0251(11) 0.0286(12) 0.0157(10) 0.0087(9) 0.0086(8) 0.0019(9) C415 0.0332(12) 0.0241(11) 0.0203(11) 0.0152(9) 0.0091(9) 0.0069(10) C416 0.0228(10) 0.0184(10) 0.0190(10) 0.0100(9) 0.0084(8) 0.0075(8) C421 0.0134(9) 0.0116(9) 0.0123(8) 0.0041(7) 0.0003(7) 0.0038(7) C422 0.0163(9) 0.0161(10) 0.0166(9) 0.0036(8) 0.0025(7) 0.0061(8) C423 0.0201(10) 0.0249(12) 0.0211(11) 0.0005(9) 0.0002(8) 0.0121(9) C424 0.0323(12) 0.0129(10) 0.0256(11) -0.0007(9) -0.0057(9) 0.0089(9) C425 0.0295(12) 0.0137(10) 0.0285(12) 0.0059(9) -0.0034(10) -0.0011(9) C426 0.0211(10) 0.0160(10) 0.0206(10) 0.0063(9) 0.0040(8) 0.0028(8) C20 0.0116(8) 0.0146(9) 0.0120(8) 0.0058(7) 0.0048(7) 0.0043(7) P5 0.0119(2) 0.0116(2) 0.0108(2) 0.00522(19) 0.00308(17) 0.00353(18) C511 0.0147(9) 0.0112(9) 0.0131(9) 0.0045(7) 0.0003(7) 0.0021(7) C512 0.0148(9) 0.0199(10) 0.0182(10) 0.0096(8) 0.0023(7) 0.0027(8) C513 0.0158(9) 0.0218(11) 0.0204(10) 0.0065(9) 0.0047(8) 0.0071(8) C514 0.0211(10) 0.0145(10) 0.0192(10) 0.0049(8) -0.0048(8) 0.0048(8) C515 0.0240(10) 0.0170(10) 0.0177(10) 0.0097(8) -0.0009(8) 0.0022(8) C516 0.0148(9) 0.0213(10) 0.0169(9) 0.0101(8) 0.0022(7) 0.0030(8) C521 0.0152(9) 0.0147(9) 0.0118(9) 0.0055(7) -0.0004(7) 0.0049(7) C522 0.0207(10) 0.0212(11) 0.0146(9) 0.0056(8) 0.0031(8) 0.0050(8) C523 0.0294(12) 0.0274(12) 0.0143(10) 0.0045(9) 0.0054(8) 0.0128(10) C524 0.0410(13) 0.0165(10) 0.0140(10) 0.0003(8) -0.0019(9) 0.0140(10) C525 0.0316(12) 0.0139(10) 0.0216(11) 0.0056(9) -0.0054(9) 0.0020(9) C526 0.0205(10) 0.0171(10) 0.0156(9) 0.0057(8) -0.0003(8) 0.0023(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C12 1.788(2) . ? Co1 C11 1.814(2) . ? Co1 C1 1.9050(19) . ? Co1 P1 2.2091(5) . ? Co1 Co2 2.4767(3) . ? Co1 Co3 2.4894(3) . ? Co2 C22 1.7859(19) . ? Co2 C21 1.797(2) . ? Co2 C1 1.9069(18) . ? Co2 P2 2.2093(5) . ? Co2 Co3 2.4783(4) . ? Co3 C32 1.797(2) . ? Co3 C31 1.813(2) . ? Co3 C33 1.814(2) . ? Co3 C1 1.9130(17) . ? Co4 C42 1.7938(19) . ? Co4 C41 1.799(2) . ? Co4 C5 1.9003(18) . ? Co4 P4 2.1850(5) . ? Co4 Co6 2.4680(4) . ? Co4 Co5 2.4870(3) . ? Co5 C52 1.7734(18) . ? Co5 C51 1.801(2) . ? Co5 C5 1.8849(19) . ? Co5 P5 2.2104(5) . ? Co5 Co6 2.4804(4) . ? Co6 C62 1.788(2) . ? Co6 C63 1.796(2) . ? Co6 C61 1.803(3) . ? Co6 C5 1.9327(18) . ? C11 O11 1.142(3) . ? C12 O12 1.139(2) . ? C21 O21 1.146(2) . ? C22 O22 1.139(2) . ? C31 O31 1.138(3) . ? C32 O32 1.136(2) . ? C33 O33 1.131(3) . ? C41 O41 1.141(2) . ? C42 O42 1.142(2) . ? C51 O51 1.145(2) . ? C52 O52 1.142(2) . ? C61 O61 1.155(3) . ? C62 O62 1.139(3) . ? C63 O63 1.133(2) . ? P1 C111 1.8272(18) . ? P1 C121 1.8284(19) . ? P1 C10 1.8349(18) . ? C111 C112 1.390(3) . ? C111 C116 1.405(3) . ? C112 C113 1.389(2) . ? C112 H112 0.95 . ? C113 C114 1.388(3) . ? C113 H113 0.95 . ? C114 C115 1.375(3) . ? C114 H114 0.95 . ? C115 C116 1.394(3) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.385(3) . ? C121 C122 1.405(2) . ? C122 C123 1.379(3) . ? C122 H122 0.95 . ? C123 C124 1.396(3) . ? C123 H123 0.95 . ? C124 C125 1.379(3) . ? C124 H124 0.95 . ? C125 C126 1.397(3) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 P2 1.8295(16) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? P2 C221 1.825(2) . ? P2 C211 1.8369(19) . ? C211 C216 1.389(3) . ? C211 C212 1.409(2) . ? C212 C213 1.382(3) . ? C212 H212 0.95 . ? C213 C214 1.375(3) . ? C213 H213 0.95 . ? C214 C215 1.378(3) . ? C214 H214 0.95 . ? C215 C216 1.399(3) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.396(3) . ? C221 C222 1.397(2) . ? C222 C223 1.379(3) . ? C222 H222 0.95 . ? C223 C224 1.382(3) . ? C223 H223 0.95 . ? C224 C225 1.382(3) . ? C224 H224 0.95 . ? C225 C226 1.392(3) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C1 C2 1.400(3) . ? C2 C3 1.225(3) . ? C3 C4 1.440(3) . ? C4 O4 1.251(2) . ? C4 C5 1.457(3) . ? P4 C411 1.8208(17) . ? P4 C421 1.826(2) . ? P4 C20 1.8351(17) . ? C411 C412 1.381(3) . ? C411 C416 1.398(2) . ? C412 C413 1.394(3) . ? C412 H412 0.95 . ? C413 C414 1.378(3) . ? C413 H413 0.95 . ? C414 C415 1.380(3) . ? C414 H414 0.95 . ? C415 C416 1.383(3) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C422 1.388(3) . ? C421 C426 1.397(2) . ? C422 C423 1.395(3) . ? C422 H422 0.95 . ? C423 C424 1.383(3) . ? C423 H423 0.95 . ? C424 C425 1.377(3) . ? C424 H424 0.95 . ? C425 C426 1.383(3) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C20 P5 1.8334(16) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P5 C511 1.8328(18) . ? P5 C521 1.837(2) . ? C511 C512 1.390(3) . ? C511 C516 1.397(2) . ? C512 C513 1.392(3) . ? C512 H512 0.95 . ? C513 C514 1.384(3) . ? C513 H513 0.95 . ? C514 C515 1.379(3) . ? C514 H514 0.95 . ? C515 C516 1.393(3) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C526 1.394(2) . ? C521 C522 1.395(3) . ? C522 C523 1.389(3) . ? C522 H522 0.95 . ? C523 C524 1.382(3) . ? C523 H523 0.95 . ? C524 C525 1.381(3) . ? C524 H524 0.95 . ? C525 C526 1.386(3) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? 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 C12 Co1 C11 100.61(9) . . ? C12 Co1 C1 105.15(9) . . ? C11 Co1 C1 142.44(8) . . ? C12 Co1 P1 96.09(6) . . ? C11 Co1 P1 107.99(6) . . ? C1 Co1 P1 96.04(5) . . ? C12 Co1 Co2 152.77(7) . . ? C11 Co1 Co2 98.27(6) . . ? C1 Co1 Co2 49.51(5) . . ? P1 Co1 Co2 96.536(16) . . ? C12 Co1 Co3 97.18(6) . . ? C11 Co1 Co3 100.90(6) . . ? C1 Co1 Co3 49.44(5) . . ? P1 Co1 Co3 145.252(19) . . ? Co2 Co1 Co3 59.872(10) . . ? C22 Co2 C21 99.55(8) . . ? C22 Co2 C1 107.28(8) . . ? C21 Co2 C1 141.26(8) . . ? C22 Co2 P2 96.83(6) . . ? C21 Co2 P2 106.72(6) . . ? C1 Co2 P2 97.41(5) . . ? C22 Co2 Co1 154.63(6) . . ? C21 Co2 Co1 97.21(6) . . ? C1 Co2 Co1 49.44(6) . . ? P2 Co2 Co1 96.417(15) . . ? C22 Co2 Co3 97.91(6) . . ? C21 Co2 Co3 100.00(6) . . ? C1 Co2 Co3 49.66(5) . . ? P2 Co2 Co3 146.738(17) . . ? Co1 Co2 Co3 60.318(10) . . ? C32 Co3 C31 100.89(9) . . ? C32 Co3 C33 97.48(10) . . ? C31 Co3 C33 106.41(9) . . ? C32 Co3 C1 104.40(8) . . ? C31 Co3 C1 141.26(9) . . ? C33 Co3 C1 98.90(8) . . ? C32 Co3 Co2 151.85(6) . . ? C31 Co3 Co2 97.89(6) . . ? C33 Co3 Co2 97.09(7) . . ? C1 Co3 Co2 49.44(6) . . ? C32 Co3 Co1 96.30(6) . . ? C31 Co3 Co1 99.52(6) . . ? C33 Co3 Co1 147.62(6) . . ? C1 Co3 Co1 49.17(6) . . ? Co2 Co3 Co1 59.810(10) . . ? C42 Co4 C41 102.23(8) . . ? C42 Co4 C5 102.99(8) . . ? C41 Co4 C5 144.18(8) . . ? C42 Co4 P4 95.02(6) . . ? C41 Co4 P4 102.26(6) . . ? C5 Co4 P4 100.43(6) . . ? C42 Co4 Co6 101.47(6) . . ? C41 Co4 Co6 99.62(6) . . ? C5 Co4 Co6 50.49(5) . . ? P4 Co4 Co6 149.040(17) . . ? C42 Co4 Co5 151.48(6) . . ? C41 Co4 Co5 102.29(6) . . ? C5 Co4 Co5 48.66(6) . . ? P4 Co4 Co5 93.796(15) . . ? Co6 Co4 Co5 60.074(10) . . ? C52 Co5 C51 106.39(8) . . ? C52 Co5 C5 98.89(8) . . ? C51 Co5 C5 142.98(8) . . ? C52 Co5 P5 97.30(6) . . ? C51 Co5 P5 103.33(6) . . ? C5 Co5 P5 99.70(6) . . ? C52 Co5 Co6 92.74(6) . . ? C51 Co5 Co6 101.11(6) . . ? C5 Co5 Co6 50.32(6) . . ? P5 Co5 Co6 149.669(18) . . ? C52 Co5 Co4 146.17(7) . . ? C51 Co5 Co4 98.38(5) . . ? C5 Co5 Co4 49.19(5) . . ? P5 Co5 Co4 99.018(15) . . ? Co6 Co5 Co4 59.583(10) . . ? C62 Co6 C63 97.97(10) . . ? C62 Co6 C61 104.34(11) . . ? C63 Co6 C61 99.86(9) . . ? C62 Co6 C5 103.36(10) . . ? C63 Co6 C5 105.34(8) . . ? C61 Co6 C5 139.17(9) . . ? C62 Co6 Co4 91.69(7) . . ? C63 Co6 Co4 154.56(7) . . ? C61 Co6 Co4 100.44(6) . . ? C5 Co6 Co4 49.34(5) . . ? C62 Co6 Co5 148.76(7) . . ? C63 Co6 Co5 102.75(7) . . ? C61 Co6 Co5 94.92(7) . . ? C5 Co6 Co5 48.64(6) . . ? Co4 Co6 Co5 60.343(10) . . ? O11 C11 Co1 176.14(18) . . ? O12 C12 Co1 179.15(18) . . ? O21 C21 Co2 176.26(17) . . ? O22 C22 Co2 177.54(17) . . ? O31 C31 Co3 178.13(18) . . ? O32 C32 Co3 179.2(3) . . ? O33 C33 Co3 177.5(2) . . ? O41 C41 Co4 178.54(19) . . ? O42 C42 Co4 179.00(18) . . ? O51 C51 Co5 176.68(16) . . ? O52 C52 Co5 176.55(18) . . ? O61 C61 Co6 177.32(18) . . ? O62 C62 Co6 179.7(2) . . ? O63 C63 Co6 176.78(19) . . ? C111 P1 C121 100.07(8) . . ? C111 P1 C10 104.53(8) . . ? C121 P1 C10 99.94(8) . . ? C111 P1 Co1 115.50(6) . . ? C121 P1 Co1 124.49(6) . . ? C10 P1 Co1 109.72(5) . . ? C112 C111 C116 119.23(17) . . ? C112 C111 P1 124.23(13) . . ? C116 C111 P1 116.53(15) . . ? C113 C112 C111 120.58(18) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C114 C113 C112 119.8(2) . . ? C114 C113 H113 120.1 . . ? C112 C113 H113 120.1 . . ? C115 C114 C113 120.30(18) . . ? C115 C114 H114 119.8 . . ? C113 C114 H114 119.8 . . ? C114 C115 C116 120.49(19) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 119.6(2) . . ? C115 C116 H116 120.2 . . ? C111 C116 H116 120.2 . . ? C126 C121 C122 118.83(17) . . ? C126 C121 P1 123.29(13) . . ? C122 C121 P1 117.58(15) . . ? C123 C122 C121 120.72(19) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C122 C123 C124 119.80(18) . . ? C122 C123 H123 120.1 . . ? C124 C123 H123 120.1 . . ? C125 C124 C123 120.02(19) . . ? C125 C124 H124 120 . . ? C123 C124 H124 120 . . ? C124 C125 C126 120.06(19) . . ? C124 C125 H125 120 . . ? C126 C125 H125 120 . . ? C121 C126 C125 120.47(17) . . ? C121 C126 H126 119.8 . . ? C125 C126 H126 119.8 . . ? P2 C10 P1 108.61(9) . . ? P2 C10 H10A 110 . . ? P1 C10 H10A 110 . . ? P2 C10 H10B 110 . . ? P1 C10 H10B 110 . . ? H10A C10 H10B 108.3 . . ? C221 P2 C10 105.91(8) . . ? C221 P2 C211 100.14(8) . . ? C10 P2 C211 103.58(8) . . ? C221 P2 Co2 120.32(6) . . ? C10 P2 Co2 109.23(6) . . ? C211 P2 Co2 115.97(6) . . ? C216 C211 C212 118.99(17) . . ? C216 C211 P2 123.66(13) . . ? C212 C211 P2 117.35(15) . . ? C213 C212 C211 119.9(2) . . ? C213 C212 H212 120 . . ? C211 C212 H212 120 . . ? C214 C213 C212 120.85(18) . . ? C214 C213 H213 119.6 . . ? C212 C213 H213 119.6 . . ? C213 C214 C215 119.82(18) . . ? C213 C214 H214 120.1 . . ? C215 C214 H214 120.1 . . ? C214 C215 C216 120.5(2) . . ? C214 C215 H215 119.7 . . ? C216 C215 H215 119.7 . . ? C211 C216 C215 119.87(17) . . ? C211 C216 H216 120.1 . . ? C215 C216 H216 120.1 . . ? C226 C221 C222 117.52(19) . . ? C226 C221 P2 119.91(14) . . ? C222 C221 P2 122.36(15) . . ? C223 C222 C221 121.23(19) . . ? C223 C222 H222 119.4 . . ? C221 C222 H222 119.4 . . ? C222 C223 C224 120.46(19) . . ? C222 C223 H223 119.8 . . ? C224 C223 H223 119.8 . . ? C225 C224 C223 119.7(2) . . ? C225 C224 H224 120.2 . . ? C223 C224 H224 120.2 . . ? C224 C225 C226 119.8(2) . . ? C224 C225 H225 120.1 . . ? C226 C225 H225 120.1 . . ? C225 C226 C221 121.31(18) . . ? C225 C226 H226 119.3 . . ? C221 C226 H226 119.3 . . ? C2 C1 Co1 129.80(13) . . ? C2 C1 Co2 133.02(14) . . ? Co1 C1 Co2 81.05(8) . . ? C2 C1 Co3 131.18(14) . . ? Co1 C1 Co3 81.39(7) . . ? Co2 C1 Co3 80.90(7) . . ? C3 C2 C1 174.1(2) . . ? C2 C3 C4 166.8(2) . . ? O4 C4 C3 118.14(19) . . ? O4 C4 C5 122.96(18) . . ? C3 C4 C5 118.90(16) . . ? C4 C5 Co5 134.02(13) . . ? C4 C5 Co4 131.38(12) . . ? Co5 C5 Co4 82.15(8) . . ? C4 C5 Co6 128.36(13) . . ? Co5 C5 Co6 81.03(7) . . ? Co4 C5 Co6 80.16(7) . . ? C411 P4 C421 104.64(8) . . ? C411 P4 C20 102.85(8) . . ? C421 P4 C20 103.30(8) . . ? C411 P4 Co4 112.70(6) . . ? C421 P4 Co4 120.23(6) . . ? C20 P4 Co4 111.35(6) . . ? C412 C411 C416 118.97(17) . . ? C412 C411 P4 120.50(13) . . ? C416 C411 P4 120.05(15) . . ? C411 C412 C413 121.25(17) . . ? C411 C412 H412 119.4 . . ? C413 C412 H412 119.4 . . ? C414 C413 C412 119.0(2) . . ? C414 C413 H413 120.5 . . ? C412 C413 H413 120.5 . . ? C413 C414 C415 120.54(18) . . ? C413 C414 H414 119.7 . . ? C415 C414 H414 119.7 . . ? C414 C415 C416 120.49(18) . . ? C414 C415 H415 119.8 . . ? C416 C415 H415 119.8 . . ? C415 C416 C411 119.76(19) . . ? C415 C416 H416 120.1 . . ? C411 C416 H416 120.1 . . ? C422 C421 C426 118.28(18) . . ? C422 C421 P4 119.96(14) . . ? C426 C421 P4 121.68(15) . . ? C421 C422 C423 121.04(18) . . ? C421 C422 H422 119.5 . . ? C423 C422 H422 119.5 . . ? C424 C423 C422 119.6(2) . . ? C424 C423 H423 120.2 . . ? C422 C423 H423 120.2 . . ? C425 C424 C423 119.9(2) . . ? C425 C424 H424 120.1 . . ? C423 C424 H424 120.1 . . ? C424 C425 C426 120.6(2) . . ? C424 C425 H425 119.7 . . ? C426 C425 H425 119.7 . . ? C425 C426 C421 120.5(2) . . ? C425 C426 H426 119.7 . . ? C421 C426 H426 119.7 . . ? P5 C20 P4 108.94(9) . . ? P5 C20 H20A 109.9 . . ? P4 C20 H20A 109.9 . . ? P5 C20 H20B 109.9 . . ? P4 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C511 P5 C20 103.04(8) . . ? C511 P5 C521 101.28(8) . . ? C20 P5 C521 105.69(8) . . ? C511 P5 Co5 117.74(6) . . ? C20 P5 Co5 108.37(6) . . ? C521 P5 Co5 119.03(6) . . ? C512 C511 C516 118.85(16) . . ? C512 C511 P5 122.51(13) . . ? C516 C511 P5 118.63(14) . . ? C511 C512 C513 120.81(17) . . ? C511 C512 H512 119.6 . . ? C513 C512 H512 119.6 . . ? C514 C513 C512 119.97(19) . . ? C514 C513 H513 120 . . ? C512 C513 H513 120 . . ? C515 C514 C513 119.62(17) . . ? C515 C514 H514 120.2 . . ? C513 C514 H514 120.2 . . ? C514 C515 C516 120.83(17) . . ? C514 C515 H515 119.6 . . ? C516 C515 H515 119.6 . . ? C515 C516 C511 119.87(19) . . ? C515 C516 H516 120.1 . . ? C511 C516 H516 120.1 . . ? C526 C521 C522 117.98(19) . . ? C526 C521 P5 122.95(15) . . ? C522 C521 P5 119.04(14) . . ? C523 C522 C521 121.05(19) . . ? C523 C522 H522 119.5 . . ? C521 C522 H522 119.5 . . ? C524 C523 C522 120.2(2) . . ? C524 C523 H523 119.9 . . ? C522 C523 H523 119.9 . . ? C525 C524 C523 119.4(2) . . ? C525 C524 H524 120.3 . . ? C523 C524 H524 120.3 . . ? C524 C525 C526 120.65(19) . . ? C524 C525 H525 119.7 . . ? C526 C525 H525 119.7 . . ? C525 C526 C521 120.7(2) . . ? C525 C526 H526 119.6 . . ? C521 C526 H526 119.6 . . ?