# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '4685_web_deposit_cif_file_0_Dr.OlivierBlacque_1300285322.cif' _audit_update_record ; 2011-03-16 # Formatted by publCIF ; # #------------------------------------------------------------------------- #2 Person making the deposition # _publ_contact_author 'Dr. Blacque, Olivier' _publ_contact_author_email oblacque@aci.uzh.ch _publ_contact_author_fax '+41 44 63 54 681' _publ_contact_author_phone '+41 44 63 54 651' #------------------------------------------------------------------------- #3 Publication details # # Provide these details if the structure has been published, # accepted or submitted for publication # # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal # # #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ _publ_section_comment ; (type here to add) ; _publ_section_abstract ; (type here to add abstract) ; _publ_contact_letter ; Please consider this CIF for publication. I certify that this contibution is the original work of those listed as authors; that it has not been published before (in any language or medium) and is not being considered for publication elsewhere; that all authors concur with and are aware of the submission; that all workers involved in the study are listed as authors or given proper credit in the acknowledgements; that I have obtained permission for and acknowledged the source of any excerpts from other copyright works; and that to the best of my knowledge the paper contains no statements which are libellous, unlawful or in any way actionable. All coauthors have made significant scientific contributions to the work reported, including the ideas and their execution, and share responsibility and accountability for the results. ; _publ_requested_category FM #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Biocompatibility and Cardiomyocyte Protection of 17 e- Rhenium Dicarbonyl CO-Releasing Molecules on a Cobalamin Scaffold ; loop_ _publ_author_name _publ_author_address #Corresponding author of the paper F.Zobi ; Institute of Inorganic Chemistry University of Z\"urich Wintherthurerstrasse 190, 8057 Z\"urich (Switzerland) ; O.Blacque ; Institute of Inorganic Chemistry University of Z\"urich Wintherthurerstrasse 190, 8057 Z\"urich (Switzerland) ; R.A.Jacobs ; Institute of Veterinary Physiology University of Z\"urich Wintherthurerstrasse 260, 8057 Z\"urich (Switzerland) ; M.C.Schaub ; Institute of Pharmacology and Toxycology University of Z\"urich Wintherthurerstrasse 190, 8057 Z\"urich (Switzerland) ; A.Yu.Bogdanova ; Institute of Veterinary Physiology University of Z\"urich Wintherthurerstrasse 260, 8057 Z\"urich (Switzerland) ; _publ_contact_author_name 'Dr. Blacque, Olivier' #----------------------------------------------------------------------------# data_2 _database_code_depnum_ccdc_archive 'CCDC 817626' #TrackingRef '4685_web_deposit_cif_file_0_Dr.OlivierBlacque_1300285322.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C70 H94 Co N16 O15 P), 5(C3 H6 O), 16 O' _chemical_formula_sum 'C155 H218 Co2 N32 O51 P2' _chemical_formula_weight 3525.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M '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 15.5066(4) _cell_length_b 22.9558(7) _cell_length_c 25.1741(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8961.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 10575 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 32.78 _chemical_absolute_configuration ad _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 71958 _diffrn_reflns_av_R_equivalents 0.1164 _diffrn_reflns_av_sigmaI/netI 0.2230 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.68 _reflns_number_total 16995 _reflns_number_gt 8376 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_structure_solution ; SHELXS97. Program for Crystal Structure solution. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_structure_refinement ; SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_molecular_graphics ; ORTEP-3 for Windows, Version 2.01. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. ; _computing_publication_material ; WinGX -- An integrated system of Windows programs for the solution, refinment and analysis of single crystal X-ray diffraction data, Version 1.80.00. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. PLATON for Windows, Version 1.12. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _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^)+(0.0657P)^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_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). Acta Cryst. A39, 876-881. 7752 Friedel pairs' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 16995 _refine_ls_number_parameters 1113 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1588 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.23444(5) 0.08876(4) 0.25648(3) 0.0194(2) Uani 1 1 d . . . P1 P -0.00905(12) 0.27072(9) -0.03091(7) 0.0333(5) Uani 1 1 d . . . C1 C 0.4203(4) 0.0883(3) 0.2421(2) 0.0254(14) Uani 1 1 d . . . C2 C 0.4302(4) 0.0299(3) 0.2634(3) 0.0271(16) Uani 1 1 d . . . C3 C 0.3631(4) -0.0050(3) 0.2737(2) 0.0219(16) Uani 1 1 d . . . C4 C 0.3649(4) -0.0677(3) 0.2948(3) 0.0310(17) Uani 1 1 d . . . C5 C 0.2741(4) -0.0906(3) 0.2782(2) 0.0299(16) Uani 1 1 d . . . H5 H 0.2501 -0.1163 0.3066 0.036 Uiso 1 1 calc R . . C6 C 0.2252(4) -0.0345(3) 0.2763(2) 0.0253(13) Uani 1 1 d U . . C7 C 0.1368(4) -0.0310(3) 0.2855(2) 0.0276(14) Uani 1 1 d U . . H7 H 0.1074 -0.0665 0.2922 0.033 Uiso 1 1 calc R . . C8 C 0.0875(4) 0.0193(3) 0.2858(2) 0.0262(14) Uani 1 1 d U . . C9 C -0.0060(4) 0.0216(3) 0.3051(3) 0.044(2) Uani 1 1 d . . . C10 C -0.0354(4) 0.0783(3) 0.2789(3) 0.0302(18) Uani 1 1 d . . . H10 H -0.0766 0.0995 0.3027 0.036 Uiso 1 1 calc R . . C11 C 0.0493(4) 0.1122(3) 0.2743(2) 0.0232(16) Uani 1 1 d . . . C12 C 0.0551(4) 0.1706(3) 0.2685(2) 0.0218(15) Uani 1 1 d . . . C13 C 0.1360(4) 0.1996(3) 0.2572(2) 0.0220(15) Uani 1 1 d . . . C14 C 0.1562(4) 0.2651(2) 0.2573(2) 0.0201(14) Uani 1 1 d . . . C15 C 0.2458(4) 0.2663(2) 0.2324(2) 0.0237(15) Uani 1 1 d . . . H15 H 0.2392 0.2653 0.1929 0.028 Uiso 1 1 calc R . . C16 C 0.2849(3) 0.2078(2) 0.2504(2) 0.0202(14) Uani 1 1 d . . . H16 H 0.3055 0.2120 0.2879 0.024 Uiso 1 1 calc R . . C17 C 0.3558(4) 0.1747(3) 0.2176(2) 0.0232(15) Uani 1 1 d . . . C18 C 0.4527(4) 0.1877(3) 0.2306(2) 0.0231(16) Uani 1 1 d . . . C19 C 0.4924(4) 0.1264(3) 0.2234(2) 0.0277(16) Uani 1 1 d . B . H19 H 0.5419 0.1222 0.2487 0.033 Uiso 1 1 calc R . . C20 C 0.2578(4) 0.1028(2) 0.3285(3) 0.0246(15) Uani 1 1 d . . . C21 C 0.1360(4) 0.0885(3) 0.1555(2) 0.0234(15) Uani 1 1 d . . . H21A H 0.0965 0.1142 0.1724 0.028 Uiso 1 1 calc R . . C22 C 0.1961(4) 0.0346(3) 0.0955(2) 0.0238(16) Uani 1 1 d . . . C23 C 0.2450(4) 0.0344(3) 0.1409(2) 0.0232(15) Uani 1 1 d . . . C24 C 0.2196(5) 0.0041(3) 0.0499(3) 0.042(2) Uani 1 1 d . . . H24 H 0.1838 0.0049 0.0192 0.050 Uiso 1 1 calc R . . C25 C 0.2947(5) -0.0269(3) 0.0497(3) 0.0382(19) Uani 1 1 d . . . C26 C 0.3469(4) -0.0271(3) 0.0963(3) 0.040(2) Uani 1 1 d . . . C27 C 0.3219(4) 0.0032(3) 0.1406(3) 0.0305(17) Uani 1 1 d . . . H27 H 0.3574 0.0028 0.1714 0.037 Uiso 1 1 calc R . . C28 C 0.3218(6) -0.0606(4) 0.0017(3) 0.083(3) Uani 1 1 d . . . H28A H 0.2860 -0.0494 -0.0286 0.125 Uiso 1 1 calc R . . H28B H 0.3148 -0.1024 0.0086 0.125 Uiso 1 1 calc R . . H28C H 0.3824 -0.0523 -0.0062 0.125 Uiso 1 1 calc R . . C30 C 0.5229(4) 0.0112(3) 0.2777(3) 0.043(2) Uani 1 1 d . . . H30A H 0.5606 0.0455 0.2780 0.065 Uiso 1 1 calc R . . H30B H 0.5439 -0.0167 0.2513 0.065 Uiso 1 1 calc R . . H30C H 0.5232 -0.0070 0.3129 0.065 Uiso 1 1 calc R . . C31 C 0.4378(4) -0.1076(3) 0.2743(3) 0.0379(19) Uani 1 1 d . . . H31A H 0.4919 -0.0975 0.2923 0.057 Uiso 1 1 calc R . . H31B H 0.4447 -0.1023 0.2359 0.057 Uiso 1 1 calc R . . H31C H 0.4233 -0.1483 0.2818 0.057 Uiso 1 1 calc R . . C32 C 0.3677(5) -0.0621(3) 0.3561(3) 0.0366(19) Uani 1 1 d . . . H32A H 0.4245 -0.0462 0.3667 0.044 Uiso 1 1 calc R . . H32B H 0.3230 -0.0340 0.3676 0.044 Uiso 1 1 calc R . . C33 C 0.3533(6) -0.1186(3) 0.3841(3) 0.045(2) Uani 1 1 d . . . C34 C 0.2726(4) -0.1220(3) 0.2250(3) 0.0389(18) Uani 1 1 d . . . H34A H 0.3066 -0.1583 0.2283 0.047 Uiso 1 1 calc R . . H34B H 0.3017 -0.0971 0.1983 0.047 Uiso 1 1 calc R . . C35 C 0.1827(5) -0.1375(3) 0.2043(3) 0.047(2) Uani 1 1 d . . . H35A H 0.1515 -0.1605 0.2314 0.057 Uiso 1 1 calc R . . H35B H 0.1497 -0.1013 0.1976 0.057 Uiso 1 1 calc R . . C36 C 0.1890(6) -0.1716(4) 0.1546(4) 0.058(2) Uani 1 1 d . . . C38 C 0.4313(5) -0.0614(3) 0.0975(3) 0.058(3) Uani 1 1 d . . . H38A H 0.4725 -0.0438 0.0727 0.086 Uiso 1 1 calc R . . H38B H 0.4203 -0.1018 0.0871 0.086 Uiso 1 1 calc R . . H38C H 0.4554 -0.0604 0.1335 0.086 Uiso 1 1 calc R . . C39 C -0.0563(5) -0.0348(3) 0.2933(5) 0.092(4) Uani 1 1 d . . . H39A H -0.0322 -0.0668 0.3143 0.138 Uiso 1 1 calc R . . H39B H -0.0514 -0.0441 0.2554 0.138 Uiso 1 1 calc R . . H39C H -0.1171 -0.0293 0.3025 0.138 Uiso 1 1 calc R . . C40 C 0.0000(5) 0.0318(4) 0.3661(3) 0.070(3) Uani 1 1 d . . . H40A H 0.0370 0.0655 0.3732 0.105 Uiso 1 1 calc R . . H40B H 0.0245 -0.0028 0.3832 0.105 Uiso 1 1 calc R . . H40C H -0.0578 0.0391 0.3804 0.105 Uiso 1 1 calc R . . C41 C -0.0263(4) 0.2072(3) 0.2751(3) 0.042(2) Uani 1 1 d . . . H41A H -0.0727 0.1829 0.2895 0.063 Uiso 1 1 calc R . . H41B H -0.0438 0.2228 0.2405 0.063 Uiso 1 1 calc R . . H41C H -0.0147 0.2395 0.2996 0.063 Uiso 1 1 calc R . . C42 C 0.1558(4) 0.2849(3) 0.3164(2) 0.0354(18) Uani 1 1 d . . . H42A H 0.2004 0.2637 0.3360 0.053 Uiso 1 1 calc R . . H42B H 0.0993 0.2767 0.3321 0.053 Uiso 1 1 calc R . . H42C H 0.1674 0.3268 0.3183 0.053 Uiso 1 1 calc R . . C43 C 0.0922(4) 0.3036(3) 0.2274(2) 0.0241(16) Uani 1 1 d . . . H43A H 0.0377 0.3049 0.2479 0.029 Uiso 1 1 calc R . . H43B H 0.1156 0.3437 0.2264 0.029 Uiso 1 1 calc R . . C44 C 0.0709(5) 0.2853(3) 0.1707(2) 0.0385(19) Uani 1 1 d . . . H44A H 0.1226 0.2904 0.1480 0.046 Uiso 1 1 calc R . . H44B H 0.0552 0.2435 0.1702 0.046 Uiso 1 1 calc R . . C45 C 0.4950(4) 0.2352(3) 0.1959(3) 0.0392(19) Uani 1 1 d . . . H45A H 0.4731 0.2735 0.2064 0.059 Uiso 1 1 calc R . . H45B H 0.4813 0.2280 0.1585 0.059 Uiso 1 1 calc R . . H45C H 0.5577 0.2341 0.2008 0.059 Uiso 1 1 calc R . . C46 C 0.4612(4) 0.2067(3) 0.2888(3) 0.0270(17) Uani 1 1 d . . . H46A H 0.4346 0.1765 0.3116 0.032 Uiso 1 1 calc R . . H46B H 0.4283 0.2432 0.2939 0.032 Uiso 1 1 calc R . . C47 C 0.5542(5) 0.2166(4) 0.3074(3) 0.0395(19) Uani 1 1 d . . . C48 C 0.5246(5) 0.1129(4) 0.1670(3) 0.053(2) Uani 1 1 d D . . H48A H 0.4735 0.1079 0.1439 0.064 Uiso 1 1 calc R A 1 H48B H 0.5562 0.1475 0.1540 0.064 Uiso 1 1 calc R A 1 C49A C 0.5811(10) 0.0613(6) 0.1596(4) 0.028(5) Uani 0.56(3) 1 d PD B 1 H49A H 0.5455 0.0256 0.1613 0.033 Uiso 0.56(3) 1 calc PR B 1 H49B H 0.6233 0.0597 0.1891 0.033 Uiso 0.56(3) 1 calc PR B 1 C49B C 0.6177(12) 0.0984(15) 0.1574(7) 0.085(11) Uani 0.44(3) 1 d PD B 2 H49C H 0.6403 0.0761 0.1881 0.102 Uiso 0.44(3) 1 calc PR B 2 H49D H 0.6512 0.1350 0.1546 0.102 Uiso 0.44(3) 1 calc PR B 2 C50 C 0.6308(6) 0.0622(5) 0.1061(3) 0.066(3) Uani 1 1 d D . . C51 C 0.3338(4) 0.1793(3) 0.1586(2) 0.0265(16) Uani 1 1 d . . . H51A H 0.3514 0.2176 0.1452 0.040 Uiso 1 1 calc R . . H51B H 0.2715 0.1745 0.1537 0.040 Uiso 1 1 calc R . . H51C H 0.3644 0.1488 0.1389 0.040 Uiso 1 1 calc R . . C52 C -0.0030(5) 0.3208(3) 0.1480(3) 0.0394(19) Uani 1 1 d . . . C53 C -0.0545(5) 0.3791(3) 0.0740(3) 0.050(2) Uani 1 1 d . . . H53A H -0.0283 0.4158 0.0612 0.060 Uiso 1 1 calc R . . H53B H -0.1012 0.3894 0.0991 0.060 Uiso 1 1 calc R . . C54 C -0.0933(5) 0.3471(3) 0.0272(3) 0.042(2) Uani 1 1 d . . . H54 H -0.1205 0.3100 0.0395 0.051 Uiso 1 1 calc R . . C55 C -0.1571(5) 0.3823(4) -0.0034(3) 0.055(2) Uani 1 1 d . . . H55A H -0.1307 0.4192 -0.0141 0.082 Uiso 1 1 calc R . . H55B H -0.2076 0.3901 0.0189 0.082 Uiso 1 1 calc R . . H55C H -0.1750 0.3606 -0.0351 0.082 Uiso 1 1 calc R . . C56 C 0.0098(4) 0.1753(3) 0.0254(3) 0.0335(18) Uani 1 1 d . . . H56 H -0.0072 0.1591 -0.0099 0.040 Uiso 1 1 calc R . . C57 C -0.0525(5) 0.1545(3) 0.0688(3) 0.0388(19) Uani 1 1 d . . . H57 H -0.0595 0.1862 0.0957 0.047 Uiso 1 1 calc R . . C58 C 0.0656(4) 0.0917(3) 0.0664(2) 0.0302(16) Uani 1 1 d . . . H58 H 0.0553 0.0624 0.0377 0.036 Uiso 1 1 calc R . . C59 C 0.0964(4) 0.1496(3) 0.0435(2) 0.0281(17) Uani 1 1 d . . . H59 H 0.1365 0.1436 0.0129 0.034 Uiso 1 1 calc R . . C60 C -0.1387(5) 0.1389(4) 0.0473(3) 0.048(2) Uani 1 1 d . . . H60A H -0.1772 0.1253 0.0761 0.058 Uiso 1 1 calc R . . H60B H -0.1657 0.1730 0.0299 0.058 Uiso 1 1 calc R . . C61 C -0.1875(5) 0.0767(5) -0.0235(4) 0.060(3) Uani 1 1 d . . . C62 C -0.2206(6) 0.0098(4) -0.0953(3) 0.062(3) Uani 1 1 d . . . H62A H -0.1872 0.0039 -0.1284 0.074 Uiso 1 1 calc R . . H62B H -0.2673 0.0379 -0.1031 0.074 Uiso 1 1 calc R . . C63 C -0.2598(5) -0.0469(4) -0.0789(3) 0.050(2) Uani 1 1 d . . . C64 C -0.3067(7) -0.0537(5) -0.0341(4) 0.076(3) Uani 1 1 d . . . H64 H -0.3190 -0.0210 -0.0121 0.091 Uiso 1 1 calc R . . C65 C -0.3365(8) -0.1081(5) -0.0204(4) 0.098(4) Uani 1 1 d . . . H65 H -0.3632 -0.1131 0.0133 0.118 Uiso 1 1 calc R . . C66 C -0.2802(7) -0.1484(5) -0.0957(5) 0.088(3) Uani 1 1 d . . . H66 H -0.2667 -0.1816 -0.1167 0.106 Uiso 1 1 calc R . . C67 C -0.2483(6) -0.0947(5) -0.1105(4) 0.076(3) Uani 1 1 d . . . H67 H -0.2179 -0.0908 -0.1431 0.091 Uiso 1 1 calc R . . C68 C 0.3041(4) 0.3181(3) 0.2470(3) 0.0358(17) Uani 1 1 d . . . H68A H 0.3051 0.3224 0.2861 0.043 Uiso 1 1 calc R . . H68B H 0.3636 0.3097 0.2351 0.043 Uiso 1 1 calc R . . C69 C 0.2749(5) 0.3752(3) 0.2224(3) 0.043(2) Uani 1 1 d . . . C70 C -0.0735(5) 0.0732(4) 0.2215(3) 0.066(3) Uani 1 1 d . . . H70A H -0.0529 0.1081 0.2023 0.079 Uiso 1 1 calc R . . H70B H -0.0436 0.0396 0.2051 0.079 Uiso 1 1 calc R . . C71 C -0.1566(7) 0.0674(7) 0.2079(4) 0.149(7) Uani 1 1 d . . . H71A H -0.1663 0.0259 0.1991 0.179 Uiso 1 1 calc R . . H71B H -0.1655 0.0898 0.1748 0.179 Uiso 1 1 calc R . . C72 C -0.2245(5) 0.0849(6) 0.2453(4) 0.069(3) Uani 1 1 d . . . C76 C 0.0247(7) -0.0654(6) -0.0454(5) 0.093(4) Uani 1 1 d . . . C77 C -0.0028(7) -0.0920(6) -0.0970(4) 0.121(5) Uani 1 1 d . . . H77A H 0.0482 -0.1054 -0.1165 0.182 Uiso 1 1 calc R . . H77B H -0.0335 -0.0628 -0.1182 0.182 Uiso 1 1 calc R . . H77C H -0.0410 -0.1251 -0.0901 0.182 Uiso 1 1 calc R . . O79 O 0.0049(6) -0.0171(4) -0.0311(4) 0.130(3) Uani 1 1 d . . . N1 N 0.3465(3) 0.1137(2) 0.23639(18) 0.0184(12) Uani 1 1 d . . . N3 N 0.2073(3) 0.1694(2) 0.25006(18) 0.0188(11) Uani 1 1 d . . . N4 N 0.1155(3) 0.0719(2) 0.27304(17) 0.0190(13) Uani 1 1 d . . . N5 N 0.2051(3) 0.0699(2) 0.17931(19) 0.0199(12) Uani 1 1 d . . . N6 N 0.1238(3) 0.0694(2) 0.1063(2) 0.0251(13) Uani 1 1 d . . . N7 N 0.2728(4) 0.1133(3) 0.3716(2) 0.0479(17) Uani 1 1 d . . . N8 N -0.3294(7) -0.1547(4) -0.0528(5) 0.108(3) Uani 1 1 d . . . N9 N 0.4212(4) -0.1531(3) 0.3901(2) 0.058(2) Uani 1 1 d . . . H9B H 0.4150 -0.1877 0.4047 0.070 Uiso 1 1 calc R . . H9A H 0.4724 -0.1414 0.3795 0.070 Uiso 1 1 calc R . . O2 O 0.2528(5) -0.1987(3) 0.1396(3) 0.115(3) Uani 1 1 d . . . N11 N 0.5711(4) 0.2681(3) 0.3261(2) 0.0566(19) Uani 1 1 d . . . H11B H 0.6225 0.2757 0.3393 0.068 Uiso 1 1 calc R . . H11A H 0.5313 0.2954 0.3255 0.068 Uiso 1 1 calc R . . O4 O 0.6606(5) 0.0157(3) 0.0952(3) 0.102(3) Uani 1 1 d . B . N13 N 0.0095(4) 0.3462(3) 0.1016(2) 0.0505(18) Uani 1 1 d . . . H13 H 0.0605 0.3425 0.0867 0.061 Uiso 1 1 calc R . . N14 N -0.1638(5) 0.0345(3) -0.0546(3) 0.062(2) Uani 1 1 d . . . H14 H -0.1114 0.0202 -0.0510 0.074 Uiso 1 1 calc R . . O14 O 0.2505(4) 0.3768(2) 0.1752(2) 0.0611(15) Uani 1 1 d . . . O15 O -0.2633(5) 0.0496(3) 0.2726(3) 0.098(3) Uani 1 1 d . . . N38 N 0.2767(3) 0.0106(2) 0.26694(18) 0.0205(12) Uani 1 1 d . . . O1 O 0.2802(3) -0.1332(2) 0.3984(2) 0.0632(17) Uani 1 1 d . . . N10 N 0.1178(5) -0.1717(3) 0.1247(3) 0.077(2) Uani 1 1 d . . . H10B H 0.1170 -0.1911 0.0945 0.092 Uiso 1 1 calc R . . H10A H 0.0718 -0.1524 0.1352 0.092 Uiso 1 1 calc R . . O3 O 0.6082(4) 0.1769(3) 0.3075(3) 0.080(2) Uani 1 1 d . . . N12 N 0.6322(4) 0.1048(3) 0.0724(3) 0.0528(19) Uani 1 1 d . B . H12A H 0.6554 0.0998 0.0409 0.063 Uiso 1 1 calc R . . H12B H 0.6100 0.1388 0.0811 0.063 Uiso 1 1 calc R . . O5 O -0.0716(3) 0.3261(3) 0.1727(2) 0.0580(16) Uani 1 1 d . . . O6 O -0.0203(3) 0.3341(2) -0.00846(17) 0.0363(12) Uani 1 1 d . . . O7 O -0.0894(3) 0.2457(2) -0.05206(17) 0.0400(13) Uani 1 1 d . . . O8 O 0.0667(3) 0.2723(2) -0.06678(19) 0.0508(14) Uani 1 1 d . . . O9 O 0.0139(3) 0.2377(2) 0.02341(18) 0.0401(13) Uani 1 1 d . . . O10 O -0.0123(3) 0.1061(2) 0.09333(17) 0.0348(12) Uani 1 1 d . . . O11 O 0.1353(3) 0.1823(2) 0.08387(16) 0.0329(12) Uani 1 1 d . . . H11 H 0.1641 0.2095 0.0703 0.049 Uiso 1 1 calc R . . O12 O -0.1244(3) 0.0935(3) 0.0097(2) 0.0540(14) Uani 1 1 d . . . O13 O -0.2585(4) 0.1041(3) -0.0239(2) 0.0706(17) Uani 1 1 d . . . N15 N 0.2803(4) 0.4214(3) 0.2507(3) 0.064(2) Uani 1 1 d . . . H15A H 0.2668 0.4554 0.2369 0.077 Uiso 1 1 calc R . . H15B H 0.2977 0.4191 0.2839 0.077 Uiso 1 1 calc R . . N16 N -0.2414(4) 0.1418(3) 0.2483(3) 0.070(2) Uani 1 1 d . . . H16A H -0.2812 0.1546 0.2703 0.083 Uiso 1 1 calc R . . H16B H -0.2127 0.1665 0.2282 0.083 Uiso 1 1 calc R . . O17 O 0.2384(4) 0.2473(3) -0.0780(2) 0.0803(19) Uani 1 1 d . . . O18 O -0.1792(5) 0.2251(4) 0.1712(3) 0.115(3) Uani 1 1 d . . . C79 C 0.0832(7) -0.1032(5) -0.0109(4) 0.119(4) Uani 1 1 d . . . H79A H 0.1290 -0.1200 -0.0329 0.178 Uiso 1 1 calc R . . H79B H 0.0493 -0.1345 0.0052 0.178 Uiso 1 1 calc R . . H79C H 0.1090 -0.0792 0.0171 0.178 Uiso 1 1 calc R . . O22 O -0.1023(3) 0.1508(2) -0.1188(2) 0.0633(17) Uani 1 1 d . . . O23 O 0.2343(4) 0.2698(3) 0.0513(3) 0.102(2) Uani 1 1 d . . . O24 O 0.4139(5) 0.3131(3) 0.3881(3) 0.115(3) Uani 1 1 d . . . O25 O 0.3064(8) 0.2241(4) 0.4195(3) 0.174(4) Uani 1 1 d . . . O26 O 0.3502(6) 0.4142(4) 0.3530(3) 0.165(4) Uani 1 1 d . . . O28A O -0.3088(10) -0.2719(7) -0.0289(6) 0.107(5) Uiso 0.50 1 d P C 1 O28B O -0.3887(9) -0.2607(6) -0.0214(5) 0.097(4) Uiso 0.50 1 d P D 2 C73 C -0.0864(9) -0.0796(7) 0.0987(5) 0.105(4) Uani 1 1 d . . . C74 C -0.1168(11) -0.0256(7) 0.0933(7) 0.186(7) Uani 1 1 d . . . H74A H -0.1668 -0.0204 0.1166 0.278 Uiso 1 1 calc R . . H74B H -0.1342 -0.0192 0.0563 0.278 Uiso 1 1 calc R . . H74C H -0.0719 0.0024 0.1030 0.278 Uiso 1 1 calc R . . C75 C -0.1433(16) -0.1179(8) 0.0665(7) 0.235(11) Uani 1 1 d . . . H75A H -0.1582 -0.0982 0.0332 0.353 Uiso 1 1 calc R . . H75B H -0.1961 -0.1264 0.0865 0.353 Uiso 1 1 calc R . . H75C H -0.1131 -0.1544 0.0586 0.353 Uiso 1 1 calc R . . O20 O -0.0348(6) -0.0979(7) 0.1269(5) 0.253(9) Uani 1 1 d . . . C81 C 0.5634(10) 0.2942(7) 0.5155(6) 0.121(4) Uani 0.50 1 d PD . . C82 C 0.5011(11) 0.3216(9) 0.4777(6) 0.121(4) Uani 0.50 1 d PD . . H82A H 0.4439 0.3233 0.4941 0.182 Uiso 0.50 1 calc PR . . H82B H 0.4981 0.2982 0.4451 0.182 Uiso 0.50 1 calc PR . . H82C H 0.5204 0.3611 0.4690 0.182 Uiso 0.50 1 calc PR . . C83 C 0.6251(12) 0.2533(8) 0.4888(6) 0.121(4) Uani 0.50 1 d PD . . H83A H 0.6454 0.2243 0.5144 0.182 Uiso 0.50 1 calc PR . . H83B H 0.6745 0.2754 0.4751 0.182 Uiso 0.50 1 calc PR . . H83C H 0.5959 0.2336 0.4593 0.182 Uiso 0.50 1 calc PR . . O27 O 0.5712(10) 0.2996(6) 0.5593(4) 0.121(4) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0219(4) 0.0179(4) 0.0185(4) 0.0032(4) -0.0024(4) 0.0021(4) P1 0.0423(12) 0.0282(12) 0.0295(11) 0.0032(9) -0.0068(9) 0.0073(10) C1 0.033(4) 0.026(4) 0.017(3) -0.004(3) -0.005(3) 0.012(4) C2 0.016(3) 0.029(4) 0.036(4) -0.005(3) -0.005(3) -0.001(3) C3 0.031(4) 0.009(4) 0.025(4) 0.001(3) -0.012(3) 0.004(3) C4 0.031(4) 0.022(4) 0.040(4) 0.006(3) -0.007(3) 0.003(3) C5 0.032(4) 0.018(4) 0.040(4) 0.003(3) -0.004(3) -0.005(4) C6 0.037(3) 0.017(3) 0.022(3) 0.001(2) -0.010(3) -0.003(3) C7 0.040(3) 0.016(3) 0.027(3) 0.003(3) -0.005(3) -0.008(3) C8 0.038(3) 0.017(3) 0.024(3) 0.000(3) -0.005(3) -0.005(3) C9 0.021(4) 0.024(5) 0.087(7) -0.002(4) 0.007(4) -0.008(3) C10 0.016(4) 0.030(5) 0.045(4) -0.004(4) 0.010(3) -0.002(3) C11 0.016(4) 0.040(5) 0.013(3) 0.003(3) 0.000(3) 0.002(3) C12 0.015(3) 0.022(4) 0.028(4) -0.002(3) 0.001(3) 0.003(3) C13 0.033(4) 0.025(4) 0.008(3) 0.002(3) 0.002(3) 0.011(3) C14 0.024(4) 0.013(3) 0.023(4) 0.003(3) 0.004(3) 0.004(3) C15 0.025(4) 0.020(4) 0.026(4) 0.000(3) -0.003(3) 0.007(3) C16 0.020(3) 0.017(3) 0.024(4) 0.001(3) -0.003(3) -0.004(3) C17 0.033(4) 0.016(4) 0.020(4) 0.001(3) 0.008(3) -0.002(3) C18 0.023(4) 0.019(4) 0.027(4) 0.005(3) -0.002(3) 0.000(3) C19 0.032(4) 0.023(4) 0.028(4) 0.006(3) -0.003(3) -0.007(3) C20 0.020(4) 0.019(4) 0.035(4) 0.001(3) -0.002(3) 0.008(3) C21 0.027(4) 0.014(4) 0.030(4) -0.002(3) 0.002(3) -0.003(3) C22 0.030(4) 0.017(4) 0.025(4) 0.004(3) -0.004(3) 0.001(3) C23 0.024(4) 0.025(4) 0.021(3) 0.003(3) -0.007(3) -0.001(3) C24 0.068(6) 0.036(5) 0.022(4) 0.005(3) -0.014(4) 0.000(4) C25 0.055(5) 0.033(5) 0.027(4) -0.006(3) 0.003(4) 0.014(4) C26 0.036(5) 0.044(5) 0.041(5) -0.008(4) 0.001(4) 0.010(4) C27 0.033(4) 0.037(5) 0.022(4) 0.006(3) -0.014(3) 0.000(4) C28 0.091(7) 0.110(9) 0.049(6) -0.040(6) -0.014(5) 0.031(6) C30 0.023(4) 0.035(5) 0.070(6) 0.014(4) -0.005(4) 0.000(3) C31 0.039(4) 0.029(5) 0.045(5) -0.003(3) -0.014(3) 0.014(3) C32 0.045(5) 0.016(4) 0.049(5) 0.003(4) -0.006(4) -0.001(4) C33 0.061(6) 0.039(5) 0.033(5) 0.009(4) -0.017(4) 0.008(5) C34 0.040(4) 0.025(4) 0.051(5) 0.007(4) -0.003(4) 0.003(4) C35 0.039(5) 0.052(6) 0.052(5) -0.017(4) -0.017(4) 0.012(4) C36 0.064(6) 0.040(6) 0.069(6) -0.012(5) -0.036(5) 0.022(5) C38 0.040(5) 0.068(6) 0.065(6) -0.035(5) -0.011(4) 0.025(4) C39 0.028(5) 0.032(6) 0.216(12) 0.031(7) 0.015(6) -0.001(4) C40 0.065(6) 0.078(7) 0.067(7) 0.038(6) 0.038(5) 0.020(5) C41 0.037(5) 0.030(5) 0.059(5) 0.001(4) 0.012(4) -0.005(4) C42 0.037(5) 0.033(5) 0.037(4) -0.001(4) -0.006(3) 0.002(4) C43 0.028(4) 0.023(4) 0.022(4) -0.001(3) 0.000(3) -0.004(3) C44 0.051(5) 0.033(5) 0.032(4) 0.007(4) -0.006(4) 0.018(4) C45 0.031(4) 0.042(5) 0.045(5) -0.002(4) 0.005(4) 0.008(4) C46 0.016(4) 0.024(4) 0.041(4) -0.003(3) -0.001(3) -0.006(3) C47 0.035(5) 0.046(6) 0.038(5) 0.006(4) -0.002(4) 0.001(4) C48 0.038(5) 0.071(7) 0.051(5) 0.006(5) 0.014(4) 0.009(5) C49A 0.046(10) 0.024(9) 0.013(7) 0.004(6) 0.016(6) -0.008(7) C49B 0.09(2) 0.12(3) 0.046(14) 0.027(16) 0.008(13) 0.021(19) C50 0.073(7) 0.090(9) 0.036(5) 0.011(6) 0.017(5) 0.050(6) C51 0.028(4) 0.019(4) 0.033(4) -0.001(3) 0.003(3) -0.005(3) C52 0.053(5) 0.028(5) 0.037(5) -0.007(4) -0.024(4) 0.002(4) C53 0.075(6) 0.042(5) 0.033(5) 0.001(4) -0.012(4) 0.019(5) C54 0.055(5) 0.035(5) 0.037(5) 0.007(4) 0.007(4) 0.013(4) C55 0.053(6) 0.067(6) 0.044(5) 0.004(4) -0.006(4) 0.030(5) C56 0.037(4) 0.028(5) 0.036(4) 0.003(4) -0.012(4) -0.007(4) C57 0.044(5) 0.041(5) 0.032(4) -0.001(4) -0.003(4) 0.000(4) C58 0.041(4) 0.018(4) 0.031(4) -0.002(3) -0.003(3) 0.004(4) C59 0.028(4) 0.034(5) 0.023(4) -0.009(3) 0.002(3) 0.006(3) C60 0.042(5) 0.066(6) 0.036(5) -0.011(4) -0.005(4) 0.004(4) C61 0.030(5) 0.094(8) 0.057(6) 0.011(6) -0.006(4) 0.002(5) C62 0.095(7) 0.053(6) 0.038(5) -0.001(4) -0.013(5) -0.015(5) C63 0.054(5) 0.047(6) 0.050(5) -0.008(4) -0.015(5) 0.001(5) C64 0.108(8) 0.067(8) 0.052(7) -0.009(6) 0.007(6) -0.007(6) C65 0.153(11) 0.073(9) 0.068(8) -0.018(7) 0.012(7) -0.033(8) C66 0.108(9) 0.064(8) 0.092(8) -0.013(6) 0.015(7) -0.003(7) C67 0.089(7) 0.063(7) 0.076(6) -0.008(6) -0.016(6) 0.001(7) C68 0.036(4) 0.018(4) 0.053(5) 0.005(4) 0.003(4) -0.001(3) C69 0.032(4) 0.031(5) 0.067(6) -0.007(4) 0.007(4) -0.014(4) C70 0.022(4) 0.104(8) 0.070(6) -0.022(6) 0.007(4) -0.021(5) C71 0.075(8) 0.30(2) 0.073(8) -0.051(10) -0.014(6) 0.095(10) C72 0.030(5) 0.098(9) 0.081(7) -0.032(7) -0.011(5) 0.005(6) C76 0.081(8) 0.085(9) 0.114(10) 0.008(8) -0.020(7) 0.019(7) C77 0.136(10) 0.161(12) 0.066(7) -0.045(8) -0.044(7) 0.035(10) O79 0.148(8) 0.087(6) 0.154(8) -0.045(6) -0.045(6) 0.057(6) N1 0.024(3) 0.021(3) 0.010(3) -0.003(2) -0.006(2) 0.003(2) N3 0.025(3) 0.018(3) 0.013(3) 0.003(2) -0.001(2) -0.004(2) N4 0.015(3) 0.023(3) 0.018(3) 0.001(2) -0.006(2) 0.003(3) N5 0.026(3) 0.012(3) 0.021(3) 0.002(2) -0.005(2) 0.003(2) N6 0.027(3) 0.027(3) 0.021(3) 0.001(2) -0.009(2) 0.002(3) N7 0.057(4) 0.055(4) 0.032(4) 0.001(3) -0.017(3) 0.003(4) N8 0.131(9) 0.074(8) 0.120(9) -0.004(7) 0.000(7) -0.036(7) N9 0.054(5) 0.050(5) 0.072(5) 0.027(4) -0.001(4) 0.005(4) O2 0.083(5) 0.132(7) 0.130(6) -0.095(5) -0.058(5) 0.054(5) N11 0.047(4) 0.041(5) 0.082(5) 0.004(4) -0.021(4) -0.016(4) O4 0.128(6) 0.094(6) 0.084(5) 0.036(4) 0.050(5) 0.058(5) N13 0.062(4) 0.062(5) 0.027(4) 0.001(3) -0.011(3) 0.032(4) N14 0.083(6) 0.051(5) 0.052(5) -0.019(4) -0.011(4) 0.009(4) O14 0.073(4) 0.053(4) 0.057(4) 0.021(3) 0.005(3) 0.004(3) O15 0.063(5) 0.062(5) 0.170(8) -0.029(5) -0.012(5) 0.022(4) N38 0.017(3) 0.014(3) 0.030(3) -0.002(2) -0.008(2) 0.007(2) O1 0.043(4) 0.068(4) 0.079(4) 0.033(3) 0.011(3) -0.006(3) N10 0.077(6) 0.077(6) 0.077(5) -0.019(5) -0.032(4) 0.020(5) O3 0.042(4) 0.090(5) 0.108(5) -0.039(4) -0.024(3) 0.026(4) N12 0.059(4) 0.048(5) 0.051(5) -0.010(4) 0.015(4) 0.018(4) O5 0.036(3) 0.077(4) 0.061(4) 0.012(3) -0.006(3) 0.012(3) O6 0.043(3) 0.029(3) 0.036(3) 0.008(2) 0.001(2) 0.014(2) O7 0.048(3) 0.032(3) 0.040(3) 0.004(2) -0.013(2) 0.005(2) O8 0.055(4) 0.043(4) 0.054(3) -0.007(3) 0.014(3) -0.001(3) O9 0.055(3) 0.027(3) 0.039(3) -0.006(2) -0.016(3) 0.000(2) O10 0.030(3) 0.038(3) 0.036(3) 0.017(2) -0.005(2) -0.001(2) O11 0.043(3) 0.026(3) 0.030(3) 0.008(2) -0.006(2) -0.007(2) O12 0.043(3) 0.066(4) 0.054(3) -0.002(3) -0.018(3) 0.000(3) O13 0.061(4) 0.094(5) 0.057(4) -0.003(3) -0.010(3) -0.008(4) N15 0.059(4) 0.025(4) 0.109(6) -0.004(4) -0.022(4) 0.003(3) N16 0.042(4) 0.073(6) 0.093(5) -0.014(5) 0.022(4) -0.012(4) O17 0.093(5) 0.077(4) 0.071(4) -0.017(3) -0.020(4) -0.008(4) O18 0.094(5) 0.160(8) 0.092(5) 0.027(5) -0.022(4) -0.048(5) C79 0.111(10) 0.120(12) 0.126(10) 0.013(9) -0.017(8) 0.026(8) O22 0.046(3) 0.072(4) 0.071(4) -0.021(3) 0.000(3) -0.006(3) O23 0.053(4) 0.092(5) 0.161(6) 0.078(5) -0.023(4) -0.038(4) O24 0.108(6) 0.118(7) 0.120(6) -0.045(5) -0.011(5) 0.041(5) O25 0.304(14) 0.097(7) 0.122(7) 0.006(6) -0.066(8) -0.011(8) O26 0.232(11) 0.117(7) 0.146(7) -0.039(6) -0.103(7) 0.019(7) C73 0.119(11) 0.094(11) 0.102(10) 0.033(9) 0.018(8) 0.055(9) C74 0.216(19) 0.147(16) 0.194(17) -0.057(14) 0.020(14) 0.035(15) C75 0.38(3) 0.156(19) 0.166(18) -0.010(14) 0.027(19) -0.04(2) O20 0.101(8) 0.39(2) 0.269(14) 0.211(15) 0.017(8) 0.107(10) C81 0.180(11) 0.115(9) 0.069(7) 0.029(7) 0.006(8) -0.059(8) C82 0.180(11) 0.115(9) 0.069(7) 0.029(7) 0.006(8) -0.059(8) C83 0.180(11) 0.115(9) 0.069(7) 0.029(7) 0.006(8) -0.059(8) O27 0.180(11) 0.115(9) 0.069(7) 0.029(7) 0.006(8) -0.059(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C20 1.877(7) . ? Co1 N1 1.898(5) . ? Co1 N3 1.906(5) . ? Co1 N38 1.928(5) . ? Co1 N4 1.930(5) . ? Co1 N5 2.042(5) . ? P1 O7 1.471(5) . ? P1 O8 1.482(5) . ? P1 O6 1.571(5) . ? P1 O9 1.603(5) . ? C1 N1 1.293(7) . ? C1 C2 1.452(9) . ? C1 C19 1.495(8) . ? C2 C3 1.338(8) . ? C2 C30 1.543(8) . ? C3 N38 1.397(7) . ? C3 C4 1.535(8) . ? C4 C31 1.544(9) . ? C4 C32 1.551(9) . ? C4 C5 1.560(8) . ? C5 C6 1.494(8) . ? C5 C34 1.522(8) . ? C5 H5 1.0000 . ? C6 N38 1.329(7) . ? C6 C7 1.393(8) . ? C7 C8 1.385(9) . ? C7 H7 0.9500 . ? C8 N4 1.323(8) . ? C8 C9 1.530(9) . ? C9 C10 1.529(10) . ? C9 C39 1.541(10) . ? C9 C40 1.556(11) . ? C10 C11 1.532(8) . ? C10 C70 1.567(10) . ? C10 H10 1.0000 . ? C11 C12 1.350(8) . ? C11 N4 1.382(8) . ? C12 C13 1.448(8) . ? C12 C41 1.525(9) . ? C13 N3 1.316(7) . ? C13 C14 1.536(8) . ? C14 C15 1.526(8) . ? C14 C43 1.529(8) . ? C14 C42 1.556(8) . ? C15 C68 1.538(8) . ? C15 C16 1.541(8) . ? C15 H15 1.0000 . ? C16 N3 1.492(7) . ? C16 C17 1.572(8) . ? C16 H16 1.0000 . ? C17 N1 1.486(7) . ? C17 C51 1.527(8) . ? C17 C18 1.566(8) . ? C18 C46 1.534(8) . ? C18 C45 1.543(9) . ? C18 C19 1.547(9) . ? C19 C48 1.537(9) . ? C19 H19 1.0000 . ? C20 N7 1.136(7) . ? C21 N5 1.300(7) . ? C21 N6 1.328(7) . ? C21 H21A 0.9500 . ? C22 C23 1.373(8) . ? C22 C24 1.393(9) . ? C22 N6 1.404(8) . ? C23 C27 1.391(9) . ? C23 N5 1.408(7) . ? C24 C25 1.364(9) . ? C24 H24 0.9500 . ? C25 C26 1.426(9) . ? C25 C28 1.494(9) . ? C26 C27 1.370(9) . ? C26 C38 1.527(9) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.494(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O1 1.236(9) . ? C33 N9 1.326(9) . ? C34 C35 1.530(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.478(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O2 1.228(9) . ? C36 N10 1.336(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.524(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C52 1.518(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.534(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 O3 1.238(9) . ? C47 N11 1.299(9) . ? C48 C49A 1.485(11) . ? C48 C49B 1.501(15) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49A C50 1.552(11) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C49B C50 1.548(16) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50 O4 1.196(10) . ? C50 N12 1.293(10) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O5 1.238(9) . ? C52 N13 1.320(9) . ? C53 N13 1.428(9) . ? C53 C54 1.512(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O6 1.474(8) . ? C54 C55 1.492(9) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 O9 1.435(8) . ? C56 C57 1.534(9) . ? C56 C59 1.536(8) . ? C56 H56 1.0000 . ? C57 O10 1.416(8) . ? C57 C60 1.487(9) . ? C57 H57 1.0000 . ? C58 O10 1.424(7) . ? C58 N6 1.444(7) . ? C58 C59 1.525(9) . ? C58 H58 1.0000 . ? C59 O11 1.399(7) . ? C59 H59 1.0000 . ? C60 O12 1.426(8) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 O13 1.267(9) . ? C61 N14 1.297(10) . ? C61 O12 1.344(9) . ? C62 N14 1.467(9) . ? C62 C63 1.495(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.351(11) . ? C63 C67 1.368(11) . ? C64 C65 1.376(13) . ? C64 H64 0.9500 . ? C65 N8 1.350(12) . ? C65 H65 0.9500 . ? C66 N8 1.332(12) . ? C66 C67 1.380(13) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.517(10) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 O14 1.247(8) . ? C69 N15 1.281(9) . ? C70 C71 1.339(11) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.468(12) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 O15 1.221(11) . ? C72 N16 1.334(12) . ? C76 O79 1.205(12) . ? C76 C77 1.497(14) . ? C76 C79 1.526(13) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? N9 H9B 0.8800 . ? N9 H9A 0.8800 . ? N11 H11B 0.8800 . ? N11 H11A 0.8800 . ? N13 H13 0.8800 . ? N14 H14 0.8800 . ? N10 H10B 0.8800 . ? N10 H10A 0.8800 . ? N12 H12A 0.8800 . ? N12 H12B 0.8800 . ? O11 H11 0.8400 . ? N15 H15A 0.8800 . ? N15 H15B 0.8800 . ? N16 H16A 0.8800 . ? N16 H16B 0.8800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C73 O20 1.150(13) . ? C73 C74 1.332(16) . ? C73 C75 1.487(19) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C81 O27 1.116(11) . ? C81 C82 1.494(5) . ? C81 C83 1.500(5) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Co1 N1 91.7(2) . . ? C20 Co1 N3 87.5(2) . . ? N1 Co1 N3 83.5(2) . . ? C20 Co1 N38 87.9(2) . . ? N1 Co1 N38 90.3(2) . . ? N3 Co1 N38 172.2(2) . . ? C20 Co1 N4 90.6(2) . . ? N1 Co1 N4 173.1(2) . . ? N3 Co1 N4 90.1(2) . . ? N38 Co1 N4 96.3(2) . . ? C20 Co1 N5 177.0(2) . . ? N1 Co1 N5 90.83(19) . . ? N3 Co1 N5 94.37(19) . . ? N38 Co1 N5 90.48(19) . . ? N4 Co1 N5 87.13(19) . . ? O7 P1 O8 117.4(3) . . ? O7 P1 O6 113.4(3) . . ? O8 P1 O6 106.6(3) . . ? O7 P1 O9 108.2(3) . . ? O8 P1 O9 110.8(3) . . ? O6 P1 O9 99.0(2) . . ? N1 C1 C2 123.4(6) . . ? N1 C1 C19 111.3(6) . . ? C2 C1 C19 125.3(5) . . ? C3 C2 C1 122.8(5) . . ? C3 C2 C30 120.9(6) . . ? C1 C2 C30 116.2(5) . . ? C2 C3 N38 124.7(6) . . ? C2 C3 C4 127.9(6) . . ? N38 C3 C4 107.4(5) . . ? C3 C4 C31 117.0(6) . . ? C3 C4 C32 105.5(5) . . ? C31 C4 C32 111.1(5) . . ? C3 C4 C5 102.0(5) . . ? C31 C4 C5 111.9(5) . . ? C32 C4 C5 108.6(5) . . ? C6 C5 C34 111.8(5) . . ? C6 C5 C4 100.2(5) . . ? C34 C5 C4 114.1(5) . . ? C6 C5 H5 110.1 . . ? C34 C5 H5 110.1 . . ? C4 C5 H5 110.1 . . ? N38 C6 C7 125.1(6) . . ? N38 C6 C5 111.8(5) . . ? C7 C6 C5 123.0(6) . . ? C8 C7 C6 126.4(6) . . ? C8 C7 H7 116.8 . . ? C6 C7 H7 116.8 . . ? N4 C8 C7 125.3(6) . . ? N4 C8 C9 111.0(6) . . ? C7 C8 C9 123.6(6) . . ? C10 C9 C8 100.1(5) . . ? C10 C9 C39 118.7(6) . . ? C8 C9 C39 112.9(6) . . ? C10 C9 C40 108.4(6) . . ? C8 C9 C40 105.2(6) . . ? C39 C9 C40 110.4(7) . . ? C9 C10 C11 102.1(5) . . ? C9 C10 C70 116.5(6) . . ? C11 C10 C70 107.0(5) . . ? C9 C10 H10 110.3 . . ? C11 C10 H10 110.3 . . ? C70 C10 H10 110.3 . . ? C12 C11 N4 127.8(5) . . ? C12 C11 C10 124.7(6) . . ? N4 C11 C10 107.4(5) . . ? C11 C12 C13 122.3(5) . . ? C11 C12 C41 118.7(5) . . ? C13 C12 C41 119.0(6) . . ? N3 C13 C12 120.9(6) . . ? N3 C13 C14 110.1(5) . . ? C12 C13 C14 128.7(5) . . ? C15 C14 C43 112.2(5) . . ? C15 C14 C13 101.7(4) . . ? C43 C14 C13 115.7(5) . . ? C15 C14 C42 113.1(5) . . ? C43 C14 C42 107.4(5) . . ? C13 C14 C42 106.7(5) . . ? C14 C15 C68 116.8(5) . . ? C14 C15 C16 102.8(4) . . ? C68 C15 C16 111.8(5) . . ? C14 C15 H15 108.4 . . ? C68 C15 H15 108.4 . . ? C16 C15 H15 108.4 . . ? N3 C16 C15 101.3(4) . . ? N3 C16 C17 106.0(4) . . ? C15 C16 C17 122.7(5) . . ? N3 C16 H16 108.7 . . ? C15 C16 H16 108.7 . . ? C17 C16 H16 108.7 . . ? N1 C17 C51 110.7(5) . . ? N1 C17 C18 101.9(5) . . ? C51 C17 C18 113.9(5) . . ? N1 C17 C16 102.7(4) . . ? C51 C17 C16 108.8(5) . . ? C18 C17 C16 117.9(5) . . ? C46 C18 C45 107.7(5) . . ? C46 C18 C19 109.6(5) . . ? C45 C18 C19 114.0(5) . . ? C46 C18 C17 109.7(5) . . ? C45 C18 C17 115.1(5) . . ? C19 C18 C17 100.6(5) . . ? C1 C19 C48 114.5(6) . . ? C1 C19 C18 101.4(5) . . ? C48 C19 C18 114.9(5) . . ? C1 C19 H19 108.6 . . ? C48 C19 H19 108.6 . . ? C18 C19 H19 108.6 . . ? N7 C20 Co1 177.6(6) . . ? N5 C21 N6 116.0(6) . . ? N5 C21 H21A 122.0 . . ? N6 C21 H21A 122.0 . . ? C23 C22 C24 122.7(6) . . ? C23 C22 N6 106.4(6) . . ? C24 C22 N6 130.9(6) . . ? C22 C23 C27 118.1(6) . . ? C22 C23 N5 109.1(5) . . ? C27 C23 N5 132.8(5) . . ? C25 C24 C22 119.2(6) . . ? C25 C24 H24 120.4 . . ? C22 C24 H24 120.4 . . ? C24 C25 C26 118.9(6) . . ? C24 C25 C28 120.9(7) . . ? C26 C25 C28 120.1(7) . . ? C27 C26 C25 120.4(6) . . ? C27 C26 C38 119.2(6) . . ? C25 C26 C38 120.4(6) . . ? C26 C27 C23 120.6(6) . . ? C26 C27 H27 119.7 . . ? C23 C27 H27 119.7 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C2 C30 H30A 109.5 . . ? C2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C4 C31 H31A 109.5 . . ? C4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C4 113.1(6) . . ? C33 C32 H32A 108.9 . . ? C4 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C4 C32 H32B 108.9 . . ? H32A C32 H32B 107.8 . . ? O1 C33 N9 122.2(8) . . ? O1 C33 C32 120.6(7) . . ? N9 C33 C32 117.0(8) . . ? C5 C34 C35 115.1(6) . . ? C5 C34 H34A 108.5 . . ? C35 C34 H34A 108.5 . . ? C5 C34 H34B 108.5 . . ? C35 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C36 C35 C34 110.6(6) . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? O2 C36 N10 119.4(8) . . ? O2 C36 C35 125.6(7) . . ? N10 C36 C35 115.1(8) . . ? C26 C38 H38A 109.5 . . ? C26 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C26 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C9 C39 H39A 109.5 . . ? C9 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C9 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C9 C40 H40A 109.5 . . ? C9 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C9 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C12 C41 H41A 109.5 . . ? C12 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C12 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C14 C42 H42A 109.5 . . ? C14 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C14 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C14 116.3(5) . . ? C44 C43 H43A 108.2 . . ? C14 C43 H43A 108.2 . . ? C44 C43 H43B 108.2 . . ? C14 C43 H43B 108.2 . . ? H43A C43 H43B 107.4 . . ? C52 C44 C43 111.5(6) . . ? C52 C44 H44A 109.3 . . ? C43 C44 H44A 109.3 . . ? C52 C44 H44B 109.3 . . ? C43 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C18 C45 H45A 109.5 . . ? C18 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C18 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C18 C46 C47 114.6(5) . . ? C18 C46 H46A 108.6 . . ? C47 C46 H46A 108.6 . . ? C18 C46 H46B 108.6 . . ? C47 C46 H46B 108.6 . . ? H46A C46 H46B 107.6 . . ? O3 C47 N11 122.2(7) . . ? O3 C47 C46 121.8(7) . . ? N11 C47 C46 115.9(7) . . ? C49A C48 C49B 40.1(11) . . ? C49A C48 C19 118.0(7) . . ? C49B C48 C19 120.5(9) . . ? C49A C48 H48A 107.8 . . ? C49B C48 H48A 130.5 . . ? C19 C48 H48A 107.8 . . ? C49A C48 H48B 107.8 . . ? C49B C48 H48B 69.4 . . ? C19 C48 H48B 107.8 . . ? H48A C48 H48B 107.1 . . ? C48 C49A C50 113.0(8) . . ? C48 C49A H49A 109.0 . . ? C50 C49A H49A 109.0 . . ? C48 C49A H49B 109.0 . . ? C50 C49A H49B 109.0 . . ? H49A C49A H49B 107.8 . . ? C48 C49B C50 112.4(14) . . ? C48 C49B H49C 109.1 . . ? C50 C49B H49C 109.1 . . ? C48 C49B H49D 109.1 . . ? C50 C49B H49D 109.1 . . ? H49C C49B H49D 107.9 . . ? O4 C50 N12 121.2(8) . . ? O4 C50 C49B 136.1(13) . . ? N12 C50 C49B 98.3(14) . . ? O4 C50 C49A 112.2(9) . . ? N12 C50 C49A 126.0(9) . . ? C49B C50 C49A 38.6(10) . . ? C17 C51 H51A 109.5 . . ? C17 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C17 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O5 C52 N13 121.9(7) . . ? O5 C52 C44 120.8(7) . . ? N13 C52 C44 117.3(7) . . ? N13 C53 C54 113.5(6) . . ? N13 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? N13 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? O6 C54 C55 107.7(5) . . ? O6 C54 C53 105.5(6) . . ? C55 C54 C53 113.8(6) . . ? O6 C54 H54 109.9 . . ? C55 C54 H54 109.9 . . ? C53 C54 H54 109.9 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O9 C56 C57 111.3(6) . . ? O9 C56 C59 110.8(5) . . ? C57 C56 C59 102.7(5) . . ? O9 C56 H56 110.6 . . ? C57 C56 H56 110.6 . . ? C59 C56 H56 110.6 . . ? O10 C57 C60 111.4(6) . . ? O10 C57 C56 106.0(6) . . ? C60 C57 C56 112.4(6) . . ? O10 C57 H57 108.9 . . ? C60 C57 H57 108.9 . . ? C56 C57 H57 108.9 . . ? O10 C58 N6 106.3(5) . . ? O10 C58 C59 104.1(5) . . ? N6 C58 C59 112.1(5) . . ? O10 C58 H58 111.3 . . ? N6 C58 H58 111.3 . . ? C59 C58 H58 111.3 . . ? O11 C59 C58 109.2(5) . . ? O11 C59 C56 112.7(5) . . ? C58 C59 C56 99.9(5) . . ? O11 C59 H59 111.5 . . ? C58 C59 H59 111.5 . . ? C56 C59 H59 111.5 . . ? O12 C60 C57 106.2(6) . . ? O12 C60 H60A 110.5 . . ? C57 C60 H60A 110.5 . . ? O12 C60 H60B 110.5 . . ? C57 C60 H60B 110.5 . . ? H60A C60 H60B 108.7 . . ? O13 C61 N14 127.8(8) . . ? O13 C61 O12 119.6(9) . . ? N14 C61 O12 112.5(8) . . ? N14 C62 C63 112.8(6) . . ? N14 C62 H62A 109.0 . . ? C63 C62 H62A 109.0 . . ? N14 C62 H62B 109.0 . . ? C63 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C64 C63 C67 117.7(9) . . ? C64 C63 C62 123.3(8) . . ? C67 C63 C62 118.9(9) . . ? C63 C64 C65 119.6(10) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? N8 C65 C64 122.7(10) . . ? N8 C65 H65 118.6 . . ? C64 C65 H65 118.6 . . ? N8 C66 C67 121.4(10) . . ? N8 C66 H66 119.3 . . ? C67 C66 H66 119.3 . . ? C63 C67 C66 120.8(10) . . ? C63 C67 H67 119.6 . . ? C66 C67 H67 119.6 . . ? C69 C68 C15 113.3(6) . . ? C69 C68 H68A 108.9 . . ? C15 C68 H68A 108.9 . . ? C69 C68 H68B 108.9 . . ? C15 C68 H68B 108.9 . . ? H68A C68 H68B 107.7 . . ? O14 C69 N15 121.7(8) . . ? O14 C69 C68 120.3(7) . . ? N15 C69 C68 117.9(7) . . ? C71 C70 C10 127.3(7) . . ? C71 C70 H70A 105.5 . . ? C10 C70 H70A 105.5 . . ? C71 C70 H70B 105.5 . . ? C10 C70 H70B 105.5 . . ? H70A C70 H70B 106.1 . . ? C70 C71 C72 120.0(9) . . ? C70 C71 H71A 107.3 . . ? C72 C71 H71A 107.3 . . ? C70 C71 H71B 107.3 . . ? C72 C71 H71B 107.3 . . ? H71A C71 H71B 106.9 . . ? O15 C72 N16 121.4(9) . . ? O15 C72 C71 122.2(12) . . ? N16 C72 C71 116.4(12) . . ? O79 C76 C77 124.1(11) . . ? O79 C76 C79 120.3(12) . . ? C77 C76 C79 115.6(11) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C1 N1 C17 112.0(5) . . ? C1 N1 Co1 130.2(4) . . ? C17 N1 Co1 117.3(4) . . ? C13 N3 C16 111.5(5) . . ? C13 N3 Co1 133.2(4) . . ? C16 N3 Co1 113.3(3) . . ? C8 N4 C11 111.2(5) . . ? C8 N4 Co1 123.3(4) . . ? C11 N4 Co1 125.5(4) . . ? C21 N5 C23 103.7(5) . . ? C21 N5 Co1 123.5(4) . . ? C23 N5 Co1 132.7(4) . . ? C21 N6 C22 104.8(5) . . ? C21 N6 C58 128.4(6) . . ? C22 N6 C58 124.5(5) . . ? C66 N8 C65 116.9(10) . . ? C33 N9 H9B 120.0 . . ? C33 N9 H9A 120.0 . . ? H9B N9 H9A 120.0 . . ? C47 N11 H11B 120.0 . . ? C47 N11 H11A 120.0 . . ? H11B N11 H11A 120.0 . . ? C52 N13 C53 124.2(7) . . ? C52 N13 H13 117.9 . . ? C53 N13 H13 117.9 . . ? C61 N14 C62 122.6(8) . . ? C61 N14 H14 118.7 . . ? C62 N14 H14 118.7 . . ? C6 N38 C3 110.8(5) . . ? C6 N38 Co1 123.0(4) . . ? C3 N38 Co1 125.5(4) . . ? C36 N10 H10B 120.0 . . ? C36 N10 H10A 120.0 . . ? H10B N10 H10A 120.0 . . ? C50 N12 H12A 120.0 . . ? C50 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? C54 O6 P1 119.4(4) . . ? C56 O9 P1 119.5(4) . . ? C57 O10 C58 110.4(5) . . ? C59 O11 H11 109.5 . . ? C61 O12 C60 120.6(7) . . ? C69 N15 H15A 120.0 . . ? C69 N15 H15B 120.0 . . ? H15A N15 H15B 120.0 . . ? C72 N16 H16A 120.0 . . ? C72 N16 H16B 120.0 . . ? H16A N16 H16B 120.0 . . ? C76 C79 H79A 109.5 . . ? C76 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C76 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O20 C73 C74 131(2) . . ? O20 C73 C75 122.1(17) . . ? C74 C73 C75 106.5(15) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O27 C81 C82 130.7(9) . . ? O27 C81 C83 116.3(8) . . ? C82 C81 C83 113.0(8) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.769 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.070 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 817627' #TrackingRef '4685_web_deposit_cif_file_0_Dr.OlivierBlacque_1300285322.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 0.53(C63 H86 Co N14 O14 P), 0.47(C66 H88 Co Br N14 O18 P Re), C3 H6 O, 6.53 (H2 O) ; _chemical_formula_sum 'C67.40 H106 Br0.47 Co N14 O23.40 P Re0.47' _chemical_formula_weight 1700.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 15.8806(2) _cell_length_b 21.8255(3) _cell_length_c 26.2738(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9106.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 25786 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 32.77 _chemical_absolute_configuration ad _exptl_crystal_description tablet _exptl_crystal_colour purple _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3559.4 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_T_min 0.530 _exptl_absorpt_correction_T_max 0.884 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 79318 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.10 _reflns_number_total 20093 _reflns_number_gt 13534 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_structure_solution ; SHELXS97. Program for Crystal Structure solution. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_structure_refinement ; SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_molecular_graphics ; ORTEP-3 for Windows, Version 2.01. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. ; _computing_publication_material ; WinGX -- An integrated system of Windows programs for the solution, refinment and analysis of single crystal X-ray diffraction data, Version 1.80.00. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. PLATON for Windows, Version 1.12. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _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 'w=1/[\s^2^(Fo^2^)+(0.1049P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). Acta Cryst. A39, 876-881. 9210 Friedel pairs' _refine_ls_abs_structure_Flack 0.039(7) _refine_ls_number_reflns 20093 _refine_ls_number_parameters 1076 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1816 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.23909(4) 0.10174(3) 0.25285(3) 0.02087(17) Uani 1 1 d . . . P1 P -0.01678(9) 0.26455(7) -0.02209(6) 0.0285(3) Uani 1 1 d . . . C1 C 0.3555(3) 0.1857(2) 0.2057(2) 0.0239(12) Uani 1 1 d . . . C2 C 0.4522(3) 0.2018(2) 0.2132(2) 0.0230(12) Uani 1 1 d . . . C3 C 0.4921(3) 0.1365(2) 0.2171(2) 0.0245(12) Uani 1 1 d . . . H3 H 0.5382 0.1376 0.2419 0.029 Uiso 1 1 calc R . . C4 C 0.4200(3) 0.0999(3) 0.2391(2) 0.0249(12) Uani 1 1 d . . . C5 C 0.4305(3) 0.0417(2) 0.2655(2) 0.0262(12) Uani 1 1 d . . . C6 C 0.3626(3) 0.0051(2) 0.2759(2) 0.0242(12) Uani 1 1 d . . . C7 C 0.3647(3) -0.0593(2) 0.3001(2) 0.0271(12) Uani 1 1 d . . . C8 C 0.2774(3) -0.0850(2) 0.2837(2) 0.0264(12) Uani 1 1 d . . . H8 H 0.2533 -0.1109 0.3105 0.032 Uiso 1 1 calc R . . C9 C 0.2297(3) -0.0246(2) 0.2795(2) 0.0240(12) Uani 1 1 d . . . C10 C 0.1430(3) -0.0211(3) 0.2878(2) 0.0314(13) Uani 1 1 d . . . H10 H 0.1150 -0.0574 0.2955 0.038 Uiso 1 1 calc R . . C11 C 0.0953(3) 0.0316(2) 0.2855(2) 0.0270(12) Uani 1 1 d . . . C12 C 0.0047(3) 0.0357(3) 0.3053(3) 0.0348(14) Uani 1 1 d . . . C13 C -0.0235(3) 0.0963(3) 0.2792(2) 0.0313(13) Uani 1 1 d . . . H13 H -0.0590 0.1197 0.3028 0.038 Uiso 1 1 calc R . . C14 C 0.0596(3) 0.1294(3) 0.2718(2) 0.0273(13) Uani 1 1 d . . . C15 C 0.0666(3) 0.1907(2) 0.2619(2) 0.0228(11) Uani 1 1 d . . . C16 C 0.1456(3) 0.2171(2) 0.2474(2) 0.0230(11) Uani 1 1 d . . . C17 C 0.1640(3) 0.2867(2) 0.2410(2) 0.0257(12) Uani 1 1 d . . . C18 C 0.2514(3) 0.2838(2) 0.2132(2) 0.0227(11) Uani 1 1 d . . . H18 H 0.2415 0.2783 0.1767 0.027 Uiso 1 1 calc R . . C19 C 0.2894(3) 0.2251(2) 0.2345(2) 0.0259(12) Uani 1 1 d . . . H19 H 0.3115 0.2340 0.2685 0.031 Uiso 1 1 calc R . . C20 C 0.3304(3) 0.1815(2) 0.1495(2) 0.0247(12) Uani 1 1 d . . . H20A H 0.3557 0.1459 0.1346 0.037 Uiso 1 1 calc R . . H20B H 0.3495 0.2175 0.1319 0.037 Uiso 1 1 calc R . . H20C H 0.2702 0.1786 0.1469 0.037 Uiso 1 1 calc R . . C21 C 0.4889(3) 0.2420(3) 0.1715(2) 0.0323(14) Uani 1 1 d . . . H21A H 0.4619 0.2814 0.1722 0.048 Uiso 1 1 calc R . . H21B H 0.4796 0.2231 0.1390 0.048 Uiso 1 1 calc R . . H21C H 0.5482 0.2470 0.1770 0.048 Uiso 1 1 calc R . . C22 C 0.4653(3) 0.2329(3) 0.2660(2) 0.0319(14) Uani 1 1 d . . . H22A H 0.4345 0.2713 0.2660 0.038 Uiso 1 1 calc R . . H22B H 0.4397 0.2068 0.2916 0.038 Uiso 1 1 calc R . . C23 C 0.5551(4) 0.2463(3) 0.2827(3) 0.0380(15) Uani 1 1 d . . . C24 C 0.5238(3) 0.1059(3) 0.1682(2) 0.0301(13) Uani 1 1 d . . . H24A H 0.5184 0.0619 0.1719 0.036 Uiso 1 1 calc R . . H24B H 0.4877 0.1184 0.1403 0.036 Uiso 1 1 calc R . . C25 C 0.6142(4) 0.1205(3) 0.1542(3) 0.0391(15) Uani 1 1 d . . . H25A H 0.6193 0.1641 0.1475 0.047 Uiso 1 1 calc R . . H25B H 0.6505 0.1107 0.1828 0.047 Uiso 1 1 calc R . . C26 C 0.6429(4) 0.0852(3) 0.1081(2) 0.0366(15) Uani 1 1 d . . . C27 C 0.5213(3) 0.0247(3) 0.2800(3) 0.0410(16) Uani 1 1 d . . . H27A H 0.5524 0.0613 0.2876 0.062 Uiso 1 1 calc R . . H27B H 0.5475 0.0036 0.2522 0.062 Uiso 1 1 calc R . . H27C H 0.5207 -0.0014 0.3094 0.062 Uiso 1 1 calc R . . C28 C 0.4376(3) -0.1021(3) 0.2846(3) 0.0347(14) Uani 1 1 d . . . H28A H 0.4867 -0.0924 0.3043 0.052 Uiso 1 1 calc R . . H28B H 0.4497 -0.0966 0.2491 0.052 Uiso 1 1 calc R . . H28C H 0.4216 -0.1439 0.2907 0.052 Uiso 1 1 calc R . . C29 C 0.3652(4) -0.0483(3) 0.3594(2) 0.0326(13) Uani 1 1 d . . . H29A H 0.4178 -0.0288 0.3689 0.039 Uiso 1 1 calc R . . H29B H 0.3198 -0.0205 0.3682 0.039 Uiso 1 1 calc R . . C30 C 0.3555(4) -0.1060(3) 0.3892(2) 0.0370(14) Uani 1 1 d . . . C31 C 0.0074(4) 0.0446(4) 0.3608(3) 0.054(2) Uani 1 1 d . . . H31A H 0.0384 0.0812 0.3685 0.082 Uiso 1 1 calc R . . H31B H 0.0344 0.0101 0.3765 0.082 Uiso 1 1 calc R . . H31C H -0.0490 0.0484 0.3737 0.082 Uiso 1 1 calc R . . C32 C 0.2002(4) -0.1635(3) 0.1598(3) 0.0539(19) Uani 1 1 d . . . C33 C 0.1946(4) -0.1339(3) 0.2098(3) 0.0480(18) Uani 1 1 d . . . H33A H 0.1640 -0.1606 0.2328 0.058 Uiso 1 1 calc R . . H33B H 0.1626 -0.0962 0.2065 0.058 Uiso 1 1 calc R . . C34 C 0.2803(3) -0.1189(3) 0.2333(3) 0.0339(14) Uani 1 1 d . . . H34A H 0.3108 -0.1570 0.2383 0.041 Uiso 1 1 calc R . . H34B H 0.3120 -0.0944 0.2092 0.041 Uiso 1 1 calc R . . C35 C -0.2148(3) 0.1050(3) 0.2621(3) 0.0416(17) Uani 1 1 d . . . C36 C -0.0115(4) 0.2307(3) 0.2682(3) 0.0371(15) Uani 1 1 d . . . H36A H -0.0547 0.2077 0.2852 0.056 Uiso 1 1 calc R . . H36B H -0.0314 0.2433 0.2354 0.056 Uiso 1 1 calc R . . H36C H 0.0025 0.2662 0.2881 0.056 Uiso 1 1 calc R . . C37 C 0.1725(4) 0.3130(3) 0.2949(2) 0.0380(15) Uani 1 1 d . . . H37A H 0.2137 0.2899 0.3135 0.057 Uiso 1 1 calc R . . H37B H 0.1192 0.3105 0.3120 0.057 Uiso 1 1 calc R . . H37C H 0.1899 0.3551 0.2930 0.057 Uiso 1 1 calc R . . C38 C 0.3091(3) 0.3399(2) 0.2208(2) 0.0293(13) Uani 1 1 d . . . H38A H 0.3132 0.3487 0.2569 0.035 Uiso 1 1 calc R . . H38B H 0.3651 0.3298 0.2087 0.035 Uiso 1 1 calc R . . C39 C 0.2790(3) 0.3970(3) 0.1934(2) 0.0297(13) Uani 1 1 d . . . C40 C 0.0991(3) 0.3247(2) 0.2111(2) 0.0283(13) Uani 1 1 d . . . H40A H 0.0492 0.3293 0.2320 0.034 Uiso 1 1 calc R . . H40B H 0.1223 0.3653 0.2057 0.034 Uiso 1 1 calc R . . C41 C 0.0726(4) 0.2991(3) 0.1602(2) 0.0373(15) Uani 1 1 d . . . H41A H 0.1187 0.3035 0.1363 0.045 Uiso 1 1 calc R . . H41B H 0.0609 0.2557 0.1639 0.045 Uiso 1 1 calc R . . C42 C -0.0040(3) 0.3303(3) 0.1390(2) 0.0341(13) Uani 1 1 d . . . C43 C -0.0638(4) 0.3919(3) 0.0692(2) 0.0382(15) Uani 1 1 d . . . H43A H -0.0430 0.4294 0.0538 0.046 Uiso 1 1 calc R . . H43B H -0.1075 0.4028 0.0933 0.046 Uiso 1 1 calc R . . C44 C -0.1013(4) 0.3502(3) 0.0275(2) 0.0321(13) Uani 1 1 d . . . H44 H -0.1272 0.3136 0.0423 0.039 Uiso 1 1 calc R . . C45 C -0.1627(4) 0.3845(3) -0.0048(3) 0.0398(15) Uani 1 1 d . . . H45A H -0.1334 0.4151 -0.0241 0.060 Uiso 1 1 calc R . . H45B H -0.2039 0.4038 0.0166 0.060 Uiso 1 1 calc R . . H45C H -0.1902 0.3565 -0.0276 0.060 Uiso 1 1 calc R . . C46 C 0.0052(3) 0.1674(3) 0.0350(2) 0.0281(12) Uani 1 1 d . . . H46 H -0.0114 0.1497 0.0023 0.034 Uiso 1 1 calc R . . C47 C 0.0929(3) 0.1445(3) 0.0487(2) 0.0296(13) Uani 1 1 d . . . H47 H 0.1281 0.1386 0.0185 0.036 Uiso 1 1 calc R . . C48 C 0.0709(3) 0.0840(3) 0.0742(2) 0.0310(13) Uani 1 1 d . . . H48A H 0.0661 0.0521 0.0480 0.037 Uiso 1 1 calc R . . C49 C -0.0517(4) 0.1430(3) 0.0759(2) 0.0344(14) Uani 1 1 d . . . H49 H -0.0608 0.1745 0.1019 0.041 Uiso 1 1 calc R . . C50 C -0.1363(4) 0.1196(3) 0.0565(3) 0.0482(18) Uani 1 1 d . . . H50A H -0.1684 0.1034 0.0848 0.058 Uiso 1 1 calc R . . H50B H -0.1677 0.1536 0.0421 0.058 Uiso 1 1 calc R . . C51 C 0.1395(3) 0.0896(2) 0.1579(2) 0.0287(13) Uani 1 1 d . . . C52 C 0.2514(3) 0.0346(2) 0.1457(2) 0.0233(11) Uani 1 1 d . . . C53 C 0.2033(3) 0.0297(2) 0.1025(2) 0.0259(12) Uani 1 1 d . . . C54 C 0.2277(4) -0.0045(3) 0.0611(2) 0.0339(14) Uani 1 1 d . . . H54 H 0.1931 -0.0080 0.0327 0.041 Uiso 1 1 calc R . . C55 C 0.3049(4) -0.0335(3) 0.0628(3) 0.0412(16) Uani 1 1 d . . . C56 C 0.3542(4) -0.0281(3) 0.1080(2) 0.0346(14) Uani 1 1 d . . . C57 C 0.3291(3) 0.0060(3) 0.1481(2) 0.0315(13) Uani 1 1 d . . . H57 H 0.3632 0.0103 0.1767 0.038 Uiso 1 1 calc R . . C58 C 0.4418(4) -0.0611(4) 0.1115(3) 0.056(2) Uani 1 1 d . . . H58A H 0.4791 -0.0445 0.0862 0.084 Uiso 1 1 calc R . . H58B H 0.4345 -0.1042 0.1056 0.084 Uiso 1 1 calc R . . H58C H 0.4655 -0.0548 0.1447 0.084 Uiso 1 1 calc R . . C59 C 0.3339(5) -0.0709(4) 0.0188(3) 0.069(2) Uani 1 1 d . . . H59A H 0.3835 -0.0528 0.0044 0.104 Uiso 1 1 calc R . . H59B H 0.2903 -0.0725 -0.0065 0.104 Uiso 1 1 calc R . . H59C H 0.3467 -0.1117 0.0302 0.104 Uiso 1 1 calc R . . C60 C -0.0679(3) 0.0922(3) 0.2265(2) 0.0332(14) Uani 1 1 d . . . H60A H -0.0643 0.1321 0.2104 0.040 Uiso 1 1 calc R . . H60B H -0.0364 0.0638 0.2055 0.040 Uiso 1 1 calc R . . C61 C -0.0474(4) -0.0227(3) 0.2912(4) 0.059(2) Uani 1 1 d . . . H61A H -0.0239 -0.0577 0.3083 0.088 Uiso 1 1 calc R . . H61B H -0.0454 -0.0291 0.2551 0.088 Uiso 1 1 calc R . . H61C H -0.1048 -0.0173 0.3017 0.088 Uiso 1 1 calc R . . C62 C -0.1599(4) 0.0723(3) 0.2260(3) 0.0435(17) Uani 1 1 d . . . H62A H -0.1820 0.0780 0.1919 0.052 Uiso 1 1 calc R . . H62B H -0.1625 0.0288 0.2336 0.052 Uiso 1 1 calc R . . C63 C 0.2681(4) 0.1248(3) 0.3199(2) 0.0314(13) Uani 1 1 d . A . C64 C -0.0547(6) -0.0659(4) 0.1157(4) 0.066(2) Uani 1 1 d . . . C65 C -0.1406(6) -0.0457(5) 0.1243(4) 0.092(3) Uani 1 1 d . . . H65A H -0.1788 -0.0777 0.1146 0.137 Uiso 1 1 calc R . . H65B H -0.1515 -0.0098 0.1044 0.137 Uiso 1 1 calc R . . H65C H -0.1482 -0.0364 0.1597 0.137 Uiso 1 1 calc R . . C66 C -0.0253(7) -0.0682(5) 0.0662(5) 0.103(4) Uani 1 1 d . . . H66A H -0.0348 -0.0294 0.0500 0.155 Uiso 1 1 calc R . . H66B H -0.0545 -0.0997 0.0479 0.155 Uiso 1 1 calc R . . H66C H 0.0340 -0.0770 0.0664 0.155 Uiso 1 1 calc R . . N1 N 0.3473(2) 0.12556(19) 0.23100(17) 0.0205(9) Uani 1 1 d . . . N2 N 0.2805(2) 0.02119(19) 0.26847(17) 0.0229(10) Uani 1 1 d . . . N3 N 0.1241(3) 0.08665(18) 0.27155(16) 0.0230(9) Uani 1 1 d . . . N4 N 0.2132(2) 0.18503(18) 0.24031(17) 0.0218(10) Uani 1 1 d . . . N5 N 0.2081(3) 0.07370(19) 0.18159(18) 0.0245(10) Uani 1 1 d . . . N6 N 0.1312(3) 0.06485(19) 0.11156(17) 0.0248(9) Uani 1 1 d . . . N7 N 0.2902(5) 0.1396(3) 0.3574(3) 0.0621(18) Uani 1 1 d . . . N8 N 0.1391(4) -0.1563(4) 0.1293(3) 0.085(3) Uani 1 1 d . . . H8A H 0.1417 -0.1714 0.0991 0.102 Uiso 1 1 calc R . . H8B H 0.0952 -0.1363 0.1387 0.102 Uiso 1 1 calc R . . N9 N 0.2836(3) 0.4483(2) 0.2196(2) 0.0372(13) Uani 1 1 d . . . H9A H 0.2717 0.4827 0.2053 0.045 Uiso 1 1 calc R . . H9B H 0.2984 0.4475 0.2511 0.045 Uiso 1 1 calc R . . N10 N 0.5609(3) 0.2817(3) 0.3234(2) 0.0513(15) Uani 1 1 d . . . H10A H 0.6094 0.2939 0.3338 0.062 Uiso 1 1 calc R . . H10B H 0.5161 0.2926 0.3394 0.062 Uiso 1 1 calc R . . N11 N 0.0056(3) 0.3609(2) 0.0961(2) 0.0380(13) Uani 1 1 d . . . N12 N 0.6317(3) 0.1107(3) 0.0633(2) 0.0459(14) Uani 1 1 d . . . H12A H 0.6458 0.0913 0.0361 0.055 Uiso 1 1 calc R . . H12B H 0.6102 0.1467 0.0612 0.055 Uiso 1 1 calc R . . N13 N -0.2254(3) 0.1645(2) 0.2539(3) 0.0486(14) Uani 1 1 d . . . H13A H -0.2557 0.1858 0.2745 0.058 Uiso 1 1 calc R . . H13B H -0.2021 0.1817 0.2281 0.058 Uiso 1 1 calc R . . N14 N 0.4261(3) -0.1339(2) 0.4045(2) 0.0441(14) Uani 1 1 d . . . H14A H 0.4233 -0.1680 0.4208 0.053 Uiso 1 1 calc R . . H14B H 0.4743 -0.1177 0.3981 0.053 Uiso 1 1 calc R . . O1 O -0.0293(2) 0.33389(18) -0.00489(15) 0.0302(9) Uani 1 1 d . . . O2 O -0.0942(2) 0.23855(19) -0.04555(16) 0.0369(10) Uani 1 1 d . . . O3 O 0.0616(3) 0.26298(19) -0.05348(16) 0.0373(10) Uani 1 1 d . . . O4 O -0.0017(2) 0.23228(17) 0.03215(15) 0.0318(9) Uani 1 1 d . . . O5 O -0.0073(2) 0.0915(2) 0.09783(16) 0.0382(10) Uani 1 1 d . . . O6 O 0.1322(2) 0.18362(17) 0.08522(15) 0.0318(9) Uani 1 1 d . . . H6 H 0.1433 0.2166 0.0719 0.048 Uiso 1 1 calc R . . O7 O -0.1266(3) 0.0722(2) 0.0181(2) 0.0659(15) Uani 1 1 d . . . H7 H -0.1693 0.0705 0.0006 0.099 Uiso 1 1 calc R . . O8 O 0.6733(4) 0.0341(2) 0.1124(2) 0.0707(17) Uani 1 1 d . . . O9 O -0.2474(4) 0.0783(2) 0.2991(2) 0.0656(15) Uani 1 1 d . . . O10 O 0.2854(3) -0.1274(2) 0.39761(19) 0.0474(12) Uani 1 1 d . . . O11 O 0.2642(4) -0.1929(4) 0.1453(3) 0.110(3) Uani 1 1 d . . . O12 O 0.2581(3) 0.3955(2) 0.14818(17) 0.0409(10) Uani 1 1 d . . . O13 O 0.6168(2) 0.2288(2) 0.2577(2) 0.0633(15) Uani 1 1 d . . . O14 O -0.0715(3) 0.3284(2) 0.16309(19) 0.0517(12) Uani 1 1 d . . . Re1 Re 0.37438(4) 0.16978(3) 0.42015(2) 0.0434(2) Uani 0.4647(14) 1 d PD A 1 O15 O 0.3875(8) 0.0434(6) 0.4570(4) 0.060(2) Uani 0.4647(14) 1 d PU A 1 O16 O 0.5379(8) 0.1426(6) 0.3627(4) 0.065(2) Uani 0.4647(14) 1 d PU A 1 O17 O 0.4651(9) 0.2070(6) 0.5173(4) 0.071(2) Uani 0.4647(14) 1 d PU A 1 O18 O 0.2575(7) 0.1892(8) 0.4513(5) 0.087(4) Uani 0.4647(14) 1 d PD A 1 H18A H 0.238(4) 0.171(5) 0.476(4) 0.130 Uiso 0.4647(14) 1 d PD A 1 H18B H 0.220(4) 0.208(7) 0.436(3) 0.130 Uiso 0.4647(14) 1 d PD A 1 C67 C 0.4316(12) 0.1935(8) 0.4817(6) 0.058(2) Uani 0.4647(14) 1 d PU A 1 C68 C 0.3728(11) 0.0884(8) 0.4481(5) 0.050(2) Uani 0.4647(14) 1 d PU A 1 C69 C 0.4775(12) 0.1545(8) 0.3843(6) 0.055(2) Uani 0.4647(14) 1 d PU A 1 Br1 Br 0.36545(12) 0.28341(8) 0.38521(7) 0.0607(5) Uani 0.4647(14) 1 d P A 1 O19 O 0.3962(8) 0.3354(6) 0.3706(6) 0.109(5) Uani 0.5353(14) 1 d P A 2 H19A H 0.3772 0.3036 0.3514 0.164 Uiso 0.5353(14) 1 d P A 2 H19B H 0.3976 0.3368 0.4072 0.164 Uiso 0.5353(14) 1 d P A 2 O71 O -0.1076(3) 0.1237(2) -0.0822(2) 0.0503(12) Uani 1 1 d D . . H71A H -0.152(3) 0.136(3) -0.094(3) 0.075 Uiso 1 1 d D . . H71B H -0.095(4) 0.091(2) -0.096(3) 0.075 Uiso 1 1 d D . . O72 O 0.3528(4) 0.4394(3) 0.3210(3) 0.0824(19) Uani 1 1 d D . . H72A H 0.377(7) 0.419(3) 0.343(3) 0.124 Uiso 1 1 d D . . H72B H 0.339(7) 0.417(3) 0.297(2) 0.124 Uiso 1 1 d D . . O73 O -0.1742(4) 0.2240(3) 0.1619(2) 0.0764(17) Uani 1 1 d D . . H73A H -0.209(5) 0.230(5) 0.184(2) 0.115 Uiso 1 1 d D . . H73B H -0.187(6) 0.244(4) 0.137(2) 0.115 Uiso 1 1 d D . . O74 O -0.3291(3) 0.1214(3) -0.0514(2) 0.0592(14) Uani 1 1 d D . . H74A H -0.312(6) 0.099(3) -0.074(2) 0.089 Uiso 1 1 d D . . H74B H -0.318(6) 0.1572(10) -0.058(3) 0.089 Uiso 1 1 d D . . O75 O 0.2269(3) 0.2463(2) -0.0736(2) 0.0538(12) Uani 1 1 d D . . H75A H 0.1798(18) 0.259(3) -0.067(3) 0.081 Uiso 1 1 d D . . H75B H 0.224(4) 0.2105(13) -0.083(3) 0.081 Uiso 1 1 d D . . O76 O 0.2357(3) 0.2620(2) 0.03188(18) 0.0458(11) Uani 1 1 d D . . H76A H 0.235(4) 0.261(4) 0.0007(2) 0.069 Uiso 1 1 d D . . H76B H 0.2831(18) 0.253(4) 0.042(2) 0.069 Uiso 1 1 d D . . O77 O -0.0103(5) -0.0782(4) 0.1518(3) 0.126(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0143(3) 0.0176(3) 0.0307(4) 0.0027(3) -0.0013(3) 0.0020(3) P1 0.0264(7) 0.0262(8) 0.0328(8) -0.0003(7) -0.0013(6) 0.0032(6) C1 0.013(2) 0.019(3) 0.041(3) -0.006(2) -0.002(2) 0.005(2) C2 0.011(2) 0.021(3) 0.036(3) -0.003(2) -0.003(2) -0.002(2) C3 0.015(3) 0.020(3) 0.038(3) 0.006(2) -0.007(2) -0.003(2) C4 0.018(2) 0.030(3) 0.027(3) -0.006(2) -0.001(2) 0.001(2) C5 0.018(2) 0.022(3) 0.039(3) 0.005(2) 0.000(2) 0.006(2) C6 0.018(3) 0.023(3) 0.031(3) -0.001(2) -0.005(2) 0.008(2) C7 0.017(3) 0.022(3) 0.042(3) 0.005(2) -0.004(2) 0.003(2) C8 0.024(3) 0.019(3) 0.036(3) 0.006(2) -0.004(2) 0.004(2) C9 0.019(3) 0.026(3) 0.027(3) 0.009(2) 0.001(2) 0.006(2) C10 0.022(3) 0.022(3) 0.050(4) 0.008(3) -0.002(3) -0.002(2) C11 0.027(3) 0.020(3) 0.033(3) 0.002(2) -0.006(2) -0.006(2) C12 0.022(3) 0.024(3) 0.059(4) 0.006(3) -0.002(3) 0.004(2) C13 0.021(3) 0.023(3) 0.050(4) 0.003(3) 0.008(3) -0.004(2) C14 0.018(3) 0.040(3) 0.024(3) 0.001(3) 0.000(2) 0.005(2) C15 0.015(2) 0.023(3) 0.030(3) 0.003(2) -0.001(2) -0.001(2) C16 0.027(3) 0.018(2) 0.024(3) 0.002(2) -0.013(2) 0.007(2) C17 0.023(3) 0.016(2) 0.038(3) -0.002(2) 0.000(2) 0.000(2) C18 0.016(2) 0.019(2) 0.033(3) 0.000(2) -0.005(2) -0.004(2) C19 0.016(2) 0.021(3) 0.041(3) 0.000(2) -0.004(2) -0.001(2) C20 0.014(2) 0.023(3) 0.037(3) 0.004(2) 0.002(2) 0.000(2) C21 0.019(3) 0.024(3) 0.054(4) 0.004(3) 0.001(3) 0.001(2) C22 0.022(3) 0.022(3) 0.052(4) -0.003(3) -0.008(3) 0.007(2) C23 0.022(3) 0.033(3) 0.059(4) -0.002(3) -0.008(3) 0.002(3) C24 0.021(3) 0.024(3) 0.045(4) 0.001(3) -0.002(2) 0.002(2) C25 0.023(3) 0.040(4) 0.054(4) 0.000(3) 0.001(3) -0.003(3) C26 0.027(3) 0.039(4) 0.044(4) 0.005(3) 0.010(3) 0.007(3) C27 0.014(3) 0.043(4) 0.066(5) 0.009(3) -0.001(3) 0.003(3) C28 0.022(3) 0.029(3) 0.053(4) 0.011(3) 0.003(3) 0.007(3) C29 0.027(3) 0.030(3) 0.041(3) -0.001(3) -0.005(3) 0.006(3) C30 0.035(3) 0.043(4) 0.033(3) -0.003(3) 0.004(3) 0.004(3) C31 0.041(4) 0.059(5) 0.064(5) 0.016(4) 0.022(4) 0.014(3) C32 0.042(4) 0.050(4) 0.069(5) -0.019(4) -0.017(4) 0.007(4) C33 0.023(3) 0.052(4) 0.069(5) -0.011(4) -0.005(3) -0.001(3) C34 0.023(3) 0.026(3) 0.053(4) 0.001(3) -0.010(3) 0.008(2) C35 0.019(3) 0.030(3) 0.076(5) 0.005(3) -0.004(3) -0.001(3) C36 0.027(3) 0.025(3) 0.060(4) 0.008(3) 0.000(3) 0.005(2) C37 0.034(3) 0.031(3) 0.049(4) -0.010(3) -0.005(3) -0.003(3) C38 0.030(3) 0.015(3) 0.043(3) -0.001(3) -0.003(3) 0.000(2) C39 0.018(3) 0.024(3) 0.047(4) 0.002(3) 0.007(2) -0.001(2) C40 0.016(2) 0.014(3) 0.055(4) 0.002(3) -0.002(2) 0.001(2) C41 0.030(3) 0.040(4) 0.042(4) 0.006(3) -0.001(3) 0.006(3) C42 0.025(3) 0.028(3) 0.049(4) 0.001(3) -0.004(3) 0.004(3) C43 0.038(3) 0.032(3) 0.045(4) -0.003(3) -0.008(3) 0.007(3) C44 0.031(3) 0.032(3) 0.034(3) -0.004(3) 0.003(2) 0.001(2) C45 0.042(4) 0.033(3) 0.044(4) 0.001(3) -0.004(3) 0.013(3) C46 0.030(3) 0.020(3) 0.034(3) -0.004(3) -0.006(2) 0.002(2) C47 0.022(3) 0.032(3) 0.035(3) -0.006(3) -0.002(2) 0.000(2) C48 0.023(3) 0.028(3) 0.042(4) -0.006(3) -0.006(3) 0.003(2) C49 0.028(3) 0.035(3) 0.040(4) 0.006(3) -0.004(3) 0.006(3) C50 0.027(3) 0.063(5) 0.055(4) 0.023(4) -0.002(3) -0.004(3) C51 0.021(3) 0.019(3) 0.046(4) 0.007(3) -0.003(2) -0.001(2) C52 0.020(3) 0.015(2) 0.035(3) 0.004(2) 0.002(2) 0.001(2) C53 0.023(3) 0.017(3) 0.038(3) 0.001(2) 0.003(2) -0.004(2) C54 0.035(3) 0.025(3) 0.041(3) -0.001(3) -0.010(3) -0.003(3) C55 0.048(4) 0.034(3) 0.042(4) -0.003(3) 0.010(3) 0.010(3) C56 0.032(3) 0.029(3) 0.043(4) -0.003(3) 0.002(3) 0.012(3) C57 0.027(3) 0.031(3) 0.036(3) 0.005(3) -0.003(3) 0.003(2) C58 0.033(4) 0.061(5) 0.074(5) -0.006(4) 0.006(4) 0.026(3) C59 0.065(5) 0.088(6) 0.054(5) -0.018(5) -0.009(4) 0.031(5) C60 0.022(3) 0.034(3) 0.044(4) 0.001(3) 0.007(3) 0.002(2) C61 0.022(3) 0.030(4) 0.125(7) 0.030(4) 0.002(4) 0.002(3) C62 0.028(3) 0.039(4) 0.063(5) 0.005(3) -0.009(3) -0.001(3) C63 0.030(3) 0.028(3) 0.037(4) 0.003(3) -0.003(3) 0.014(3) C64 0.060(5) 0.070(6) 0.069(6) -0.004(5) 0.020(5) 0.011(4) C65 0.076(6) 0.093(7) 0.106(8) 0.010(6) 0.010(6) 0.037(6) C66 0.074(7) 0.066(6) 0.170(13) 0.004(7) 0.000(8) 0.000(5) N1 0.0115(19) 0.019(2) 0.031(2) 0.0013(18) -0.0007(17) -0.0010(16) N2 0.018(2) 0.015(2) 0.035(3) 0.0034(19) -0.0025(19) 0.0047(17) N3 0.016(2) 0.020(2) 0.033(2) 0.0062(19) -0.0003(19) 0.0049(18) N4 0.0153(19) 0.017(2) 0.033(3) -0.0028(19) -0.0011(18) -0.0002(16) N5 0.016(2) 0.019(2) 0.039(3) 0.005(2) -0.0036(19) 0.0023(18) N6 0.024(2) 0.019(2) 0.031(2) 0.0007(19) -0.004(2) -0.0017(19) N7 0.083(5) 0.054(4) 0.049(4) -0.011(3) -0.019(4) 0.019(3) N8 0.057(4) 0.117(6) 0.081(5) -0.053(5) -0.029(4) 0.044(4) N9 0.034(3) 0.020(2) 0.058(4) -0.001(2) -0.001(2) 0.007(2) N10 0.032(3) 0.072(4) 0.050(4) -0.012(3) -0.009(3) -0.022(3) N11 0.035(3) 0.038(3) 0.041(3) -0.007(2) -0.012(2) 0.010(2) N12 0.039(3) 0.044(3) 0.055(4) 0.004(3) 0.006(3) 0.009(3) N13 0.024(2) 0.035(3) 0.087(4) 0.014(3) 0.006(3) 0.002(2) N14 0.036(3) 0.041(3) 0.056(4) 0.022(3) -0.002(3) 0.000(2) O1 0.0229(18) 0.026(2) 0.041(2) 0.0005(19) 0.0009(16) 0.0034(17) O2 0.033(2) 0.034(2) 0.044(3) 0.001(2) -0.0073(19) 0.0022(18) O3 0.032(2) 0.039(2) 0.041(2) -0.006(2) 0.0022(19) -0.0008(19) O4 0.039(2) 0.021(2) 0.035(2) 0.0005(17) -0.0069(18) -0.0003(17) O5 0.0199(19) 0.049(3) 0.045(3) 0.013(2) -0.0028(17) 0.0001(19) O6 0.0277(19) 0.031(2) 0.037(2) 0.0034(17) -0.0115(18) -0.0066(18) O7 0.063(3) 0.056(3) 0.078(4) 0.004(3) -0.021(3) -0.015(3) O8 0.090(4) 0.051(3) 0.072(4) 0.021(3) 0.037(3) 0.039(3) O9 0.071(4) 0.035(3) 0.091(4) 0.004(3) 0.033(3) -0.001(3) O10 0.030(2) 0.053(3) 0.060(3) 0.022(2) 0.004(2) 0.004(2) O11 0.077(4) 0.151(7) 0.101(5) -0.074(5) -0.053(4) 0.077(5) O12 0.035(2) 0.046(2) 0.042(3) 0.006(2) 0.002(2) 0.005(2) O13 0.016(2) 0.055(3) 0.119(5) -0.027(3) -0.019(3) 0.005(2) O14 0.024(2) 0.065(3) 0.066(3) 0.014(3) -0.001(2) 0.010(2) Re1 0.0563(4) 0.0458(4) 0.0282(3) 0.0000(3) -0.0131(3) -0.0088(3) O15 0.079(5) 0.076(5) 0.025(4) -0.006(4) -0.005(4) -0.007(5) O16 0.080(5) 0.068(5) 0.047(4) 0.007(4) -0.007(4) 0.002(5) O17 0.099(5) 0.075(5) 0.040(4) 0.001(4) -0.020(4) 0.004(5) O18 0.043(6) 0.151(15) 0.066(8) -0.007(8) 0.007(6) -0.001(8) C67 0.082(5) 0.061(5) 0.031(4) -0.001(4) -0.014(4) -0.002(4) C68 0.076(5) 0.051(5) 0.022(4) 0.002(4) -0.013(4) -0.001(4) C69 0.079(5) 0.059(5) 0.027(4) 0.000(4) -0.009(4) -0.002(4) Br1 0.0631(10) 0.0579(11) 0.0611(10) 0.0007(8) -0.0020(9) -0.0042(9) O19 0.093(9) 0.070(8) 0.165(14) -0.040(9) 0.031(9) -0.012(7) O71 0.037(3) 0.051(3) 0.063(3) -0.012(3) -0.011(2) 0.004(2) O72 0.079(4) 0.085(4) 0.084(5) -0.049(4) -0.019(4) 0.000(4) O73 0.066(4) 0.099(5) 0.064(4) 0.023(4) -0.008(3) -0.008(3) O74 0.047(3) 0.065(3) 0.065(4) -0.006(3) -0.002(3) -0.005(3) O75 0.042(3) 0.052(3) 0.067(3) -0.011(3) 0.001(3) -0.002(2) O76 0.037(2) 0.056(3) 0.045(3) 0.003(2) 0.001(2) -0.008(2) O77 0.093(5) 0.163(8) 0.123(7) -0.026(6) -0.028(5) 0.058(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.884(4) . ? Co1 C63 1.888(7) . ? Co1 N4 1.893(4) . ? Co1 N3 1.920(4) . ? Co1 N2 1.921(4) . ? Co1 N5 2.030(5) . ? P1 O2 1.488(4) . ? P1 O3 1.494(4) . ? P1 O1 1.592(4) . ? P1 O4 1.608(4) . ? C1 N1 1.477(7) . ? C1 C20 1.533(8) . ? C1 C19 1.553(7) . ? C1 C2 1.588(7) . ? C2 C21 1.518(8) . ? C2 C22 1.559(8) . ? C2 C3 1.564(7) . ? C3 C4 1.512(7) . ? C3 C24 1.531(8) . ? C3 H3 0.9800 . ? C4 N1 1.301(6) . ? C4 C5 1.456(8) . ? C5 C6 1.370(8) . ? C5 C27 1.538(7) . ? C6 N2 1.364(6) . ? C6 C7 1.542(7) . ? C7 C28 1.542(7) . ? C7 C8 1.557(7) . ? C7 C29 1.577(8) . ? C8 C34 1.517(8) . ? C8 C9 1.524(7) . ? C8 H8 0.9800 . ? C9 N2 1.317(7) . ? C9 C10 1.397(7) . ? C10 C11 1.378(8) . ? C10 H10 0.9300 . ? C11 N3 1.337(7) . ? C11 C12 1.532(8) . ? C12 C31 1.473(10) . ? C12 C13 1.554(8) . ? C12 C61 1.564(9) . ? C13 C14 1.518(8) . ? C13 C60 1.558(9) . ? C13 H13 0.9800 . ? C14 C15 1.367(8) . ? C14 N3 1.386(7) . ? C15 C16 1.432(7) . ? C15 C36 1.526(7) . ? C16 N4 1.295(6) . ? C16 C17 1.555(7) . ? C17 C37 1.535(8) . ? C17 C40 1.539(7) . ? C17 C18 1.569(7) . ? C18 C19 1.524(7) . ? C18 C38 1.543(7) . ? C18 H18 0.9800 . ? C19 N4 1.502(6) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.520(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O13 1.239(8) . ? C23 N10 1.323(8) . ? C24 C25 1.516(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.507(9) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O8 1.220(7) . ? C26 N12 1.313(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.492(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O10 1.227(7) . ? C30 N14 1.338(8) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 O11 1.262(9) . ? C32 N8 1.269(9) . ? C32 C33 1.467(10) . ? C33 C34 1.529(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 O9 1.246(8) . ? C35 N13 1.325(8) . ? C35 C62 1.472(10) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.514(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 O12 1.235(7) . ? C39 N9 1.318(8) . ? C40 C41 1.510(8) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.500(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O14 1.247(7) . ? C42 N11 1.319(8) . ? C43 N11 1.474(7) . ? C43 C44 1.544(8) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O1 1.469(7) . ? C44 C45 1.493(8) . ? C44 H44 0.9800 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 O4 1.422(7) . ? C46 C49 1.501(8) . ? C46 C47 1.522(7) . ? C46 H46 0.9800 . ? C47 O6 1.428(7) . ? C47 C48 1.521(8) . ? C47 H47 0.9800 . ? C48 O5 1.398(7) . ? C48 N6 1.434(7) . ? C48 H48A 0.9800 . ? C49 O5 1.447(7) . ? C49 C50 1.524(8) . ? C49 H49 0.9800 . ? C50 O7 1.454(9) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 N5 1.302(7) . ? C51 N6 1.339(7) . ? C52 C53 1.372(8) . ? C52 C57 1.384(7) . ? C52 N5 1.446(7) . ? C53 C54 1.375(8) . ? C53 N6 1.399(7) . ? C54 C55 1.380(9) . ? C54 H54 0.9300 . ? C55 C56 1.429(9) . ? C55 C59 1.488(10) . ? C56 C57 1.350(8) . ? C56 C58 1.570(8) . ? C57 H57 0.9300 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C62 1.524(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 N7 1.097(8) . ? C64 O77 1.211(11) . ? C64 C66 1.384(14) . ? C64 C65 1.451(12) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? N7 Re1 2.221(7) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? N9 H9A 0.8600 . ? N9 H9B 0.8600 . ? N10 H10A 0.8600 . ? N10 H10B 0.8600 . ? N12 H12A 0.8600 . ? N12 H12B 0.8600 . ? N13 H13A 0.8600 . ? N13 H13B 0.8600 . ? N14 H14A 0.8600 . ? N14 H14B 0.8600 . ? O6 H6 0.8200 . ? O7 H7 0.8200 . ? Re1 C69 1.919(19) . ? Re1 C68 1.922(16) . ? Re1 C67 1.926(16) . ? Re1 O18 2.072(12) . ? Re1 Br1 2.6482(19) . ? O15 C68 1.037(17) . ? O16 C69 1.143(19) . ? O17 C67 1.116(17) . ? O18 H18A 0.820(2) . ? O18 H18B 0.820(2) . ? Br1 H19A 1.0091(18) . ? Br1 H19B 1.3977(18) . ? O19 H19A 0.910(13) . ? O19 H19B 0.964(16) . ? O71 H71A 0.82(5) . ? O71 H71B 0.83(5) . ? O72 H72A 0.83(9) . ? O72 H72B 0.83(6) . ? O73 H73A 0.81(7) . ? O73 H73B 0.81(7) . ? O74 H74A 0.82(6) . ? O74 H74B 0.82(4) . ? O75 H75A 0.82(4) . ? O75 H75B 0.82(3) . ? O76 H76A 0.820(8) . ? O76 H76B 0.82(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 C63 89.3(2) . . ? N1 Co1 N4 83.13(17) . . ? C63 Co1 N4 87.6(2) . . ? N1 Co1 N3 173.01(17) . . ? C63 Co1 N3 92.2(2) . . ? N4 Co1 N3 90.13(17) . . ? N1 Co1 N2 90.30(18) . . ? C63 Co1 N2 87.8(2) . . ? N4 Co1 N2 172.04(17) . . ? N3 Co1 N2 96.56(17) . . ? N1 Co1 N5 91.31(18) . . ? C63 Co1 N5 177.9(2) . . ? N4 Co1 N5 94.38(18) . . ? N3 Co1 N5 87.37(18) . . ? N2 Co1 N5 90.24(18) . . ? O2 P1 O3 116.8(2) . . ? O2 P1 O1 112.1(2) . . ? O3 P1 O1 106.4(2) . . ? O2 P1 O4 108.9(2) . . ? O3 P1 O4 110.8(2) . . ? O1 P1 O4 100.6(2) . . ? N1 C1 C20 110.9(4) . . ? N1 C1 C19 102.3(4) . . ? C20 C1 C19 109.0(4) . . ? N1 C1 C2 103.2(4) . . ? C20 C1 C2 112.6(4) . . ? C19 C1 C2 118.1(4) . . ? C21 C2 C22 109.9(4) . . ? C21 C2 C3 114.8(4) . . ? C22 C2 C3 106.5(4) . . ? C21 C2 C1 114.2(5) . . ? C22 C2 C1 109.5(4) . . ? C3 C2 C1 101.4(4) . . ? C4 C3 C24 109.9(4) . . ? C4 C3 C2 101.5(4) . . ? C24 C3 C2 118.4(5) . . ? C4 C3 H3 108.9 . . ? C24 C3 H3 108.9 . . ? C2 C3 H3 108.9 . . ? N1 C4 C5 123.7(5) . . ? N1 C4 C3 112.5(5) . . ? C5 C4 C3 123.7(4) . . ? C6 C5 C4 121.0(4) . . ? C6 C5 C27 123.2(5) . . ? C4 C5 C27 115.9(5) . . ? N2 C6 C5 124.9(5) . . ? N2 C6 C7 108.3(4) . . ? C5 C6 C7 126.7(5) . . ? C6 C7 C28 117.3(5) . . ? C6 C7 C8 101.3(4) . . ? C28 C7 C8 112.1(4) . . ? C6 C7 C29 105.6(4) . . ? C28 C7 C29 110.5(5) . . ? C8 C7 C29 109.5(5) . . ? C34 C8 C9 112.0(4) . . ? C34 C8 C7 113.0(5) . . ? C9 C8 C7 98.6(4) . . ? C34 C8 H8 110.9 . . ? C9 C8 H8 110.9 . . ? C7 C8 H8 110.9 . . ? N2 C9 C10 126.6(5) . . ? N2 C9 C8 111.6(4) . . ? C10 C9 C8 121.7(5) . . ? C11 C10 C9 125.5(5) . . ? C11 C10 H10 117.3 . . ? C9 C10 H10 117.3 . . ? N3 C11 C10 125.1(5) . . ? N3 C11 C12 111.1(5) . . ? C10 C11 C12 123.4(5) . . ? C31 C12 C11 108.5(5) . . ? C31 C12 C13 109.4(5) . . ? C11 C12 C13 99.9(5) . . ? C31 C12 C61 110.9(6) . . ? C11 C12 C61 111.6(5) . . ? C13 C12 C61 115.9(5) . . ? C14 C13 C12 102.2(4) . . ? C14 C13 C60 107.8(5) . . ? C12 C13 C60 118.3(5) . . ? C14 C13 H13 109.4 . . ? C12 C13 H13 109.4 . . ? C60 C13 H13 109.4 . . ? C15 C14 N3 126.7(5) . . ? C15 C14 C13 124.2(5) . . ? N3 C14 C13 108.8(5) . . ? C14 C15 C16 121.1(5) . . ? C14 C15 C36 118.2(5) . . ? C16 C15 C36 120.7(4) . . ? N4 C16 C15 123.1(4) . . ? N4 C16 C17 110.9(4) . . ? C15 C16 C17 125.9(4) . . ? C37 C17 C40 109.2(4) . . ? C37 C17 C16 106.4(5) . . ? C40 C17 C16 117.1(4) . . ? C37 C17 C18 111.5(4) . . ? C40 C17 C18 112.1(4) . . ? C16 C17 C18 100.3(4) . . ? C19 C18 C38 112.6(4) . . ? C19 C18 C17 102.3(4) . . ? C38 C18 C17 115.8(4) . . ? C19 C18 H18 108.6 . . ? C38 C18 H18 108.6 . . ? C17 C18 H18 108.6 . . ? N4 C19 C18 102.0(4) . . ? N4 C19 C1 105.8(4) . . ? C18 C19 C1 123.7(5) . . ? N4 C19 H19 108.1 . . ? C18 C19 H19 108.1 . . ? C1 C19 H19 108.1 . . ? C1 C20 H20A 109.5 . . ? C1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C2 117.7(5) . . ? C23 C22 H22A 107.9 . . ? C2 C22 H22A 107.9 . . ? C23 C22 H22B 107.9 . . ? C2 C22 H22B 107.9 . . ? H22A C22 H22B 107.2 . . ? O13 C23 N10 123.6(6) . . ? O13 C23 C22 122.0(6) . . ? N10 C23 C22 114.2(5) . . ? C25 C24 C3 115.0(5) . . ? C25 C24 H24A 108.5 . . ? C3 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? C3 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C26 C25 C24 112.0(5) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? O8 C26 N12 121.5(6) . . ? O8 C26 C25 120.9(6) . . ? N12 C26 C25 117.6(5) . . ? C5 C27 H27A 109.5 . . ? C5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C7 C28 H28A 109.5 . . ? C7 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C7 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C7 112.9(5) . . ? C30 C29 H29A 109.0 . . ? C7 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C7 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? O10 C30 N14 122.2(6) . . ? O10 C30 C29 120.7(6) . . ? N14 C30 C29 117.1(5) . . ? C12 C31 H31A 109.5 . . ? C12 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C12 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O11 C32 N8 119.2(7) . . ? O11 C32 C33 122.9(6) . . ? N8 C32 C33 117.8(6) . . ? C32 C33 C34 113.6(5) . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C8 C34 C33 115.4(5) . . ? C8 C34 H34A 108.4 . . ? C33 C34 H34A 108.4 . . ? C8 C34 H34B 108.4 . . ? C33 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? O9 C35 N13 122.1(6) . . ? O9 C35 C62 121.4(6) . . ? N13 C35 C62 116.5(6) . . ? C15 C36 H36A 109.5 . . ? C15 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C15 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C17 C37 H37A 109.5 . . ? C17 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C17 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C18 113.8(5) . . ? C39 C38 H38A 108.8 . . ? C18 C38 H38A 108.8 . . ? C39 C38 H38B 108.8 . . ? C18 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? O12 C39 N9 122.7(6) . . ? O12 C39 C38 121.4(5) . . ? N9 C39 C38 115.7(5) . . ? C41 C40 C17 116.1(5) . . ? C41 C40 H40A 108.3 . . ? C17 C40 H40A 108.3 . . ? C41 C40 H40B 108.3 . . ? C17 C40 H40B 108.3 . . ? H40A C40 H40B 107.4 . . ? C42 C41 C40 112.8(5) . . ? C42 C41 H41A 109.0 . . ? C40 C41 H41A 109.0 . . ? C42 C41 H41B 109.0 . . ? C40 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? O14 C42 N11 123.4(5) . . ? O14 C42 C41 119.6(6) . . ? N11 C42 C41 117.0(5) . . ? N11 C43 C44 110.9(5) . . ? N11 C43 H43A 109.5 . . ? C44 C43 H43A 109.5 . . ? N11 C43 H43B 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 108.0 . . ? O1 C44 C45 107.5(5) . . ? O1 C44 C43 104.7(4) . . ? C45 C44 C43 111.1(5) . . ? O1 C44 H44 111.1 . . ? C45 C44 H44 111.1 . . ? C43 C44 H44 111.1 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O4 C46 C49 110.2(5) . . ? O4 C46 C47 114.2(4) . . ? C49 C46 C47 105.4(5) . . ? O4 C46 H46 109.0 . . ? C49 C46 H46 109.0 . . ? C47 C46 H46 109.0 . . ? O6 C47 C48 108.9(5) . . ? O6 C47 C46 111.3(5) . . ? C48 C47 C46 100.3(4) . . ? O6 C47 H47 111.9 . . ? C48 C47 H47 111.9 . . ? C46 C47 H47 111.9 . . ? O5 C48 N6 108.8(5) . . ? O5 C48 C47 107.3(4) . . ? N6 C48 C47 113.7(4) . . ? O5 C48 H48A 109.0 . . ? N6 C48 H48A 109.0 . . ? C47 C48 H48A 109.0 . . ? O5 C49 C46 105.5(4) . . ? O5 C49 C50 107.6(5) . . ? C46 C49 C50 114.2(5) . . ? O5 C49 H49 109.8 . . ? C46 C49 H49 109.8 . . ? C50 C49 H49 109.8 . . ? O7 C50 C49 112.2(5) . . ? O7 C50 H50A 109.2 . . ? C49 C50 H50A 109.2 . . ? O7 C50 H50B 109.2 . . ? C49 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? N5 C51 N6 114.2(5) . . ? C53 C52 C57 119.9(5) . . ? C53 C52 N5 108.8(4) . . ? C57 C52 N5 131.2(5) . . ? C52 C53 C54 122.6(5) . . ? C52 C53 N6 105.7(5) . . ? C54 C53 N6 131.6(5) . . ? C53 C54 C55 118.3(6) . . ? C53 C54 H54 120.8 . . ? C55 C54 H54 120.8 . . ? C54 C55 C56 118.4(6) . . ? C54 C55 C59 120.1(6) . . ? C56 C55 C59 121.5(6) . . ? C57 C56 C55 122.2(5) . . ? C57 C56 C58 118.1(6) . . ? C55 C56 C58 119.7(6) . . ? C56 C57 C52 118.5(6) . . ? C56 C57 H57 120.8 . . ? C52 C57 H57 120.8 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C55 C59 H59A 109.5 . . ? C55 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C55 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C62 C60 C13 117.2(5) . . ? C62 C60 H60A 108.0 . . ? C13 C60 H60A 108.0 . . ? C62 C60 H60B 108.0 . . ? C13 C60 H60B 108.0 . . ? H60A C60 H60B 107.2 . . ? C12 C61 H61A 109.5 . . ? C12 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C12 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C35 C62 C60 115.1(6) . . ? C35 C62 H62A 108.5 . . ? C60 C62 H62A 108.5 . . ? C35 C62 H62B 108.5 . . ? C60 C62 H62B 108.5 . . ? H62A C62 H62B 107.5 . . ? N7 C63 Co1 175.0(7) . . ? O77 C64 C66 122.0(9) . . ? O77 C64 C65 119.6(9) . . ? C66 C64 C65 118.3(10) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C4 N1 C1 112.2(4) . . ? C4 N1 Co1 129.8(4) . . ? C1 N1 Co1 117.6(3) . . ? C9 N2 C6 111.0(4) . . ? C9 N2 Co1 122.1(3) . . ? C6 N2 Co1 126.4(3) . . ? C11 N3 C14 110.6(4) . . ? C11 N3 Co1 123.3(3) . . ? C14 N3 Co1 126.1(4) . . ? C16 N4 C19 111.6(4) . . ? C16 N4 Co1 132.4(4) . . ? C19 N4 Co1 113.7(3) . . ? C51 N5 C52 104.1(5) . . ? C51 N5 Co1 124.2(4) . . ? C52 N5 Co1 131.7(3) . . ? C51 N6 C53 107.2(4) . . ? C51 N6 C48 124.9(5) . . ? C53 N6 C48 126.1(5) . . ? C63 N7 Re1 161.4(7) . . ? C32 N8 H8A 120.0 . . ? C32 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? C39 N9 H9A 120.0 . . ? C39 N9 H9B 120.0 . . ? H9A N9 H9B 120.0 . . ? C23 N10 H10A 120.0 . . ? C23 N10 H10B 120.0 . . ? H10A N10 H10B 120.0 . . ? C42 N11 C43 123.8(5) . . ? C26 N12 H12A 120.0 . . ? C26 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? C35 N13 H13A 120.0 . . ? C35 N13 H13B 120.0 . . ? H13A N13 H13B 120.0 . . ? C30 N14 H14A 120.0 . . ? C30 N14 H14B 120.0 . . ? H14A N14 H14B 120.0 . . ? C44 O1 P1 119.5(3) . . ? C46 O4 P1 119.7(3) . . ? C48 O5 C49 110.3(4) . . ? C47 O6 H6 109.5 . . ? C50 O7 H7 109.5 . . ? C69 Re1 C68 92.2(7) . . ? C69 Re1 C67 93.2(7) . . ? C68 Re1 C67 86.2(7) . . ? C69 Re1 O18 173.7(6) . . ? C68 Re1 O18 91.5(7) . . ? C67 Re1 O18 92.1(7) . . ? C69 Re1 N7 95.6(5) . . ? C68 Re1 N7 90.1(5) . . ? C67 Re1 N7 170.5(6) . . ? O18 Re1 N7 79.3(4) . . ? C69 Re1 Br1 92.2(5) . . ? C68 Re1 Br1 175.6(5) . . ? C67 Re1 Br1 93.7(5) . . ? O18 Re1 Br1 84.1(4) . . ? N7 Re1 Br1 89.32(18) . . ? Re1 O18 H18A 123.9(13) . . ? Re1 O18 H18B 123.9(13) . . ? H18A O18 H18B 109.6(6) . . ? O17 C67 Re1 179.7(19) . . ? O15 C68 Re1 163.6(17) . . ? O16 C69 Re1 176.8(15) . . ? Re1 Br1 H19A 134.77(13) . . ? Re1 Br1 H19B 128.15(10) . . ? H19A Br1 H19B 86.16(12) . . ? H19A O19 H19B 125.8(16) . . ? H71A O71 H71B 109(7) . . ? H72A O72 H72B 110(7) . . ? H73A O73 H73B 109(9) . . ? H74A O74 H74B 110(7) . . ? H75A O75 H75B 110(6) . . ? H76A O76 H76B 109(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.140 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.112 #===END