# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H92 Co N14 O34 P' _chemical_formula_weight 1763.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 12.8063(3) _cell_length_b 22.7406(6) _cell_length_c 29.1298(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8483.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 67.29 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 2.565 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5337 _exptl_absorpt_correction_T_max 0.7656 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44953 _diffrn_reflns_av_unetI/netI 0.0457 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 66.60 _reflns_number_total 14578 _reflns_number_gt 13951 _reflns_threshold_expression 'I > 2\s(I)' _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.0915P)^2^+9.4492P] 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 x determined using 5804 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.0223(15) _chemical_absolute_configuration syn _refine_ls_number_reflns 14578 _refine_ls_number_parameters 1062 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C30 C 0.6535(4) 0.7480(2) 0.17665(15) 0.0143(9) Uani 1 1 d . . . . . H30A H 0.6005 0.7594 0.1536 0.017 Uiso 1 1 calc R U . . . H30B H 0.6704 0.7833 0.1951 0.017 Uiso 1 1 calc R U . . . Co1 Co 0.34589(5) 0.74574(3) 0.28751(2) 0.00767(16) Uani 1 1 d . . . . . P1 P 0.66093(9) 1.03567(5) 0.44567(4) 0.0124(2) Uani 1 1 d . . . . . O10W O 0.2723(3) 0.36879(15) 0.10695(12) 0.0196(7) Uani 1 1 d . . . . . O10L O 0.1705(4) 0.34775(17) 0.25937(16) 0.0354(10) Uani 1 1 d . . . . . O9W O 0.8464(3) 0.56951(15) 0.13513(12) 0.0207(7) Uani 1 1 d . . . . . O11L O 0.0812(4) 0.36435(18) 0.32080(17) 0.0408(11) Uani 1 1 d . . . . . O28 O 0.7098(3) 0.58176(14) 0.20544(11) 0.0162(7) Uani 1 1 d . . . . . O1W O 0.4999(3) 0.94220(17) 0.58687(14) 0.0285(9) Uani 1 1 d . . . . . O51 O 0.1205(3) 0.91520(16) 0.48896(12) 0.0230(8) Uani 1 1 d . . . . . O7W O 0.7927(3) 0.54529(17) 0.37351(14) 0.0309(9) Uani 1 1 d . . . . . O58 O 0.5309(3) 0.84127(16) 0.53248(12) 0.0190(7) Uani 1 1 d . . . . . O3W O 0.8494(3) 0.95786(17) 0.37209(15) 0.0333(9) Uani 1 1 d . . . . . OP3 O 0.7340(2) 0.99365(14) 0.47472(11) 0.0142(7) Uani 1 1 d . . . . . O4W O 0.1136(4) 0.94150(18) 0.24113(14) 0.0332(10) Uani 1 1 d . . . . . O2W O 0.1532(4) 0.9880(2) 0.56082(14) 0.0444(12) Uani 1 1 d . . . . . OP2 O 0.5587(3) 0.99469(15) 0.44237(11) 0.0163(7) Uani 1 1 d . . . . . OR7 O 0.5373(3) 0.91460(15) 0.36801(12) 0.0185(7) Uani 1 1 d . . . . . H207 H 0.5972 0.9128 0.3796 0.028 Uiso 1 1 calc R U . . . O11W O -0.0185(5) 0.0806(3) 0.4917(2) 0.0583(14) Uani 1 1 d . . . . . OR6 O 0.3278(2) 0.96738(14) 0.37687(11) 0.0143(7) Uani 1 1 d . . . . . O8W O 0.9705(4) 0.4750(3) 0.17169(19) 0.0570(16) Uani 1 1 d . . . . . OR8 O 0.2885(3) 1.06681(16) 0.43770(13) 0.0243(8) Uani 1 1 d . . . . . H208 H 0.2586 1.0657 0.4120 0.036 Uiso 1 1 calc R U . . . O15W O 0.9625(5) 0.2453(3) 0.4856(2) 0.0659(16) Uani 1 1 d . . . . . OP4 O 0.6356(3) 1.09026(15) 0.47121(13) 0.0233(8) Uani 1 1 d . . . . . OP5 O 0.7098(3) 1.04195(15) 0.39968(11) 0.0166(7) Uani 1 1 d . . . . . O62 O 0.7831(3) 0.75642(15) 0.42244(12) 0.0199(7) Uani 1 1 d . . . . . O44 O 0.1080(3) 0.94221(15) 0.14453(12) 0.0212(8) Uani 1 1 d . . . . . O39 O -0.0100(3) 0.66075(15) 0.14265(13) 0.0206(8) Uani 1 1 d . . . . . N9L N 0.1385(4) 0.38084(18) 0.28974(17) 0.0244(10) Uani 1 1 d . . . . . N24 N 0.4269(3) 0.73756(16) 0.34117(13) 0.0096(7) Uani 1 1 d . . . . . N21 N 0.4736(3) 0.73076(15) 0.25787(12) 0.0092(7) Uani 1 1 d . . . . . N22 N 0.2763(3) 0.74540(16) 0.22945(13) 0.0106(7) Uani 1 1 d . . . . . C9 C 0.1762(3) 0.76204(19) 0.22457(15) 0.0106(9) Uani 1 1 d . . . . . N23 N 0.2251(3) 0.76173(16) 0.32380(13) 0.0108(7) Uani 1 1 d . . . . . N59 N 0.6576(3) 0.87789(17) 0.48627(13) 0.0143(8) Uani 1 1 d . . . . . H59 H 0.6809 0.8798 0.4579 0.017 Uiso 1 1 calc R U . . . NB1 N 0.3845(3) 0.92718(16) 0.30784(13) 0.0111(8) Uani 1 1 d . . . . . NB3 N 0.3679(3) 0.83518(17) 0.28242(13) 0.0111(7) Uani 1 1 d . . . . . B5 C 0.4681(4) 0.9009(2) 0.17253(16) 0.0158(9) Uani 1 1 d . . . . . B6 C 0.4816(4) 0.9587(2) 0.18933(16) 0.0137(9) Uani 1 1 d . . . . . N63 N 0.8151(3) 0.66281(18) 0.44218(15) 0.0187(9) Uani 1 1 d . . . . . H63A H 0.8664 0.6732 0.4606 0.022 Uiso 1 1 calc R U . . . H63B H 0.7986 0.6255 0.4391 0.022 Uiso 1 1 calc R U . . . O33 O 0.7263(4) 0.8053(2) 0.09730(16) 0.0488(14) Uani 1 1 d . . . . . C1L C 0.3134(3) 0.6658(2) 0.29028(16) 0.0130(9) Uani 1 1 d . . . . . C2L C 0.2820(4) 0.6156(2) 0.28933(16) 0.0153(9) Uani 1 1 d . . . . . C3L C 0.2427(4) 0.5571(2) 0.28822(17) 0.0157(9) Uani 1 1 d . . . . . C4L C 0.1730(4) 0.5374(2) 0.32216(18) 0.0217(11) Uani 1 1 d . . . . . H4L H 0.1492 0.5640 0.3450 0.026 Uiso 1 1 calc R U . . . C5L C 0.1386(4) 0.4800(2) 0.32288(19) 0.0225(11) Uani 1 1 d . . . . . H5L H 0.0925 0.4666 0.3462 0.027 Uiso 1 1 calc R U . . . C6L C 0.1733(4) 0.4421(2) 0.28857(18) 0.0183(10) Uani 1 1 d . . . . . C7L C 0.2383(4) 0.4599(2) 0.25372(19) 0.0235(11) Uani 1 1 d . . . . . H7L H 0.2592 0.4332 0.2304 0.028 Uiso 1 1 calc R U . . . C8L C 0.2727(4) 0.5178(2) 0.25337(18) 0.0216(11) Uani 1 1 d . . . . . H8L H 0.3169 0.5310 0.2293 0.026 Uiso 1 1 calc R U . . . C19 C 0.5298(3) 0.70949(19) 0.33307(15) 0.0105(9) Uani 1 1 d . . . . . H19 H 0.5189 0.6661 0.3300 0.013 Uiso 1 1 calc R U . . . C1 C 0.5704(3) 0.73342(19) 0.28676(15) 0.0098(8) Uani 1 1 d . . . . . C20 C 0.6075(3) 0.79692(19) 0.29228(15) 0.0112(9) Uani 1 1 d . . . . . H20A H 0.6178 0.8145 0.2619 0.017 Uiso 1 1 calc R U . . . H20B H 0.6736 0.7975 0.3092 0.017 Uiso 1 1 calc R U . . . H20C H 0.5549 0.8195 0.3092 0.017 Uiso 1 1 calc R U . . . C2 C 0.6487(3) 0.69361(18) 0.25856(15) 0.0098(8) Uani 1 1 d . . . . . C26 C 0.6357(3) 0.62797(19) 0.27241(15) 0.0109(9) Uani 1 1 d . . . . . H26A H 0.6465 0.6243 0.3059 0.013 Uiso 1 1 calc R U . . . H26B H 0.5632 0.6155 0.2656 0.013 Uiso 1 1 calc R U . . . C27 C 0.7102(4) 0.5869(2) 0.24807(17) 0.0154(9) Uani 1 1 d . . . . . N29 N 0.7739(4) 0.5565(2) 0.27463(15) 0.0230(9) Uani 1 1 d . . . . . H29A H 0.8182 0.5314 0.2624 0.028 Uiso 1 1 calc R U . . . H29B H 0.7721 0.5613 0.3046 0.028 Uiso 1 1 calc R U . . . C25 C 0.7638(3) 0.7104(2) 0.26397(15) 0.0128(9) Uani 1 1 d . . . . . H25A H 0.7850 0.7050 0.2960 0.019 Uiso 1 1 calc R U . . . H25B H 0.7735 0.7516 0.2552 0.019 Uiso 1 1 calc R U . . . H25C H 0.8067 0.6852 0.2442 0.019 Uiso 1 1 calc R U . . . C3 C 0.6072(3) 0.7005(2) 0.20838(15) 0.0110(9) Uani 1 1 d . . . . . H3 H 0.6146 0.6617 0.1926 0.013 Uiso 1 1 calc R U . . . C4 C 0.4920(3) 0.71113(19) 0.21685(15) 0.0112(9) Uani 1 1 d . . . . . C5 C 0.4124(4) 0.7011(2) 0.18235(15) 0.0125(9) Uani 1 1 d . . . . . C6 C 0.3116(4) 0.71948(19) 0.18905(16) 0.0115(9) Uani 1 1 d . . . . . C10 C 0.1079(4) 0.7762(2) 0.25976(16) 0.0144(9) Uani 1 1 d . . . . . H10 H 0.0409 0.7905 0.2514 0.017 Uiso 1 1 calc R U . . . C11 C 0.1299(4) 0.77099(19) 0.30620(16) 0.0126(9) Uani 1 1 d . . . . . C14 C 0.2205(3) 0.76173(19) 0.37159(15) 0.0112(9) Uani 1 1 d . . . . . C13 C 0.1119(3) 0.7802(2) 0.38662(15) 0.0124(9) Uani 1 1 d . . . . . H13 H 0.0874 0.7541 0.4120 0.015 Uiso 1 1 calc R U . . . C48 C 0.1158(4) 0.8445(2) 0.40348(16) 0.0139(9) Uani 1 1 d . . . . . H48A H 0.1803 0.8503 0.4216 0.017 Uiso 1 1 calc R U . . . H48B H 0.1195 0.8709 0.3765 0.017 Uiso 1 1 calc R U . . . C49 C 0.0217(4) 0.8621(2) 0.43287(17) 0.0169(10) Uani 1 1 d . . . . . H49A H -0.0384 0.8708 0.4126 0.020 Uiso 1 1 calc R U . . . H49B H 0.0022 0.8288 0.4530 0.020 Uiso 1 1 calc R U . . . C50 C 0.0449(4) 0.9155(2) 0.46218(17) 0.0180(10) Uani 1 1 d . . . . . N52 N -0.0196(5) 0.9606(2) 0.45774(17) 0.0363(13) Uani 1 1 d . . . . . H52A H -0.0101 0.9926 0.4743 0.044 Uiso 1 1 calc R U . . . H52B H -0.0720 0.9587 0.4383 0.044 Uiso 1 1 calc R U . . . C12 C 0.0466(3) 0.7683(2) 0.34277(16) 0.0137(9) Uani 1 1 d . . . . . C47 C -0.0466(4) 0.8089(2) 0.33447(17) 0.0188(10) Uani 1 1 d . . . . . H47A H -0.0221 0.8495 0.3316 0.028 Uiso 1 1 calc R U . . . H47B H -0.0952 0.8059 0.3604 0.028 Uiso 1 1 calc R U . . . H47C H -0.0823 0.7972 0.3061 0.028 Uiso 1 1 calc R U . . . C46 C 0.0091(4) 0.7036(2) 0.34387(17) 0.0171(10) Uani 1 1 d . . . . . H46A H -0.0202 0.6930 0.3139 0.026 Uiso 1 1 calc R U . . . H46B H -0.0446 0.6990 0.3676 0.026 Uiso 1 1 calc R U . . . H46C H 0.0683 0.6778 0.3508 0.026 Uiso 1 1 calc R U . . . C15 C 0.3009(3) 0.75102(19) 0.40137(15) 0.0114(8) Uani 1 1 d . . . . . C53 C 0.2776(4) 0.7511(2) 0.45252(15) 0.0155(9) Uani 1 1 d . . . . . H53A H 0.2939 0.7899 0.4653 0.023 Uiso 1 1 calc R U . . . H53B H 0.3204 0.7212 0.4678 0.023 Uiso 1 1 calc R U . . . H53C H 0.2036 0.7423 0.4575 0.023 Uiso 1 1 calc R U . . . C16 C 0.4039(3) 0.73762(18) 0.38503(15) 0.0104(9) Uani 1 1 d . . . . . C17 C 0.4973(4) 0.71603(19) 0.41382(15) 0.0105(9) Uani 1 1 d . . . . . C55 C 0.5238(3) 0.7509(2) 0.45777(14) 0.0120(9) Uani 1 1 d . . . . . H55A H 0.4729 0.7402 0.4819 0.014 Uiso 1 1 calc R U . . . H55B H 0.5938 0.7387 0.4686 0.014 Uiso 1 1 calc R U . . . C56 C 0.5233(4) 0.8175(2) 0.45228(15) 0.0140(9) Uani 1 1 d . . . . . H56A H 0.5630 0.8284 0.4244 0.017 Uiso 1 1 calc R U . . . H56B H 0.4506 0.8313 0.4484 0.017 Uiso 1 1 calc R U . . . C57 C 0.5716(4) 0.8475(2) 0.49378(16) 0.0127(9) Uani 1 1 d . . . . . PR1 C 0.7167(4) 0.9084(2) 0.52149(17) 0.0173(10) Uani 1 1 d . . . . . H40A H 0.7918 0.8995 0.5174 0.021 Uiso 1 1 calc R U . . . H40B H 0.6953 0.8934 0.5520 0.021 Uiso 1 1 calc R U . . . PR2 C 0.7015(4) 0.9746(2) 0.52041(16) 0.0165(10) Uani 1 1 d . . . . . H402 H 0.6264 0.9846 0.5256 0.020 Uiso 1 1 calc R U . . . R3 C 0.4841(3) 1.0045(2) 0.40695(16) 0.0125(9) Uani 1 1 d . . . . . H203 H 0.4737 1.0477 0.4020 0.015 Uiso 1 1 calc R U . . . R2 C 0.5091(4) 0.9741(2) 0.36167(17) 0.0139(9) Uani 1 1 d . . . . . H202 H 0.5613 0.9963 0.3429 0.017 Uiso 1 1 calc R U . . . R1 C 0.4002(4) 0.97445(19) 0.34040(15) 0.0119(9) Uani 1 1 d . . . . . H201 H 0.3877 1.0130 0.3249 0.014 Uiso 1 1 calc R U . . . R4 C 0.3812(4) 0.9754(2) 0.42041(16) 0.0135(9) Uani 1 1 d . . . . . H204 H 0.3966 0.9359 0.4338 0.016 Uiso 1 1 calc R U . . . R5 C 0.3113(4) 1.0081(2) 0.45257(17) 0.0183(10) Uani 1 1 d . . . . . H20D H 0.2449 0.9861 0.4558 0.022 Uiso 1 1 calc R U . . . H20E H 0.3447 1.0097 0.4832 0.022 Uiso 1 1 calc R U . . . B8 C 0.4163(4) 0.9275(2) 0.26237(15) 0.0116(9) Uani 1 1 d . . . . . B9 C 0.4046(3) 0.8702(2) 0.24646(16) 0.0114(9) Uani 1 1 d . . . . . B2 C 0.3591(4) 0.87076(19) 0.31837(15) 0.0119(9) Uani 1 1 d . . . . . H102 H 0.3376 0.8582 0.3480 0.014 Uiso 1 1 calc R U . . . B4 C 0.4297(4) 0.8568(2) 0.20092(16) 0.0127(9) Uani 1 1 d . . . . . H104 H 0.4207 0.8180 0.1895 0.015 Uiso 1 1 calc R U . . . B7 C 0.4559(4) 0.9726(2) 0.23471(16) 0.0141(9) Uani 1 1 d . . . . . H107 H 0.4650 1.0112 0.2464 0.017 Uiso 1 1 calc R U . . . B11 C 0.5245(4) 1.0064(2) 0.15863(17) 0.0201(10) Uani 1 1 d . . . . . H11A H 0.5343 1.0424 0.1765 0.030 Uiso 1 1 calc R U . . . H11B H 0.4753 1.0139 0.1335 0.030 Uiso 1 1 calc R U . . . H11C H 0.5917 0.9938 0.1459 0.030 Uiso 1 1 calc R U . . . B10 C 0.4963(5) 0.8863(2) 0.12365(17) 0.0234(11) Uani 1 1 d . . . . . H11D H 0.5725 0.8859 0.1204 0.035 Uiso 1 1 calc R U . . . H11E H 0.4665 0.9159 0.1031 0.035 Uiso 1 1 calc R U . . . H11F H 0.4684 0.8475 0.1157 0.035 Uiso 1 1 calc R U . . . PR3 C 0.7694(5) 1.0053(3) 0.55551(18) 0.0290(13) Uani 1 1 d . . . . . H40C H 0.8430 0.9979 0.5485 0.044 Uiso 1 1 calc R U . . . H40D H 0.7531 0.9902 0.5862 0.044 Uiso 1 1 calc R U . . . H40E H 0.7559 1.0477 0.5546 0.044 Uiso 1 1 calc R U . . . C54 C 0.4740(4) 0.65149(19) 0.42683(16) 0.0136(9) Uani 1 1 d . . . . . H54A H 0.4089 0.6496 0.4444 0.020 Uiso 1 1 calc R U . . . H54B H 0.5315 0.6360 0.4455 0.020 Uiso 1 1 calc R U . . . H54C H 0.4670 0.6279 0.3988 0.020 Uiso 1 1 calc R U . . . C18 C 0.5868(3) 0.7212(2) 0.37801(15) 0.0117(9) Uani 1 1 d . . . . . H18 H 0.6121 0.7628 0.3778 0.014 Uiso 1 1 calc R U . . . C60 C 0.6812(4) 0.6806(2) 0.38628(16) 0.0134(9) Uani 1 1 d . . . . . H60A H 0.6552 0.6426 0.3981 0.016 Uiso 1 1 calc R U . . . H60B H 0.7152 0.6729 0.3564 0.016 Uiso 1 1 calc R U . . . C61 C 0.7625(3) 0.7036(2) 0.41906(15) 0.0130(9) Uani 1 1 d . . . . . C8 C 0.1459(4) 0.76216(19) 0.17456(15) 0.0129(9) Uani 1 1 d . . . . . H8 H 0.0711 0.7506 0.1707 0.015 Uiso 1 1 calc R U . . . C41 C 0.1642(4) 0.8253(2) 0.15689(17) 0.0181(10) Uani 1 1 d . . . . . H41A H 0.1454 0.8529 0.1818 0.022 Uiso 1 1 calc R U . . . H41B H 0.2399 0.8301 0.1509 0.022 Uiso 1 1 calc R U . . . C42 C 0.1055(4) 0.8435(2) 0.11398(17) 0.0187(10) Uani 1 1 d . . . . . H42A H 0.1451 0.8305 0.0866 0.022 Uiso 1 1 calc R U . . . H42B H 0.0368 0.8235 0.1135 0.022 Uiso 1 1 calc R U . . . C43 C 0.0890(4) 0.9088(2) 0.11139(17) 0.0188(10) Uani 1 1 d . . . . . N45 N 0.0505(5) 0.9296(2) 0.07255(17) 0.0374(13) Uani 1 1 d . . . . . H45A H 0.0378 0.9675 0.0697 0.045 Uiso 1 1 calc R U . . . H45B H 0.0375 0.9057 0.0495 0.045 Uiso 1 1 calc R U . . . C7 C 0.2190(4) 0.7136(2) 0.15593(15) 0.0121(9) Uani 1 1 d . . . . . C37 C 0.1702(4) 0.65213(19) 0.16583(16) 0.0139(9) Uani 1 1 d . . . . . H37A H 0.2242 0.6215 0.1613 0.017 Uiso 1 1 calc R U . . . H37B H 0.1478 0.6505 0.1983 0.017 Uiso 1 1 calc R U . . . C38 C 0.0782(4) 0.6387(2) 0.13554(17) 0.0145(9) Uani 1 1 d . . . . . N40 N 0.0952(3) 0.60296(19) 0.10045(15) 0.0208(9) Uani 1 1 d . . . . . H40F H 0.0439 0.5942 0.0815 0.025 Uiso 1 1 calc R U . . . H40G H 0.1577 0.5879 0.0961 0.025 Uiso 1 1 calc R U . . . C36 C 0.2412(4) 0.7216(2) 0.10458(16) 0.0159(9) Uani 1 1 d . . . . . H36A H 0.2886 0.7549 0.1002 0.024 Uiso 1 1 calc R U . . . H36B H 0.1755 0.7291 0.0883 0.024 Uiso 1 1 calc R U . . . H36C H 0.2735 0.6858 0.0924 0.024 Uiso 1 1 calc R U . . . C35 C 0.4442(4) 0.6675(2) 0.13969(17) 0.0206(11) Uani 1 1 d . . . . . H35A H 0.3866 0.6421 0.1299 0.031 Uiso 1 1 calc R U . . . H35B H 0.5057 0.6434 0.1465 0.031 Uiso 1 1 calc R U . . . H35C H 0.4610 0.6954 0.1151 0.031 Uiso 1 1 calc R U . . . C31 C 0.7519(4) 0.7274(3) 0.15187(19) 0.0277(13) Uani 1 1 d . . . . . H31A H 0.8106 0.7267 0.1740 0.033 Uiso 1 1 calc R U . . . H31B H 0.7410 0.6866 0.1409 0.033 Uiso 1 1 calc R U . . . C32 C 0.7817(4) 0.7658(3) 0.11137(18) 0.0255(12) Uani 1 1 d . . . . . N34 N 0.8734(4) 0.7514(2) 0.09241(16) 0.0297(11) Uani 1 1 d . . . . . H34A H 0.8965 0.7710 0.0684 0.036 Uiso 1 1 calc R U . . . H34B H 0.9105 0.7224 0.1039 0.036 Uiso 1 1 calc R U . . . O5W O 0.3380(7) 0.7804(3) 0.0171(3) 0.092(2) Uani 1 1 d . . . . . O13W O 0.1865(5) 0.1022(3) 0.5221(2) 0.0659(16) Uani 1 1 d . . . . . O18W O 0.5573(4) 0.6376(2) 0.01576(19) 0.0513(13) Uiso 1 1 d . . . . . O12W O 0.7067(6) 0.8368(3) 0.0085(2) 0.0736(18) Uiso 1 1 d . . . . . O17W O 0.4735(14) 0.6803(8) -0.0080(6) 0.188(6) Uiso 1 1 d . . . . . O16W O 0.0894(16) 0.0823(8) 0.4901(6) 0.201(7) Uiso 1 1 d . . . . . O19W O 0.974(3) 0.1788(16) 0.4883(11) 0.346(16) Uiso 1 1 d . . . . . O20W O 0.654(4) 0.682(2) 0.0449(13) 0.45(2) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C30 0.014(2) 0.018(2) 0.010(2) 0.0050(17) 0.0025(17) 0.003(2) Co1 0.0074(3) 0.0076(3) 0.0080(3) -0.0005(3) -0.0002(3) 0.0004(3) P1 0.0111(5) 0.0113(5) 0.0147(6) 0.0001(4) -0.0020(4) -0.0016(4) O10W 0.0151(16) 0.0202(17) 0.0234(18) -0.0016(14) 0.0052(14) -0.0017(14) O10L 0.042(2) 0.0156(18) 0.048(3) -0.0122(18) 0.004(2) -0.0016(18) O9W 0.0191(17) 0.0210(17) 0.0219(18) -0.0044(14) 0.0021(15) -0.0030(15) O11L 0.044(3) 0.019(2) 0.059(3) -0.0004(19) 0.025(2) -0.0117(19) O28 0.0196(16) 0.0154(15) 0.0135(16) -0.0052(13) 0.0036(13) 0.0012(14) O1W 0.034(2) 0.0191(18) 0.032(2) -0.0051(16) 0.0085(18) 0.0002(16) O51 0.0233(19) 0.0261(19) 0.0197(18) -0.0059(15) 0.0028(15) -0.0048(15) O7W 0.038(2) 0.0191(18) 0.036(2) -0.0029(16) -0.0143(19) 0.0080(17) O58 0.0178(16) 0.0236(18) 0.0155(17) -0.0055(14) 0.0065(14) -0.0043(15) O3W 0.033(2) 0.0198(19) 0.047(2) 0.0038(17) 0.016(2) -0.0029(18) OP3 0.0126(15) 0.0158(16) 0.0142(16) 0.0028(13) -0.0018(13) -0.0024(13) O4W 0.050(3) 0.024(2) 0.026(2) -0.0059(16) 0.0020(19) -0.0048(19) O2W 0.068(3) 0.042(3) 0.023(2) -0.0059(18) 0.003(2) -0.015(3) OP2 0.0123(16) 0.0216(17) 0.0150(16) 0.0069(13) -0.0062(13) -0.0050(14) OR7 0.0136(15) 0.0150(16) 0.0270(19) -0.0010(14) -0.0049(14) 0.0044(14) O11W 0.063(4) 0.054(3) 0.058(3) -0.005(3) -0.003(3) 0.003(3) OR6 0.0106(15) 0.0182(16) 0.0141(16) -0.0049(13) -0.0018(12) -0.0029(13) O8W 0.049(3) 0.064(3) 0.058(3) 0.025(3) 0.030(3) 0.031(3) OR8 0.0271(19) 0.0231(19) 0.0225(19) -0.0099(15) -0.0040(16) 0.0081(16) O15W 0.065(4) 0.056(3) 0.077(4) 0.001(3) 0.007(3) -0.001(3) OP4 0.0261(19) 0.0145(16) 0.0292(19) -0.0070(14) -0.0002(16) 0.0042(15) OP5 0.0141(16) 0.0195(17) 0.0162(16) 0.0040(13) 0.0008(13) -0.0019(14) O62 0.0153(16) 0.0172(17) 0.0273(18) 0.0015(14) -0.0012(14) -0.0012(14) O44 0.0293(19) 0.0156(17) 0.0186(17) 0.0007(14) -0.0047(15) -0.0003(15) O39 0.0124(16) 0.0178(17) 0.032(2) -0.0073(15) 0.0003(14) 0.0012(14) N9L 0.021(2) 0.014(2) 0.039(3) -0.0049(19) -0.001(2) -0.0006(17) N24 0.0080(16) 0.0082(17) 0.0125(18) -0.0002(14) 0.0016(14) 0.0007(14) N21 0.0122(17) 0.0059(16) 0.0095(17) -0.0017(14) -0.0001(14) 0.0015(14) N22 0.0107(17) 0.0089(17) 0.0121(17) -0.0014(14) 0.0010(14) 0.0016(15) C9 0.012(2) 0.0070(19) 0.013(2) -0.0003(16) -0.0043(16) 0.0004(16) N23 0.0120(17) 0.0077(17) 0.0129(18) 0.0008(14) -0.0020(15) -0.0005(15) N59 0.0144(19) 0.0151(18) 0.0134(19) 0.0012(15) 0.0002(16) -0.0024(16) NB1 0.0158(18) 0.0073(17) 0.0102(18) -0.0005(14) -0.0009(15) -0.0027(14) NB3 0.0121(18) 0.0119(17) 0.0093(18) -0.0008(14) 0.0004(14) -0.0006(15) B5 0.016(2) 0.017(2) 0.014(2) 0.0016(18) 0.0005(18) 0.0004(19) B6 0.014(2) 0.012(2) 0.015(2) 0.0046(18) -0.0009(17) 0.0012(18) N63 0.020(2) 0.0152(19) 0.021(2) 0.0014(17) -0.0101(17) 0.0019(17) O33 0.039(3) 0.067(3) 0.040(3) 0.037(2) 0.020(2) 0.028(3) C1L 0.010(2) 0.017(2) 0.012(2) -0.0017(18) 0.0011(17) 0.0036(18) C2L 0.017(2) 0.014(2) 0.015(2) -0.0017(18) -0.0015(19) 0.0007(19) C3L 0.016(2) 0.011(2) 0.020(2) -0.0001(18) -0.0021(19) 0.0002(18) C4L 0.028(3) 0.014(2) 0.023(3) -0.0044(19) 0.003(2) -0.003(2) C5L 0.026(3) 0.011(2) 0.030(3) -0.004(2) 0.009(2) -0.006(2) C6L 0.017(2) 0.010(2) 0.028(3) -0.0023(19) -0.002(2) 0.0000(18) C7L 0.030(3) 0.018(2) 0.023(3) -0.008(2) 0.003(2) -0.002(2) C8L 0.025(3) 0.020(2) 0.020(2) -0.003(2) 0.007(2) -0.002(2) C19 0.008(2) 0.011(2) 0.012(2) 0.0015(17) 0.0009(17) 0.0022(17) C1 0.010(2) 0.009(2) 0.010(2) -0.0010(16) 0.0005(17) 0.0006(17) C20 0.011(2) 0.011(2) 0.012(2) 0.0007(17) -0.0004(17) 0.0013(17) C2 0.009(2) 0.009(2) 0.012(2) -0.0009(16) -0.0012(17) 0.0019(17) C26 0.011(2) 0.009(2) 0.013(2) -0.0006(17) 0.0006(17) -0.0006(17) C27 0.014(2) 0.011(2) 0.021(3) -0.0021(18) -0.0007(19) -0.0015(18) N29 0.023(2) 0.025(2) 0.021(2) -0.0021(18) -0.0015(18) 0.0133(19) C25 0.011(2) 0.015(2) 0.013(2) 0.0001(17) 0.0004(17) -0.0010(18) C3 0.010(2) 0.015(2) 0.009(2) 0.0002(17) 0.0011(17) 0.0013(17) C4 0.011(2) 0.009(2) 0.013(2) 0.0007(17) 0.0004(17) -0.0020(17) C5 0.012(2) 0.015(2) 0.010(2) -0.0019(17) 0.0004(17) 0.0024(18) C6 0.012(2) 0.009(2) 0.014(2) -0.0007(17) -0.0016(17) -0.0003(17) C10 0.012(2) 0.015(2) 0.016(2) 0.0006(18) -0.0048(18) 0.0039(18) C11 0.015(2) 0.010(2) 0.013(2) -0.0002(17) -0.0025(18) -0.0001(17) C14 0.011(2) 0.011(2) 0.012(2) -0.0007(16) 0.0020(17) -0.0024(17) C13 0.011(2) 0.015(2) 0.012(2) 0.0008(17) 0.0017(17) 0.0015(17) C48 0.012(2) 0.015(2) 0.015(2) -0.0008(18) 0.0042(18) -0.0004(18) C49 0.014(2) 0.018(2) 0.019(2) -0.0048(19) 0.0043(19) 0.0005(19) C50 0.020(2) 0.016(2) 0.018(2) 0.0007(19) 0.008(2) -0.002(2) N52 0.061(4) 0.020(2) 0.028(3) -0.013(2) -0.013(2) 0.016(2) C12 0.009(2) 0.015(2) 0.017(2) 0.0001(18) 0.0006(18) 0.0015(18) C47 0.014(2) 0.024(2) 0.018(2) -0.006(2) 0.0001(19) 0.005(2) C46 0.013(2) 0.019(2) 0.020(2) -0.003(2) 0.0023(19) -0.0034(19) C15 0.011(2) 0.011(2) 0.012(2) 0.0004(17) 0.0022(17) -0.0008(17) C53 0.012(2) 0.023(2) 0.011(2) -0.0001(18) 0.0014(17) 0.0032(19) C16 0.013(2) 0.0061(19) 0.012(2) 0.0000(16) -0.0006(17) -0.0009(17) C17 0.015(2) 0.008(2) 0.009(2) 0.0012(16) -0.0027(17) 0.0029(17) C55 0.013(2) 0.014(2) 0.009(2) -0.0001(17) 0.0011(16) 0.0006(18) C56 0.016(2) 0.015(2) 0.011(2) 0.0000(17) -0.0021(18) -0.0003(18) C57 0.013(2) 0.010(2) 0.015(2) -0.0016(17) 0.0019(18) 0.0042(18) PR1 0.017(2) 0.016(2) 0.019(2) 0.0031(19) -0.0059(19) -0.0046(19) PR2 0.021(2) 0.016(2) 0.013(2) -0.0005(18) -0.0026(19) -0.0074(19) R3 0.010(2) 0.014(2) 0.013(2) 0.0017(18) -0.0046(17) -0.0032(18) R2 0.011(2) 0.012(2) 0.019(2) -0.0002(18) -0.0001(18) 0.0005(17) R1 0.015(2) 0.009(2) 0.011(2) -0.0021(17) 0.0007(18) -0.0007(17) R4 0.011(2) 0.019(2) 0.011(2) 0.0012(18) -0.0004(17) -0.0037(18) R5 0.018(2) 0.022(2) 0.015(2) -0.0012(19) 0.0004(19) -0.002(2) B8 0.012(2) 0.011(2) 0.011(2) 0.0016(17) 0.0005(17) 0.0030(18) B9 0.009(2) 0.010(2) 0.016(2) 0.0022(17) -0.0015(17) 0.0013(17) B2 0.014(2) 0.009(2) 0.014(2) -0.0008(17) -0.0013(17) 0.0029(17) B4 0.013(2) 0.012(2) 0.013(2) -0.0007(17) 0.0006(17) 0.0006(18) B7 0.016(2) 0.010(2) 0.016(2) 0.0018(17) -0.0011(18) -0.0007(18) B11 0.027(3) 0.016(2) 0.017(2) 0.0048(19) 0.001(2) -0.006(2) B10 0.036(3) 0.020(3) 0.014(2) 0.0024(19) 0.005(2) 0.002(2) PR3 0.043(3) 0.028(3) 0.016(2) 0.001(2) -0.012(2) -0.015(3) C54 0.018(2) 0.008(2) 0.014(2) 0.0030(17) -0.0009(18) 0.0008(18) C18 0.011(2) 0.012(2) 0.012(2) 0.0011(17) -0.0015(17) 0.0023(18) C60 0.012(2) 0.011(2) 0.018(2) -0.0028(17) -0.0011(18) 0.0032(17) C61 0.009(2) 0.019(2) 0.010(2) -0.0001(18) 0.0020(17) 0.0012(18) C8 0.014(2) 0.011(2) 0.013(2) -0.0022(17) -0.0039(17) 0.0036(18) C41 0.025(3) 0.013(2) 0.016(2) 0.0012(18) -0.007(2) 0.000(2) C42 0.021(2) 0.016(2) 0.019(2) 0.0016(19) -0.005(2) 0.003(2) C43 0.021(2) 0.019(2) 0.017(2) 0.0044(19) 0.000(2) 0.002(2) N45 0.072(4) 0.018(2) 0.022(2) 0.0019(19) -0.014(3) 0.011(3) C7 0.011(2) 0.013(2) 0.013(2) -0.0027(17) -0.0033(18) 0.0011(18) C37 0.013(2) 0.010(2) 0.020(2) -0.0002(17) -0.0034(18) 0.0015(18) C38 0.013(2) 0.011(2) 0.020(2) -0.0030(18) -0.0004(19) 0.0003(18) N40 0.015(2) 0.020(2) 0.027(2) -0.0101(18) -0.0017(18) 0.0023(17) C36 0.017(2) 0.018(2) 0.012(2) -0.0025(18) -0.0037(18) -0.0001(19) C35 0.017(2) 0.027(3) 0.017(2) -0.013(2) -0.004(2) 0.006(2) C31 0.023(3) 0.037(3) 0.023(3) 0.017(2) 0.013(2) 0.012(2) C32 0.021(3) 0.035(3) 0.020(3) 0.009(2) 0.009(2) 0.005(2) N34 0.028(2) 0.035(3) 0.025(2) 0.006(2) 0.0179(19) 0.005(2) O5W 0.104(6) 0.067(4) 0.106(6) -0.001(4) 0.046(5) 0.001(4) O13W 0.062(4) 0.071(4) 0.065(4) -0.005(3) -0.001(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C30 C31 1.526(7) . ? C30 C3 1.541(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? Co1 C1L 1.867(5) . ? Co1 N21 1.881(4) . ? Co1 N24 1.885(4) . ? Co1 N23 1.909(4) . ? Co1 N22 1.912(4) . ? Co1 NB3 2.059(4) . ? P1 OP4 1.483(4) . ? P1 OP5 1.486(3) . ? P1 OP3 1.583(3) . ? P1 OP2 1.610(3) . ? O10L N9L 1.231(6) . ? O11L N9L 1.224(7) . ? O28 C27 1.247(6) . ? O51 C50 1.243(7) . ? O58 C57 1.250(6) . ? OP3 PR2 1.460(6) . ? OP2 R3 1.424(5) . ? OR7 R2 1.411(6) . ? OR7 H207 0.8400 . ? O11W O16W 1.38(2) . ? OR6 R1 1.419(6) . ? OR6 R4 1.452(5) . ? OR8 R5 1.434(6) . ? OR8 H208 0.8400 . ? O15W O19W 1.52(4) . ? O62 C61 1.234(6) . ? O44 C43 1.253(7) . ? O39 C38 1.253(6) . ? N9L C6L 1.463(6) . ? N24 C16 1.311(6) . ? N24 C19 1.483(5) . ? N21 C4 1.297(6) . ? N21 C1 1.499(6) . ? N22 C9 1.343(6) . ? N22 C6 1.392(6) . ? C9 C10 1.385(7) . ? C9 C8 1.508(6) . ? N23 C11 1.339(6) . ? N23 C14 1.394(6) . ? N59 C57 1.319(6) . ? N59 PR1 1.451(6) . ? N59 H59 0.8800 . ? NB1 B2 1.359(6) . ? NB1 B8 1.386(6) . ? NB1 R1 1.447(6) . ? NB3 B2 1.328(6) . ? NB3 B9 1.397(6) . ? B5 B4 1.390(7) . ? B5 B6 1.413(7) . ? B5 B10 1.506(7) . ? B6 B7 1.399(7) . ? B6 B11 1.509(6) . ? N63 C61 1.330(6) . ? N63 H63A 0.8800 . ? N63 H63B 0.8800 . ? O33 C32 1.217(7) . ? C1L C2L 1.210(7) . ? C2L C3L 1.423(7) . ? C3L C8L 1.405(7) . ? C3L C4L 1.406(7) . ? C4L C5L 1.377(7) . ? C4L H4L 0.9500 . ? C5L C6L 1.392(7) . ? C5L H5L 0.9500 . ? C6L C7L 1.374(8) . ? C7L C8L 1.389(8) . ? C7L H7L 0.9500 . ? C8L H8L 0.9500 . ? C19 C18 1.523(6) . ? C19 C1 1.545(6) . ? C19 H19 1.0000 . ? C1 C20 1.529(6) . ? C1 C2 1.581(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C2 C25 1.532(6) . ? C2 C26 1.555(6) . ? C2 C3 1.563(6) . ? C26 C27 1.511(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 N29 1.320(7) . ? N29 H29A 0.8800 . ? N29 H29B 0.8800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C3 C4 1.515(6) . ? C3 H3 1.0000 . ? C4 C5 1.449(6) . ? C5 C6 1.371(7) . ? C5 C35 1.514(6) . ? C6 C7 1.535(6) . ? C10 C11 1.387(7) . ? C10 H10 0.9500 . ? C11 C12 1.509(6) . ? C14 C15 1.368(6) . ? C14 C13 1.517(6) . ? C13 C48 1.544(6) . ? C13 C12 1.551(6) . ? C13 H13 1.0000 . ? C48 C49 1.531(6) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.514(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 N52 1.323(7) . ? N52 H52A 0.8800 . ? N52 H52B 0.8800 . ? C12 C47 1.527(7) . ? C12 C46 1.550(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C15 C16 1.435(6) . ? C15 C53 1.519(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C16 C17 1.541(6) . ? C17 C55 1.544(6) . ? C17 C54 1.545(6) . ? C17 C18 1.554(6) . ? C55 C56 1.523(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.520(6) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? PR1 PR2 1.519(6) . ? PR1 H40A 0.9900 . ? PR1 H40B 0.9900 . ? PR2 PR3 1.513(7) . ? PR2 H402 1.0000 . ? R3 R2 1.524(7) . ? R3 R4 1.525(6) . ? R3 H203 1.0000 . ? R2 R1 1.527(6) . ? R2 H202 1.0000 . ? R1 H201 1.0000 . ? R4 R5 1.494(7) . ? R4 H204 1.0000 . ? R5 H20D 0.9900 . ? R5 H20E 0.9900 . ? B8 B9 1.391(7) . ? B8 B7 1.399(7) . ? B9 B4 1.398(7) . ? B2 H102 0.9500 . ? B4 H104 0.9500 . ? B7 H107 0.9500 . ? B11 H11A 0.9800 . ? B11 H11B 0.9800 . ? B11 H11C 0.9800 . ? B10 H11D 0.9800 . ? B10 H11E 0.9800 . ? B10 H11F 0.9800 . ? PR3 H40C 0.9800 . ? PR3 H40D 0.9800 . ? PR3 H40E 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C18 C60 1.538(6) . ? C18 H18 1.0000 . ? C60 C61 1.506(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C8 C41 1.543(6) . ? C8 C7 1.545(6) . ? C8 H8 1.0000 . ? C41 C42 1.516(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.501(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 N45 1.323(7) . ? N45 H45A 0.8800 . ? N45 H45B 0.8800 . ? C7 C36 1.533(6) . ? C7 C37 1.559(6) . ? C37 C38 1.504(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N40 1.324(7) . ? N40 H40F 0.8800 . ? N40 H40G 0.8800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C31 C32 1.517(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N34 1.337(7) . ? N34 H34A 0.8800 . ? N34 H34B 0.8800 . ? O13W O16W 1.62(2) . ? O18W O17W 1.604(19) . ? O18W O20W 1.80(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 C31 C30 C3 112.7(4) . . ? C31 C30 H30A 109.1 . . ? C3 C30 H30A 109.1 . . ? C31 C30 H30B 109.1 . . ? C3 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C1L Co1 N21 92.14(17) . . ? C1L Co1 N24 89.47(18) . . ? N21 Co1 N24 83.36(16) . . ? C1L Co1 N23 88.90(18) . . ? N21 Co1 N23 173.59(16) . . ? N24 Co1 N23 90.32(16) . . ? C1L Co1 N22 86.00(18) . . ? N21 Co1 N22 89.93(16) . . ? N24 Co1 N22 171.76(16) . . ? N23 Co1 N22 96.46(16) . . ? C1L Co1 NB3 174.74(18) . . ? N21 Co1 NB3 91.53(15) . . ? N24 Co1 NB3 94.70(15) . . ? N23 Co1 NB3 87.87(15) . . ? N22 Co1 NB3 90.24(15) . . ? OP4 P1 OP5 117.6(2) . . ? OP4 P1 OP3 111.5(2) . . ? OP5 P1 OP3 106.92(19) . . ? OP4 P1 OP2 109.7(2) . . ? OP5 P1 OP2 110.16(19) . . ? OP3 P1 OP2 99.39(17) . . ? PR2 OP3 P1 119.9(3) . . ? R3 OP2 P1 119.9(3) . . ? R2 OR7 H207 109.5 . . ? R1 OR6 R4 109.4(3) . . ? R5 OR8 H208 109.5 . . ? O11L N9L O10L 122.9(4) . . ? O11L N9L C6L 119.4(4) . . ? O10L N9L C6L 117.7(5) . . ? C16 N24 C19 110.8(4) . . ? C16 N24 Co1 133.2(3) . . ? C19 N24 Co1 113.5(3) . . ? C4 N21 C1 112.4(4) . . ? C4 N21 Co1 130.0(3) . . ? C1 N21 Co1 117.0(3) . . ? C9 N22 C6 109.9(4) . . ? C9 N22 Co1 122.5(3) . . ? C6 N22 Co1 126.7(3) . . ? N22 C9 C10 126.1(4) . . ? N22 C9 C8 110.4(4) . . ? C10 C9 C8 123.5(4) . . ? C11 N23 C14 110.1(4) . . ? C11 N23 Co1 123.8(3) . . ? C14 N23 Co1 126.0(3) . . ? C57 N59 PR1 124.7(4) . . ? C57 N59 H59 117.7 . . ? PR1 N59 H59 117.7 . . ? B2 NB1 B8 106.9(4) . . ? B2 NB1 R1 125.9(4) . . ? B8 NB1 R1 125.6(4) . . ? B2 NB3 B9 105.8(4) . . ? B2 NB3 Co1 122.2(3) . . ? B9 NB3 Co1 131.5(3) . . ? B4 B5 B6 120.6(4) . . ? B4 B5 B10 119.2(4) . . ? B6 B5 B10 120.2(4) . . ? B7 B6 B5 120.6(4) . . ? B7 B6 B11 118.9(4) . . ? B5 B6 B11 120.5(4) . . ? C61 N63 H63A 120.0 . . ? C61 N63 H63B 120.0 . . ? H63A N63 H63B 120.0 . . ? C2L C1L Co1 172.5(4) . . ? C1L C2L C3L 178.7(5) . . ? C8L C3L C4L 118.6(5) . . ? C8L C3L C2L 121.0(5) . . ? C4L C3L C2L 120.4(4) . . ? C5L C4L C3L 121.1(5) . . ? C5L C4L H4L 119.5 . . ? C3L C4L H4L 119.5 . . ? C4L C5L C6L 118.2(5) . . ? C4L C5L H5L 120.9 . . ? C6L C5L H5L 120.9 . . ? C7L C6L C5L 122.8(5) . . ? C7L C6L N9L 118.8(5) . . ? C5L C6L N9L 118.4(5) . . ? C6L C7L C8L 118.5(5) . . ? C6L C7L H7L 120.8 . . ? C8L C7L H7L 120.8 . . ? C7L C8L C3L 120.7(5) . . ? C7L C8L H8L 119.6 . . ? C3L C8L H8L 119.6 . . ? N24 C19 C18 102.4(3) . . ? N24 C19 C1 106.6(3) . . ? C18 C19 C1 121.9(4) . . ? N24 C19 H19 108.4 . . ? C18 C19 H19 108.4 . . ? C1 C19 H19 108.4 . . ? N21 C1 C20 110.7(3) . . ? N21 C1 C19 101.4(3) . . ? C20 C1 C19 110.2(4) . . ? N21 C1 C2 102.1(3) . . ? C20 C1 C2 113.5(3) . . ? C19 C1 C2 117.7(3) . . ? 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 . . ? C25 C2 C26 108.4(4) . . ? C25 C2 C3 113.5(4) . . ? C26 C2 C3 107.6(3) . . ? C25 C2 C1 114.5(3) . . ? C26 C2 C1 110.3(4) . . ? C3 C2 C1 102.3(3) . . ? C27 C26 C2 113.8(4) . . ? C27 C26 H26A 108.8 . . ? C2 C26 H26A 108.8 . . ? C27 C26 H26B 108.8 . . ? C2 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? O28 C27 N29 122.5(5) . . ? O28 C27 C26 121.5(4) . . ? N29 C27 C26 116.0(4) . . ? C27 N29 H29A 120.0 . . ? C27 N29 H29B 120.0 . . ? H29A N29 H29B 120.0 . . ? C2 C25 H25A 109.5 . . ? C2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C4 C3 C30 111.1(4) . . ? C4 C3 C2 101.2(3) . . ? C30 C3 C2 120.0(4) . . ? C4 C3 H3 107.9 . . ? C30 C3 H3 107.9 . . ? C2 C3 H3 107.9 . . ? N21 C4 C5 124.4(4) . . ? N21 C4 C3 112.4(4) . . ? C5 C4 C3 123.1(4) . . ? C6 C5 C4 121.0(4) . . ? C6 C5 C35 121.6(4) . . ? C4 C5 C35 117.3(4) . . ? C5 C6 N22 123.8(4) . . ? C5 C6 C7 127.7(4) . . ? N22 C6 C7 108.5(4) . . ? C9 C10 C11 125.0(4) . . ? C9 C10 H10 117.5 . . ? C11 C10 H10 117.5 . . ? N23 C11 C10 124.9(4) . . ? N23 C11 C12 111.6(4) . . ? C10 C11 C12 123.3(4) . . ? C15 C14 N23 127.0(4) . . ? C15 C14 C13 123.8(4) . . ? N23 C14 C13 109.1(4) . . ? C14 C13 C48 108.9(4) . . ? C14 C13 C12 102.0(3) . . ? C48 C13 C12 116.4(4) . . ? C14 C13 H13 109.7 . . ? C48 C13 H13 109.7 . . ? C12 C13 H13 109.7 . . ? C49 C48 C13 113.6(4) . . ? C49 C48 H48A 108.8 . . ? C13 C48 H48A 108.8 . . ? C49 C48 H48B 108.8 . . ? C13 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C48 111.8(4) . . ? C50 C49 H49A 109.3 . . ? C48 C49 H49A 109.3 . . ? C50 C49 H49B 109.3 . . ? C48 C49 H49B 109.3 . . ? H49A C49 H49B 107.9 . . ? O51 C50 N52 123.5(5) . . ? O51 C50 C49 120.1(5) . . ? N52 C50 C49 116.4(5) . . ? C50 N52 H52A 120.0 . . ? C50 N52 H52B 120.0 . . ? H52A N52 H52B 120.0 . . ? C11 C12 C47 114.6(4) . . ? C11 C12 C46 105.8(4) . . ? C47 C12 C46 109.6(4) . . ? C11 C12 C13 101.1(4) . . ? C47 C12 C13 116.6(4) . . ? C46 C12 C13 108.4(4) . . ? C12 C47 H47A 109.5 . . ? C12 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C12 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C12 C46 H46A 109.5 . . ? C12 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C12 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C14 C15 C16 121.3(4) . . ? C14 C15 C53 118.3(4) . . ? C16 C15 C53 120.4(4) . . ? C15 C53 H53A 109.5 . . ? C15 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C15 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N24 C16 C15 122.0(4) . . ? N24 C16 C17 110.8(4) . . ? C15 C16 C17 126.9(4) . . ? C16 C17 C55 117.3(4) . . ? C16 C17 C54 106.6(4) . . ? C55 C17 C54 109.1(4) . . ? C16 C17 C18 100.6(3) . . ? C55 C17 C18 110.8(4) . . ? C54 C17 C18 112.2(4) . . ? C56 C55 C17 115.0(4) . . ? C56 C55 H55A 108.5 . . ? C17 C55 H55A 108.5 . . ? C56 C55 H55B 108.5 . . ? C17 C55 H55B 108.5 . . ? H55A C55 H55B 107.5 . . ? C57 C56 C55 111.2(4) . . ? C57 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C57 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? O58 C57 N59 123.9(4) . . ? O58 C57 C56 119.8(4) . . ? N59 C57 C56 116.3(4) . . ? N59 PR1 PR2 113.1(4) . . ? N59 PR1 H40A 109.0 . . ? PR2 PR1 H40A 109.0 . . ? N59 PR1 H40B 109.0 . . ? PR2 PR1 H40B 109.0 . . ? H40A PR1 H40B 107.8 . . ? OP3 PR2 PR3 108.4(4) . . ? OP3 PR2 PR1 106.0(4) . . ? PR3 PR2 PR1 111.7(4) . . ? OP3 PR2 H402 110.2 . . ? PR3 PR2 H402 110.2 . . ? PR1 PR2 H402 110.2 . . ? OP2 R3 R2 114.5(4) . . ? OP2 R3 R4 109.0(4) . . ? R2 R3 R4 101.9(4) . . ? OP2 R3 H203 110.4 . . ? R2 R3 H203 110.4 . . ? R4 R3 H203 110.4 . . ? OR7 R2 R3 112.1(4) . . ? OR7 R2 R1 107.0(4) . . ? R3 R2 R1 99.0(4) . . ? OR7 R2 H202 112.6 . . ? R3 R2 H202 112.6 . . ? R1 R2 H202 112.6 . . ? OR6 R1 NB1 108.4(4) . . ? OR6 R1 R2 107.0(4) . . ? NB1 R1 R2 112.9(4) . . ? OR6 R1 H201 109.5 . . ? NB1 R1 H201 109.5 . . ? R2 R1 H201 109.5 . . ? OR6 R4 R5 109.2(4) . . ? OR6 R4 R3 103.7(3) . . ? R5 R4 R3 117.6(4) . . ? OR6 R4 H204 108.7 . . ? R5 R4 H204 108.7 . . ? R3 R4 H204 108.7 . . ? OR8 R5 R4 113.3(4) . . ? OR8 R5 H20D 108.9 . . ? R4 R5 H20D 108.9 . . ? OR8 R5 H20E 108.9 . . ? R4 R5 H20E 108.9 . . ? H20D R5 H20E 107.7 . . ? NB1 B8 B9 106.4(4) . . ? NB1 B8 B7 131.3(4) . . ? B9 B8 B7 122.2(4) . . ? B8 B9 NB3 108.6(4) . . ? B8 B9 B4 119.7(4) . . ? NB3 B9 B4 131.7(4) . . ? NB3 B2 NB1 112.2(4) . . ? NB3 B2 H102 123.9 . . ? NB1 B2 H102 123.9 . . ? B5 B4 B9 119.2(4) . . ? B5 B4 H104 120.4 . . ? B9 B4 H104 120.4 . . ? B6 B7 B8 117.7(4) . . ? B6 B7 H107 121.2 . . ? B8 B7 H107 121.2 . . ? B6 B11 H11A 109.5 . . ? B6 B11 H11B 109.5 . . ? H11A B11 H11B 109.5 . . ? B6 B11 H11C 109.5 . . ? H11A B11 H11C 109.5 . . ? H11B B11 H11C 109.5 . . ? B5 B10 H11D 109.5 . . ? B5 B10 H11E 109.5 . . ? H11D B10 H11E 109.5 . . ? B5 B10 H11F 109.5 . . ? H11D B10 H11F 109.5 . . ? H11E B10 H11F 109.5 . . ? PR2 PR3 H40C 109.5 . . ? PR2 PR3 H40D 109.5 . . ? H40C PR3 H40D 109.5 . . ? PR2 PR3 H40E 109.5 . . ? H40C PR3 H40E 109.5 . . ? H40D PR3 H40E 109.5 . . ? C17 C54 H54A 109.5 . . ? C17 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C17 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C19 C18 C60 114.0(4) . . ? C19 C18 C17 102.1(3) . . ? C60 C18 C17 115.4(4) . . ? C19 C18 H18 108.3 . . ? C60 C18 H18 108.3 . . ? C17 C18 H18 108.3 . . ? C61 C60 C18 115.8(4) . . ? C61 C60 H60A 108.3 . . ? C18 C60 H60A 108.3 . . ? C61 C60 H60B 108.3 . . ? C18 C60 H60B 108.3 . . ? H60A C60 H60B 107.4 . . ? O62 C61 N63 122.0(4) . . ? O62 C61 C60 122.4(4) . . ? N63 C61 C60 115.4(4) . . ? C9 C8 C41 106.5(4) . . ? C9 C8 C7 100.5(3) . . ? C41 C8 C7 117.1(4) . . ? C9 C8 H8 110.7 . . ? C41 C8 H8 110.7 . . ? C7 C8 H8 110.7 . . ? C42 C41 C8 117.0(4) . . ? C42 C41 H41A 108.1 . . ? C8 C41 H41A 108.1 . . ? C42 C41 H41B 108.1 . . ? C8 C41 H41B 108.1 . . ? H41A C41 H41B 107.3 . . ? C43 C42 C41 112.4(4) . . ? C43 C42 H42A 109.1 . . ? C41 C42 H42A 109.1 . . ? C43 C42 H42B 109.1 . . ? C41 C42 H42B 109.1 . . ? H42A C42 H42B 107.8 . . ? O44 C43 N45 120.9(5) . . ? O44 C43 C42 122.3(4) . . ? N45 C43 C42 116.8(5) . . ? C43 N45 H45A 120.0 . . ? C43 N45 H45B 120.0 . . ? H45A N45 H45B 120.0 . . ? C36 C7 C6 117.4(4) . . ? C36 C7 C8 111.8(4) . . ? C6 C7 C8 100.7(3) . . ? C36 C7 C37 111.1(4) . . ? C6 C7 C37 105.7(4) . . ? C8 C7 C37 109.5(4) . . ? C38 C37 C7 112.8(4) . . ? C38 C37 H37A 109.0 . . ? C7 C37 H37A 109.0 . . ? C38 C37 H37B 109.0 . . ? C7 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? O39 C38 N40 121.4(4) . . ? O39 C38 C37 121.9(4) . . ? N40 C38 C37 116.7(4) . . ? C38 N40 H40F 120.0 . . ? C38 N40 H40G 120.0 . . ? H40F N40 H40G 120.0 . . ? C7 C36 H36A 109.5 . . ? C7 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C7 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C5 C35 H35A 109.5 . . ? C5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C31 C30 113.5(4) . . ? C32 C31 H31A 108.9 . . ? C30 C31 H31A 108.9 . . ? C32 C31 H31B 108.9 . . ? C30 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? O33 C32 N34 123.6(5) . . ? O33 C32 C31 122.7(5) . . ? N34 C32 C31 113.7(5) . . ? C32 N34 H34A 120.0 . . ? C32 N34 H34B 120.0 . . ? H34A N34 H34B 120.0 . . ? O17W O18W O20W 109.0(16) . . ? O11W O16W O13W 139.1(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag OP4 P1 OP3 PR2 55.8(4) . . . . ? OP5 P1 OP3 PR2 -174.4(3) . . . . ? OP2 P1 OP3 PR2 -59.8(3) . . . . ? OP4 P1 OP2 R3 84.2(4) . . . . ? OP5 P1 OP2 R3 -46.8(4) . . . . ? OP3 P1 OP2 R3 -158.8(3) . . . . ? C1L Co1 N24 C16 -83.3(4) . . . . ? N21 Co1 N24 C16 -175.5(4) . . . . ? N23 Co1 N24 C16 5.6(4) . . . . ? NB3 Co1 N24 C16 93.5(4) . . . . ? C1L Co1 N24 C19 76.7(3) . . . . ? N21 Co1 N24 C19 -15.5(3) . . . . ? N23 Co1 N24 C19 165.6(3) . . . . ? NB3 Co1 N24 C19 -106.5(3) . . . . ? C1L Co1 N21 C4 68.6(4) . . . . ? N24 Co1 N21 C4 157.8(4) . . . . ? N22 Co1 N21 C4 -17.4(4) . . . . ? NB3 Co1 N21 C4 -107.6(4) . . . . ? C1L Co1 N21 C1 -101.8(3) . . . . ? N24 Co1 N21 C1 -12.6(3) . . . . ? N22 Co1 N21 C1 172.2(3) . . . . ? NB3 Co1 N21 C1 82.0(3) . . . . ? C6 N22 C9 C10 163.6(4) . . . . ? Co1 N22 C9 C10 -6.2(6) . . . . ? C6 N22 C9 C8 -15.2(5) . . . . ? Co1 N22 C9 C8 175.1(3) . . . . ? B4 B5 B6 B7 -0.5(7) . . . . ? B10 B5 B6 B7 -179.8(5) . . . . ? B4 B5 B6 B11 179.3(4) . . . . ? B10 B5 B6 B11 0.0(7) . . . . ? C8L C3L C4L C5L 3.4(8) . . . . ? C2L C3L C4L C5L -176.6(5) . . . . ? C3L C4L C5L C6L -1.1(8) . . . . ? C4L C5L C6L C7L -1.3(8) . . . . ? C4L C5L C6L N9L 178.8(5) . . . . ? O11L N9L C6L C7L 179.5(5) . . . . ? O10L N9L C6L C7L 0.7(7) . . . . ? O11L N9L C6L C5L -0.7(7) . . . . ? O10L N9L C6L C5L -179.4(5) . . . . ? C5L C6L C7L C8L 1.5(8) . . . . ? N9L C6L C7L C8L -178.7(5) . . . . ? C6L C7L C8L C3L 0.8(8) . . . . ? C4L C3L C8L C7L -3.2(8) . . . . ? C2L C3L C8L C7L 176.8(5) . . . . ? C16 N24 C19 C18 -28.0(4) . . . . ? Co1 N24 C19 C18 167.5(3) . . . . ? C16 N24 C19 C1 -157.0(4) . . . . ? Co1 N24 C19 C1 38.4(4) . . . . ? C4 N21 C1 C20 105.5(4) . . . . ? Co1 N21 C1 C20 -82.4(4) . . . . ? C4 N21 C1 C19 -137.6(4) . . . . ? Co1 N21 C1 C19 34.5(4) . . . . ? C4 N21 C1 C2 -15.6(5) . . . . ? Co1 N21 C1 C2 156.5(3) . . . . ? N24 C19 C1 N21 -43.2(4) . . . . ? C18 C19 C1 N21 -159.9(4) . . . . ? N24 C19 C1 C20 74.1(4) . . . . ? C18 C19 C1 C20 -42.6(5) . . . . ? N24 C19 C1 C2 -153.6(4) . . . . ? C18 C19 C1 C2 89.7(5) . . . . ? N21 C1 C2 C25 150.8(4) . . . . ? C20 C1 C2 C25 31.6(5) . . . . ? C19 C1 C2 C25 -99.2(4) . . . . ? N21 C1 C2 C26 -86.6(4) . . . . ? C20 C1 C2 C26 154.2(4) . . . . ? C19 C1 C2 C26 23.3(5) . . . . ? N21 C1 C2 C3 27.6(4) . . . . ? C20 C1 C2 C3 -91.5(4) . . . . ? C19 C1 C2 C3 137.6(4) . . . . ? C25 C2 C26 C27 -52.1(5) . . . . ? C3 C2 C26 C27 70.9(5) . . . . ? C1 C2 C26 C27 -178.2(4) . . . . ? C2 C26 C27 O28 -61.0(6) . . . . ? C2 C26 C27 N29 120.1(5) . . . . ? C31 C30 C3 C4 -156.8(4) . . . . ? C31 C30 C3 C2 85.6(5) . . . . ? C25 C2 C3 C4 -153.3(4) . . . . ? C26 C2 C3 C4 86.8(4) . . . . ? C1 C2 C3 C4 -29.4(4) . . . . ? C25 C2 C3 C30 -30.7(5) . . . . ? C26 C2 C3 C30 -150.5(4) . . . . ? C1 C2 C3 C30 93.2(4) . . . . ? C1 N21 C4 C5 176.7(4) . . . . ? Co1 N21 C4 C5 6.0(7) . . . . ? C1 N21 C4 C3 -4.2(5) . . . . ? Co1 N21 C4 C3 -174.9(3) . . . . ? C30 C3 C4 N21 -106.4(4) . . . . ? C2 C3 C4 N21 22.2(5) . . . . ? C30 C3 C4 C5 72.7(5) . . . . ? C2 C3 C4 C5 -158.7(4) . . . . ? N21 C4 C5 C6 8.9(7) . . . . ? C3 C4 C5 C6 -170.1(4) . . . . ? N21 C4 C5 C35 -168.8(4) . . . . ? C3 C4 C5 C35 12.2(7) . . . . ? C4 C5 C6 N22 -3.9(7) . . . . ? C35 C5 C6 N22 173.6(4) . . . . ? C4 C5 C6 C7 178.6(4) . . . . ? C35 C5 C6 C7 -3.9(8) . . . . ? C9 N22 C6 C5 176.0(4) . . . . ? Co1 N22 C6 C5 -14.8(6) . . . . ? C9 N22 C6 C7 -6.1(5) . . . . ? Co1 N22 C6 C7 163.1(3) . . . . ? N22 C9 C10 C11 -5.2(8) . . . . ? C8 C9 C10 C11 173.3(4) . . . . ? C14 N23 C11 C10 177.0(4) . . . . ? Co1 N23 C11 C10 -6.9(6) . . . . ? C14 N23 C11 C12 -9.4(5) . . . . ? Co1 N23 C11 C12 166.7(3) . . . . ? C9 C10 C11 N23 12.5(8) . . . . ? C9 C10 C11 C12 -160.4(4) . . . . ? C11 N23 C14 C15 176.8(4) . . . . ? Co1 N23 C14 C15 0.7(6) . . . . ? C11 N23 C14 C13 -7.4(5) . . . . ? Co1 N23 C14 C13 176.6(3) . . . . ? C15 C14 C13 C48 72.4(6) . . . . ? N23 C14 C13 C48 -103.6(4) . . . . ? C15 C14 C13 C12 -164.0(4) . . . . ? N23 C14 C13 C12 20.0(5) . . . . ? C14 C13 C48 C49 -162.1(4) . . . . ? C12 C13 C48 C49 83.3(5) . . . . ? C13 C48 C49 C50 159.5(4) . . . . ? C48 C49 C50 O51 -56.0(6) . . . . ? C48 C49 C50 N52 124.8(5) . . . . ? N23 C11 C12 C47 147.6(4) . . . . ? C10 C11 C12 C47 -38.8(6) . . . . ? N23 C11 C12 C46 -91.6(4) . . . . ? C10 C11 C12 C46 82.1(5) . . . . ? N23 C11 C12 C13 21.3(5) . . . . ? C10 C11 C12 C13 -165.0(4) . . . . ? C14 C13 C12 C11 -23.3(4) . . . . ? C48 C13 C12 C11 95.1(4) . . . . ? C14 C13 C12 C47 -148.3(4) . . . . ? C48 C13 C12 C47 -29.9(6) . . . . ? C14 C13 C12 C46 87.6(4) . . . . ? C48 C13 C12 C46 -154.0(4) . . . . ? N23 C14 C15 C16 -0.4(7) . . . . ? C13 C14 C15 C16 -175.7(4) . . . . ? N23 C14 C15 C53 -177.9(4) . . . . ? C13 C14 C15 C53 6.8(7) . . . . ? C19 N24 C16 C15 -167.1(4) . . . . ? Co1 N24 C16 C15 -6.6(6) . . . . ? C19 N24 C16 C17 7.4(5) . . . . ? Co1 N24 C16 C17 167.9(3) . . . . ? C14 C15 C16 N24 3.1(7) . . . . ? C53 C15 C16 N24 -179.5(4) . . . . ? C14 C15 C16 C17 -170.5(4) . . . . ? C53 C15 C16 C17 6.9(7) . . . . ? N24 C16 C17 C55 135.9(4) . . . . ? C15 C16 C17 C55 -50.0(6) . . . . ? N24 C16 C17 C54 -101.6(4) . . . . ? C15 C16 C17 C54 72.6(5) . . . . ? N24 C16 C17 C18 15.6(5) . . . . ? C15 C16 C17 C18 -170.2(4) . . . . ? C16 C17 C55 C56 -44.8(5) . . . . ? C54 C17 C55 C56 -166.1(4) . . . . ? C18 C17 C55 C56 69.8(5) . . . . ? C17 C55 C56 C57 -168.2(4) . . . . ? PR1 N59 C57 O58 -0.2(7) . . . . ? PR1 N59 C57 C56 -178.4(4) . . . . ? C55 C56 C57 O58 -61.6(6) . . . . ? C55 C56 C57 N59 116.7(4) . . . . ? C57 N59 PR1 PR2 -104.7(5) . . . . ? P1 OP3 PR2 PR3 -108.8(4) . . . . ? P1 OP3 PR2 PR1 131.1(3) . . . . ? N59 PR1 PR2 OP3 -58.5(5) . . . . ? N59 PR1 PR2 PR3 -176.4(4) . . . . ? P1 OP2 R3 R2 85.5(4) . . . . ? P1 OP2 R3 R4 -161.2(3) . . . . ? OP2 R3 R2 OR7 47.2(5) . . . . ? R4 R3 R2 OR7 -70.2(4) . . . . ? OP2 R3 R2 R1 159.8(4) . . . . ? R4 R3 R2 R1 42.3(4) . . . . ? R4 OR6 R1 NB1 134.4(4) . . . . ? R4 OR6 R1 R2 12.4(5) . . . . ? B2 NB1 R1 OR6 -36.5(6) . . . . ? B8 NB1 R1 OR6 159.8(4) . . . . ? B2 NB1 R1 R2 81.8(5) . . . . ? B8 NB1 R1 R2 -81.8(5) . . . . ? OR7 R2 R1 OR6 82.1(4) . . . . ? R3 R2 R1 OR6 -34.4(4) . . . . ? OR7 R2 R1 NB1 -37.0(5) . . . . ? R3 R2 R1 NB1 -153.5(4) . . . . ? R1 OR6 R4 R5 141.4(4) . . . . ? R1 OR6 R4 R3 15.2(5) . . . . ? OP2 R3 R4 OR6 -158.0(4) . . . . ? R2 R3 R4 OR6 -36.6(4) . . . . ? OP2 R3 R4 R5 81.5(5) . . . . ? R2 R3 R4 R5 -157.2(4) . . . . ? OR6 R4 R5 OR8 -64.7(5) . . . . ? R3 R4 R5 OR8 53.0(6) . . . . ? B2 NB1 B8 B9 2.3(5) . . . . ? R1 NB1 B8 B9 168.5(4) . . . . ? B2 NB1 B8 B7 -176.1(5) . . . . ? R1 NB1 B8 B7 -9.8(8) . . . . ? NB1 B8 B9 NB3 -1.1(5) . . . . ? B7 B8 B9 NB3 177.4(4) . . . . ? NB1 B8 B9 B4 179.3(4) . . . . ? B7 B8 B9 B4 -2.2(7) . . . . ? B2 NB3 B9 B8 -0.5(5) . . . . ? Co1 NB3 B9 B8 -173.0(3) . . . . ? B2 NB3 B9 B4 179.1(5) . . . . ? Co1 NB3 B9 B4 6.5(7) . . . . ? B9 NB3 B2 NB1 2.0(5) . . . . ? Co1 NB3 B2 NB1 175.4(3) . . . . ? B8 NB1 B2 NB3 -2.7(5) . . . . ? R1 NB1 B2 NB3 -168.9(4) . . . . ? B6 B5 B4 B9 0.0(7) . . . . ? B10 B5 B4 B9 179.3(4) . . . . ? B8 B9 B4 B5 1.3(7) . . . . ? NB3 B9 B4 B5 -178.1(5) . . . . ? B5 B6 B7 B8 -0.3(7) . . . . ? B11 B6 B7 B8 179.9(4) . . . . ? NB1 B8 B7 B6 179.8(5) . . . . ? B9 B8 B7 B6 1.6(7) . . . . ? N24 C19 C18 C60 161.0(4) . . . . ? C1 C19 C18 C60 -80.2(5) . . . . ? N24 C19 C18 C17 35.8(4) . . . . ? C1 C19 C18 C17 154.6(4) . . . . ? C16 C17 C18 C19 -31.0(4) . . . . ? C55 C17 C18 C19 -155.8(4) . . . . ? C54 C17 C18 C19 82.0(4) . . . . ? C16 C17 C18 C60 -155.3(4) . . . . ? C55 C17 C18 C60 79.9(5) . . . . ? C54 C17 C18 C60 -42.3(5) . . . . ? C19 C18 C60 C61 157.6(4) . . . . ? C17 C18 C60 C61 -84.6(5) . . . . ? C18 C60 C61 O62 -33.3(6) . . . . ? C18 C60 C61 N63 150.6(4) . . . . ? N22 C9 C8 C41 -93.4(4) . . . . ? C10 C9 C8 C41 87.9(5) . . . . ? N22 C9 C8 C7 29.1(5) . . . . ? C10 C9 C8 C7 -149.6(4) . . . . ? C9 C8 C41 C42 -158.6(4) . . . . ? C7 C8 C41 C42 90.0(5) . . . . ? C8 C41 C42 C43 154.3(4) . . . . ? C41 C42 C43 O44 -10.1(7) . . . . ? C41 C42 C43 N45 171.6(5) . . . . ? C5 C6 C7 C36 -37.3(7) . . . . ? N22 C6 C7 C36 145.0(4) . . . . ? C5 C6 C7 C8 -158.8(5) . . . . ? N22 C6 C7 C8 23.4(4) . . . . ? C5 C6 C7 C37 87.3(6) . . . . ? N22 C6 C7 C37 -90.5(4) . . . . ? C9 C8 C7 C36 -155.0(4) . . . . ? C41 C8 C7 C36 -40.2(5) . . . . ? C9 C8 C7 C6 -29.6(4) . . . . ? C41 C8 C7 C6 85.2(4) . . . . ? C9 C8 C7 C37 81.4(4) . . . . ? C41 C8 C7 C37 -163.7(4) . . . . ? C36 C7 C37 C38 -50.8(5) . . . . ? C6 C7 C37 C38 -179.2(4) . . . . ? C8 C7 C37 C38 73.1(5) . . . . ? C7 C37 C38 O39 -77.3(6) . . . . ? C7 C37 C38 N40 101.8(5) . . . . ? C3 C30 C31 C32 164.1(5) . . . . ? C30 C31 C32 O33 -7.3(9) . . . . ? C30 C31 C32 N34 173.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OR7 H207 O10W 0.84 1.99 2.751(5) 150.8 3_655 OR8 H208 O9W 0.84 1.92 2.737(5) 162.2 3_655 N59 H59 O10W 0.88 2.00 2.868(5) 169.7 3_655 N63 H63A O58 0.88 2.14 2.862(5) 138.7 2_566 N63 H63B O7W 0.88 2.64 3.350(6) 138.4 . C5L H5L O44 0.95 2.64 3.408(6) 138.2 3_545 C20 H20C NB3 0.98 2.54 3.202(6) 124.5 . N29 H29A O4W 0.88 2.23 3.021(6) 150.1 3_645 N29 H29B O7W 0.88 2.06 2.902(6) 160.5 . C3 H3 O28 1.00 2.22 3.004(6) 134.3 . N52 H52A O11W 0.88 2.07 2.902(8) 157.8 1_565 N52 H52A O16W 0.88 2.45 3.24(2) 149.6 1_565 N52 H52B O3W 0.88 2.17 3.007(7) 157.7 1_455 C56 H56A O10W 0.99 2.48 3.345(6) 146.4 3_655 C56 H56A OR7 0.99 2.58 3.307(6) 130.3 . PR2 H402 O1W 1.00 2.60 3.310(6) 128.3 . R1 H201 O28 1.00 2.19 3.118(6) 154.2 3_655 R5 H20D O51 0.99 2.46 3.399(6) 157.3 . C8 H8 O39 1.00 2.43 3.189(6) 131.8 . N45 H45A O1W 0.88 2.17 3.014(6) 161.1 4_574 N45 H45B O18W 0.88 2.16 2.993(8) 158.8 2_465 N45 H45B O17W 0.88 2.44 3.281(18) 159.6 2_465 N40 H40F O11W 0.88 2.18 2.903(8) 139.2 3 N40 H40G OP5 0.88 2.00 2.857(5) 165.4 3_645 N34 H34A O15W 0.88 2.47 3.099(8) 129.4 3_755 N34 H34A O17W 0.88 2.30 3.179(19) 174.3 2_565 N34 H34B O39 0.88 2.07 2.937(6) 169.4 1_655 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.429 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.092 _database_code_depnum_ccdc_archive 'CCDC 961228' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\users\admin\desktop\mik557\nowyfo~1\mik557_0 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H103 Co N13 O25 P' _chemical_formula_weight 1700.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21 21 21' 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 15.8339(4) _cell_length_b 21.8117(6) _cell_length_c 25.9778(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8971.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 2.324 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44222 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 67.54 _reflns_number_total 14407 _reflns_number_gt 12835 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1293P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(4) _refine_ls_number_reflns 14407 _refine_ls_number_parameters 1049 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 4.331 _refine_ls_shift/su_mean 0.013 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 0.26280(3) 0.39435(2) 0.75629(2) 0.01542(14) Uani 1 1 d . . . P1 P 0.52121(6) 0.23649(4) 0.47777(4) 0.0197(2) Uani 1 1 d . . . O1S O 0.76741(19) 0.25956(13) 0.46798(12) 0.0314(11) Uani 1.000(13) 1 d . . . R6 O 0.51455(17) 0.40811(13) 0.60095(11) 0.0246(6) Uani 1 1 d . . . O2S O 0.6117(2) 0.37958(15) 0.42043(13) 0.0365(12) Uani 1.000(12) 1 d . . . O2 O 0.50851(17) 0.26731(12) 0.53307(10) 0.0221(6) Uani 1 1 d . . . O3S O 0.2760(2) 0.25693(15) 0.42532(14) 0.0397(13) Uani 1.000(14) 1 d . . . O4 O 0.44146(17) 0.23969(12) 0.44748(11) 0.0248(6) Uani 1 1 d . . . O4S O 0.8339(2) 0.37561(16) 0.44934(12) 0.0339(12) Uani 0.976(13) 1 d P . . O3 O 0.53335(17) 0.16743(12) 0.49358(10) 0.0215(6) Uani 1 1 d . . . O5S O 0.3235(2) 0.77340(17) 0.83631(15) 0.0485(14) Uani 1.000(14) 1 d . . . O58 O 0.57678(18) 0.16885(14) 0.66412(12) 0.0298(7) Uani 1 1 d . . . O6S O 0.1372(3) 0.05640(18) 0.81609(15) 0.0451(15) Uani 0.917(14) 1 d P . . O62 O 0.24752(18) 0.10399(13) 0.64602(10) 0.0279(6) Uani 1 1 d . . . O7S O 0.0991(3) 0.1670(2) 0.87657(18) 0.0587(18) Uani 0.911(15) 1 d P . . O8S O 0.1417(4) 0.0792(3) 0.9509(2) 0.076(3) Uani 0.824(16) 1 d P . . O28 O -0.11507(18) 0.27016(15) 0.75934(14) 0.0395(8) Uani 1 1 d . . . O34 O -0.1608(2) 0.46739(15) 0.61092(14) 0.0443(9) Uani 1 1 d . . . O39 O 0.21200(18) 0.62269(14) 0.90451(12) 0.0317(7) Uani 1 1 d . . . O52 O 0.7493(2) 0.41749(15) 0.80585(14) 0.0442(8) Uani 1 1 d . . . O5 O 0.59795(17) 0.26274(12) 0.45310(10) 0.0243(6) Uani 1 1 d . . . R7 O 0.37510(17) 0.31570(12) 0.58740(10) 0.0215(6) Uani 1 1 d . . . O83A O 0.5199(3) 0.5719(2) 0.66009(19) 0.0618(15) Uiso 0.871(8) 1 d P . . R8 O 0.6351(2) 0.42762(15) 0.52121(14) 0.0441(9) Uani 1 1 d . . . O45 O 0.2432(2) 0.69399(19) 0.65295(14) 0.0534(10) Uani 1 1 d . . . O73A O 0.2058(4) -0.0953(3) 0.5070(3) 0.053(2) Uiso 0.586(9) 1 d PD A 1 B3 N 0.29433(19) 0.42511(14) 0.68322(12) 0.0176(6) Uani 1 1 d . . . B1 N 0.3759(2) 0.43490(14) 0.61392(12) 0.0189(6) Uani 1 1 d . . . N59 N 0.5004(2) 0.13810(15) 0.59554(13) 0.0231(7) Uani 1 1 d . . . H59 H 0.4495 0.1363 0.5820 0.028 Uiso 1 1 calc R . . N24 N 0.28938(18) 0.31154(13) 0.74223(12) 0.0163(6) Uani 1 1 d . . . N21 N 0.15492(19) 0.37126(14) 0.73327(12) 0.0174(6) Uani 1 1 d . . . N22 N 0.22127(19) 0.47449(14) 0.77272(12) 0.0189(6) Uani 1 1 d . . . N40 N 0.0701(2) 0.63020(17) 0.90869(14) 0.0273(8) Uani 1 1 d . . . H40A H 0.0731 0.6652 0.9255 0.033 Uiso 1 1 calc R . . H40B H 0.0206 0.6142 0.9012 0.033 Uiso 1 1 calc R . . N23 N 0.37758(19) 0.40979(14) 0.77558(12) 0.0185(6) Uani 1 1 d . . . N51 N 0.7271(2) 0.33160(18) 0.7584(2) 0.0448(10) Uani 1 1 d . . . H51A H 0.7573 0.3087 0.7793 0.054 Uiso 1 1 calc R . . H51B H 0.7033 0.3151 0.7311 0.054 Uiso 1 1 calc R . . N44 N 0.3747(3) 0.66036(19) 0.63771(15) 0.0372(9) Uani 1 1 d . . . H44A H 0.3777 0.6806 0.6084 0.045 Uiso 1 1 calc R . . H44B H 0.4177 0.6381 0.6482 0.045 Uiso 1 1 calc R . . N33 N -0.1289(2) 0.38587(17) 0.56261(14) 0.0309(8) Uani 1 1 d . . . H33A H -0.1413 0.4056 0.5340 0.037 Uiso 1 1 calc R . . H33B H -0.1115 0.3476 0.5613 0.037 Uiso 1 1 calc R . . N29 N -0.0631(2) 0.21268(19) 0.82226(15) 0.0367(9) Uani 1 1 d . . . H29A H -0.1141 0.2024 0.8325 0.044 Uiso 1 1 calc R . . H29B H -0.0186 0.1983 0.8385 0.044 Uiso 1 1 calc R . . N63 N 0.2163(2) 0.04797(15) 0.71642(15) 0.0274(8) Uani 1 1 d . . . H63A H 0.2289 0.0132 0.7010 0.033 Uiso 1 1 calc R . . H63B H 0.1989 0.0479 0.7486 0.033 Uiso 1 1 calc R . . C1 C 0.1479(2) 0.31070(16) 0.70728(14) 0.0177(7) Uani 1 1 d . . . C2 C 0.0509(2) 0.29456(17) 0.71531(15) 0.0190(8) Uani 1 1 d . . . C3 C 0.0107(2) 0.35991(16) 0.71838(15) 0.0186(8) Uani 1 1 d . . . H3 H -0.0372 0.3587 0.7434 0.022 Uiso 1 1 calc R . . C4 C 0.0817(2) 0.39665(17) 0.74172(14) 0.0177(7) Uani 1 1 d . . . C5 C 0.0699(2) 0.45389(17) 0.76776(14) 0.0191(7) Uani 1 1 d . . . C6 C 0.1367(2) 0.49078(17) 0.78006(14) 0.0190(8) Uani 1 1 d . . . C7 C 0.1344(2) 0.55411(17) 0.80513(15) 0.0199(8) Uani 1 1 d . . . C8 C 0.2233(2) 0.57968(17) 0.78983(15) 0.0210(8) Uani 1 1 d . . . H8 H 0.2471 0.6059 0.8179 0.025 Uiso 1 1 calc R . . C9 C 0.2721(2) 0.52085(16) 0.78479(14) 0.0197(8) Uani 1 1 d . . . C10 C 0.3575(2) 0.51736(17) 0.79344(15) 0.0213(8) Uani 1 1 d . . . H10 H 0.3859 0.5545 0.8016 0.026 Uiso 1 1 calc R . . C11 C 0.4059(2) 0.46440(18) 0.79129(15) 0.0209(8) Uani 1 1 d . . . C13 C 0.5260(2) 0.40082(18) 0.78459(16) 0.0227(8) Uani 1 1 d . . . H13 H 0.5625 0.3770 0.8088 0.027 Uiso 1 1 calc R . . C14 C 0.4428(2) 0.36720(18) 0.77585(15) 0.0210(8) Uani 1 1 d . . . C15 C 0.4365(2) 0.30579(17) 0.76520(15) 0.0199(8) Uani 1 1 d . . . C16 C 0.3572(2) 0.27903(16) 0.74961(14) 0.0173(7) Uani 1 1 d . . . C17 C 0.3383(2) 0.21038(16) 0.74267(15) 0.0195(8) Uani 1 1 d . . . C18 C 0.2520(2) 0.21291(15) 0.71410(14) 0.0176(7) Uani 1 1 d . . . H18 H 0.2630 0.2193 0.6766 0.021 Uiso 1 1 calc R . . C19 C 0.2135(2) 0.27170(16) 0.73614(14) 0.0171(7) Uani 1 1 d . . . H19 H 0.1907 0.2623 0.7712 0.020 Uiso 1 1 calc R . . C20 C 0.1729(2) 0.31578(17) 0.65062(14) 0.0193(8) Uani 1 1 d . . . H20A H 0.1417 0.3496 0.6346 0.029 Uiso 1 1 calc R . . H20B H 0.1593 0.2773 0.6329 0.029 Uiso 1 1 calc R . . H20C H 0.2336 0.3237 0.6480 0.029 Uiso 1 1 calc R . . C25 C 0.0143(2) 0.25458(18) 0.67240(16) 0.0235(8) Uani 1 1 d . . . H25A H 0.0441 0.2152 0.6715 0.035 Uiso 1 1 calc R . . H25B H 0.0211 0.2755 0.6393 0.035 Uiso 1 1 calc R . . H25C H -0.0459 0.2474 0.6789 0.035 Uiso 1 1 calc R . . C26 C 0.0381(2) 0.26320(18) 0.76784(16) 0.0228(8) Uani 1 1 d . . . H26A H 0.0701 0.2242 0.7678 0.027 Uiso 1 1 calc R . . H26B H 0.0630 0.2898 0.7947 0.027 Uiso 1 1 calc R . . C27 C -0.0534(3) 0.24917(19) 0.78301(17) 0.0263(9) Uani 1 1 d . . . C30 C -0.0196(2) 0.39132(18) 0.66915(15) 0.0217(8) Uani 1 1 d . . . H30A H -0.0137 0.4362 0.6734 0.026 Uiso 1 1 calc R . . H30B H 0.0176 0.3788 0.6404 0.026 Uiso 1 1 calc R . . C31 C -0.1110(3) 0.3771(2) 0.65440(16) 0.0264(9) Uani 1 1 d . . . H31A H -0.1170 0.3326 0.6475 0.032 Uiso 1 1 calc R . . H31B H -0.1489 0.3878 0.6833 0.032 Uiso 1 1 calc R . . C32 C -0.1364(3) 0.4133(2) 0.60672(17) 0.0287(9) Uani 1 1 d . . . C35 C -0.0207(3) 0.47164(19) 0.78143(17) 0.0273(9) Uani 1 1 d . . . H35A H -0.0201 0.5010 0.8100 0.041 Uiso 1 1 calc R . . H35B H -0.0522 0.4349 0.7917 0.041 Uiso 1 1 calc R . . H35C H -0.0479 0.4904 0.7514 0.041 Uiso 1 1 calc R . . C36 C 0.0628(2) 0.59714(18) 0.78820(16) 0.0246(8) Uani 1 1 d . . . H36A H 0.0520 0.5917 0.7513 0.037 Uiso 1 1 calc R . . H36B H 0.0791 0.6397 0.7948 0.037 Uiso 1 1 calc R . . H36C H 0.0114 0.5874 0.8076 0.037 Uiso 1 1 calc R . . C37 C 0.1317(3) 0.54303(18) 0.86469(15) 0.0230(8) Uani 1 1 d . . . H37A H 0.0775 0.5232 0.8738 0.028 Uiso 1 1 calc R . . H37B H 0.1779 0.5147 0.8744 0.028 Uiso 1 1 calc R . . C38 C 0.1406(3) 0.60150(19) 0.89462(15) 0.0235(8) Uani 1 1 d . . . C41 C 0.2210(2) 0.61520(17) 0.73780(16) 0.0236(8) Uani 1 1 d . . . H41A H 0.1883 0.5910 0.7125 0.028 Uiso 1 1 calc R . . H41B H 0.1911 0.6546 0.7430 0.028 Uiso 1 1 calc R . . C42 C 0.3082(3) 0.6282(2) 0.71577(19) 0.0319(10) Uani 1 1 d . . . H42A H 0.3413 0.6518 0.7413 0.038 Uiso 1 1 calc R . . H42B H 0.3378 0.5888 0.7099 0.038 Uiso 1 1 calc R . . C43 C 0.3052(3) 0.6634(2) 0.66602(18) 0.0334(10) Uani 1 1 d . . . C46 C 0.4920(3) 0.4503(2) 0.86882(18) 0.0384(11) Uani 1 1 d . . . H46A H 0.4628 0.4849 0.8849 0.058 Uiso 1 1 calc R . . H46B H 0.5494 0.4472 0.8826 0.058 Uiso 1 1 calc R . . H46C H 0.4612 0.4123 0.8762 0.058 Uiso 1 1 calc R . . C47 C 0.5471(3) 0.51835(19) 0.7991(2) 0.0356(11) Uani 1 1 d . . . H47A H 0.5476 0.5261 0.7619 0.053 Uiso 1 1 calc R . . H47B H 0.6051 0.5129 0.8114 0.053 Uiso 1 1 calc R . . H47C H 0.5212 0.5533 0.8169 0.053 Uiso 1 1 calc R . . C48 C 0.5695(2) 0.40610(19) 0.73114(17) 0.0268(9) Uani 1 1 d . . . H48A H 0.5655 0.3658 0.7138 0.032 Uiso 1 1 calc R . . H48B H 0.5371 0.4358 0.7101 0.032 Uiso 1 1 calc R . . C49 C 0.6629(3) 0.4260(2) 0.73105(19) 0.0339(10) Uani 1 1 d . . . C50 C 0.7173(3) 0.3918(2) 0.7681(2) 0.0370(11) Uani 1 1 d . . . C53 C 0.5147(2) 0.26539(18) 0.77141(18) 0.0276(9) Uani 1 1 d . . . H53A H 0.5364 0.2542 0.7374 0.041 Uiso 1 1 calc R . . H53B H 0.4995 0.2282 0.7904 0.041 Uiso 1 1 calc R . . H53C H 0.5581 0.2879 0.7904 0.041 Uiso 1 1 calc R . . C54 C 0.3301(3) 0.18265(18) 0.79710(15) 0.0234(8) Uani 1 1 d . . . H54A H 0.3828 0.1892 0.8161 0.035 Uiso 1 1 calc R . . H54B H 0.3190 0.1386 0.7944 0.035 Uiso 1 1 calc R . . H54C H 0.2834 0.2025 0.8154 0.035 Uiso 1 1 calc R . . C55 C 0.4038(2) 0.17250(17) 0.71238(16) 0.0211(8) Uani 1 1 d . . . H55A H 0.4545 0.1672 0.7342 0.025 Uiso 1 1 calc R . . H55B H 0.3799 0.1313 0.7060 0.025 Uiso 1 1 calc R . . C56 C 0.4314(2) 0.19982(17) 0.66084(16) 0.0233(8) Uani 1 1 d . . . H56A H 0.3849 0.1957 0.6356 0.028 Uiso 1 1 calc R . . H56B H 0.4434 0.2440 0.6653 0.028 Uiso 1 1 calc R . . C57 C 0.5099(3) 0.16766(18) 0.64031(15) 0.0232(8) Uani 1 1 d . . . C60 C 0.1948(2) 0.15743(17) 0.72033(16) 0.0221(8) Uani 1 1 d . . . H60A H 0.1375 0.1686 0.7084 0.027 Uiso 1 1 calc R . . H60B H 0.1909 0.1473 0.7574 0.027 Uiso 1 1 calc R . . C61 C 0.2235(2) 0.10028(16) 0.69125(15) 0.0193(7) Uani 1 1 d . . . PR1 C 0.5692(3) 0.10894(19) 0.56821(16) 0.0248(8) Uani 1 1 d . . . HR1A H 0.5490 0.0698 0.5534 0.030 Uiso 1 1 calc R . . HR1B H 0.6150 0.0994 0.5929 0.030 Uiso 1 1 calc R . . PR2 C 0.6042(2) 0.14860(17) 0.52547(15) 0.0209(8) Uani 1 1 d . . . HR2 H 0.6323 0.1856 0.5405 0.025 Uiso 1 1 calc R . . PR3 C 0.6664(3) 0.11386(19) 0.49188(16) 0.0266(9) Uani 1 1 d . . . HR3A H 0.6366 0.0813 0.4733 0.040 Uiso 1 1 calc R . . HR3B H 0.7105 0.0957 0.5135 0.040 Uiso 1 1 calc R . . HR3C H 0.6922 0.1421 0.4671 0.040 Uiso 1 1 calc R . . R3 C 0.5017(2) 0.33224(17) 0.53586(15) 0.0210(8) Uani 1 1 d . . . H3A H 0.5184 0.3508 0.5022 0.025 Uiso 1 1 calc R . . R4 C 0.5584(3) 0.35693(18) 0.57864(17) 0.0250(9) Uani 1 1 d . . . H4 H 0.5681 0.3246 0.6052 0.030 Uiso 1 1 calc R . . R1 C 0.4363(2) 0.41619(17) 0.57560(15) 0.0209(8) Uani 1 1 d . . . H1 H 0.4416 0.4485 0.5484 0.025 Uiso 1 1 calc R . . R2 C 0.4133(2) 0.35403(17) 0.55083(15) 0.0203(8) Uani 1 1 d . . . H2 H 0.3766 0.3596 0.5199 0.024 Uiso 1 1 calc R . . R5 C 0.6437(3) 0.3808(2) 0.5581(2) 0.0371(11) Uani 1 1 d . . . H5A H 0.6775 0.3966 0.5874 0.044 Uiso 1 1 calc R . . H5B H 0.6752 0.3463 0.5426 0.044 Uiso 1 1 calc R . . B2 C 0.3654(2) 0.40862(16) 0.66033(14) 0.0185(7) Uani 1 1 d . . . H2A H 0.4050 0.3811 0.6751 0.022 Uiso 1 1 calc R . . B9 C 0.2537(2) 0.46403(16) 0.64844(14) 0.0182(7) Uani 1 1 d . . . B4 C 0.1762(2) 0.49369(17) 0.64982(15) 0.0210(8) Uani 1 1 d . . . H4A H 0.1403 0.4894 0.6789 0.025 Uiso 1 1 calc R . . B5 C 0.1517(3) 0.52935(18) 0.60868(17) 0.0259(9) Uani 1 1 d . . . B6 C 0.2037(3) 0.53621(19) 0.56501(18) 0.0293(9) Uani 1 1 d . . . B7 C 0.2815(3) 0.50656(17) 0.56255(16) 0.0259(9) Uani 1 1 d . . . H7 H 0.3177 0.5108 0.5336 0.031 Uiso 1 1 calc R . . B8 C 0.3037(3) 0.47023(16) 0.60488(16) 0.0212(8) Uani 1 1 d . . . B10 C 0.0666(3) 0.5612(2) 0.61029(18) 0.0358(10) Uani 1 1 d . . . H10A H 0.0317 0.5469 0.5815 0.054 Uiso 1 1 calc R . . H10B H 0.0748 0.6056 0.6075 0.054 Uiso 1 1 calc R . . H10C H 0.0383 0.5517 0.6429 0.054 Uiso 1 1 calc R . . B11 C 0.1764(4) 0.5755(3) 0.5205(2) 0.0538(15) Uani 1 1 d . . . H11A H 0.2140 0.5683 0.4911 0.081 Uiso 1 1 calc R . . H11B H 0.1792 0.6188 0.5304 0.081 Uiso 1 1 calc R . . H11C H 0.1183 0.5650 0.5108 0.081 Uiso 1 1 calc R . . L1 C 0.2356(2) 0.36879(17) 0.82277(15) 0.0215(8) Uani 1 1 d . . . L2 C 0.2167(3) 0.3478(2) 0.86447(16) 0.0314(10) Uani 1 1 d . . . L3 C 0.1942(4) 0.3226(2) 0.91316(19) 0.0479(14) Uani 1 1 d . . . L4 C 0.2383(5) 0.2686(3) 0.9314(2) 0.0633(17) Uani 1 1 d . . . H4B H 0.2825 0.2514 0.9113 0.076 Uiso 1 1 calc R . . L5 C 0.2164(5) 0.2418(3) 0.9778(3) 0.0681(19) Uani 1 1 d . . . H5 H 0.2433 0.2050 0.9886 0.082 Uiso 1 1 calc R . . L6 C 0.1563(5) 0.2681(3) 1.0080(2) 0.0597(17) Uani 1 1 d . . . L7 C 0.1139(4) 0.3222(4) 0.9917(2) 0.0619(17) Uani 1 1 d . . . H7A H 0.0704 0.3398 1.0121 0.074 Uiso 1 1 calc R . . L8 C 0.1380(4) 0.3490(3) 0.9448(2) 0.0558(15) Uani 1 1 d . . . H8A H 0.1138 0.3871 0.9351 0.067 Uiso 1 1 calc R . . L9 O 0.1286(4) 0.2463(2) 1.05419(17) 0.0780(15) Uani 1 1 d . . . L10 C 0.1788(8) 0.1967(4) 1.0760(3) 0.111(4) Uani 1 1 d . . . H10D H 0.1720 0.1597 1.0550 0.166 Uiso 1 1 calc R . . H10E H 0.1597 0.1883 1.1112 0.166 Uiso 1 1 calc R . . H10F H 0.2385 0.2086 1.0766 0.166 Uiso 1 1 calc R . . C80A C 0.5621(4) 0.5603(3) 0.6220(2) 0.0442(15) Uiso 0.871(8) 1 d P . . C81A C 0.5248(5) 0.5624(3) 0.5694(3) 0.0550(18) Uiso 0.871(8) 1 d P . . H81A H 0.4637 0.5557 0.5715 0.083 Uiso 0.871(8) 1 calc PR . . H81B H 0.5503 0.5303 0.5481 0.083 Uiso 0.871(8) 1 calc PR . . H81C H 0.5359 0.6026 0.5539 0.083 Uiso 0.871(8) 1 calc PR . . C82A C 0.6496(5) 0.5425(4) 0.6247(3) 0.064(2) Uiso 0.871(8) 1 d P . . H82A H 0.6659 0.5368 0.6607 0.096 Uiso 0.871(8) 1 calc PR . . H82B H 0.6847 0.5745 0.6091 0.096 Uiso 0.871(8) 1 calc PR . . H82C H 0.6576 0.5039 0.6059 0.096 Uiso 0.871(8) 1 calc PR . . C70A C 0.1969(6) -0.0621(4) 0.5446(4) 0.049(2) Uiso 0.586(9) 1 d PD A 1 C71A C 0.2658(8) -0.0233(6) 0.5649(5) 0.073(3) Uiso 0.586(9) 1 d PD A 1 H71A H 0.3183 -0.0325 0.5465 0.109 Uiso 0.586(9) 1 calc PR A 1 H71B H 0.2735 -0.0316 0.6017 0.109 Uiso 0.586(9) 1 calc PR A 1 H71C H 0.2513 0.0200 0.5600 0.109 Uiso 0.586(9) 1 calc PR A 1 O78A O 0.5689(7) 0.7029(5) 0.5677(4) 0.082(3) Uiso 0.500(9) 1 d P . . C75A C 0.5633(8) 0.7530(6) 0.5395(5) 0.060(3) Uiso 0.500(9) 1 d P . . C77A C 0.5564(9) 0.8087(6) 0.5689(5) 0.062(3) Uiso 0.500(9) 1 d P . . H77A H 0.5408 0.7988 0.6044 0.093 Uiso 0.500(9) 1 calc PR . . H77B H 0.5129 0.8350 0.5537 0.093 Uiso 0.500(9) 1 calc PR . . H77C H 0.6108 0.8302 0.5686 0.093 Uiso 0.500(9) 1 calc PR . . C76A C 0.5721(12) 0.7538(9) 0.4844(7) 0.092(5) Uiso 0.500(9) 1 d P . . H76A H 0.5814 0.7119 0.4718 0.138 Uiso 0.500(9) 1 calc PR . . H76B H 0.6204 0.7796 0.4749 0.138 Uiso 0.500(9) 1 calc PR . . H76C H 0.5206 0.7704 0.4688 0.138 Uiso 0.500(9) 1 calc PR . . C72A C 0.1056(11) -0.0611(8) 0.5741(6) 0.099(5) Uiso 0.586(9) 1 d PD A 1 H72A H 0.0822 -0.0195 0.5730 0.149 Uiso 0.586(9) 1 calc PR A 1 H72B H 0.1132 -0.0738 0.6100 0.149 Uiso 0.586(9) 1 calc PR A 1 H72C H 0.0667 -0.0895 0.5569 0.149 Uiso 0.586(9) 1 calc PR A 1 C12 C 0.4960(3) 0.46024(19) 0.81030(16) 0.0250(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0148(3) 0.0128(3) 0.0187(3) -0.0020(2) 0.0010(2) 0.0011(2) P1 0.0218(5) 0.0166(4) 0.0208(5) -0.0005(4) 0.0017(4) 0.0030(4) O1S 0.0288(17) 0.0299(17) 0.0355(19) -0.0005(13) 0.0007(13) 0.0017(12) R6 0.0209(13) 0.0233(14) 0.0294(14) -0.0076(12) 0.0036(12) 0.0018(11) O2S 0.0317(18) 0.0331(19) 0.045(2) 0.0085(15) 0.0072(14) 0.0017(13) O2 0.0310(14) 0.0124(12) 0.0229(13) 0.0033(11) 0.0034(11) 0.0041(10) O3S 0.035(2) 0.0337(19) 0.050(2) 0.0045(15) -0.0013(15) 0.0018(14) O4 0.0263(14) 0.0213(13) 0.0268(15) 0.0015(12) -0.0046(12) 0.0016(11) O4S 0.0299(18) 0.043(2) 0.0293(19) 0.0052(14) -0.0043(13) -0.0032(13) O3 0.0239(14) 0.0165(13) 0.0242(14) -0.0032(11) -0.0007(11) 0.0034(10) O5S 0.046(2) 0.041(2) 0.059(3) -0.0018(18) 0.0037(18) -0.0001(16) O58 0.0257(15) 0.0297(15) 0.0340(16) -0.0046(13) 0.0017(13) 0.0054(12) O6S 0.055(3) 0.040(2) 0.040(2) 0.0071(17) 0.0057(18) 0.0007(18) O62 0.0261(14) 0.0327(15) 0.0249(14) -0.0044(12) 0.0000(12) 0.0026(12) O7S 0.043(3) 0.067(3) 0.066(3) 0.013(2) -0.013(2) -0.001(2) O8S 0.104(5) 0.047(3) 0.077(4) -0.011(3) 0.001(3) -0.022(3) O28 0.0207(14) 0.0380(17) 0.060(2) 0.0169(17) 0.0017(15) 0.0026(13) O34 0.060(2) 0.0287(17) 0.045(2) -0.0081(15) -0.0204(17) 0.0185(15) O39 0.0247(15) 0.0351(16) 0.0354(16) -0.0132(14) -0.0049(13) 0.0008(12) O52 0.0389(19) 0.0313(17) 0.062(2) 0.0004(16) -0.0132(17) -0.0004(14) O5 0.0287(14) 0.0200(13) 0.0242(14) 0.0001(12) 0.0061(12) 0.0027(11) R7 0.0217(13) 0.0177(13) 0.0250(14) 0.0008(11) 0.0057(11) -0.0043(10) R8 0.052(2) 0.0310(17) 0.049(2) -0.0013(16) 0.0213(17) -0.0110(15) O45 0.044(2) 0.067(2) 0.050(2) 0.0266(19) 0.0149(18) 0.0267(19) B3 0.0180(15) 0.0151(14) 0.0196(15) -0.0049(12) 0.0028(12) -0.0020(12) B1 0.0201(16) 0.0144(14) 0.0222(15) 0.0016(12) 0.0057(13) 0.0021(12) N59 0.0231(18) 0.0212(16) 0.0251(17) 0.0011(14) 0.0040(14) 0.0058(13) N24 0.0158(14) 0.0145(14) 0.0185(14) -0.0017(12) 0.0030(12) -0.0025(11) N21 0.0200(15) 0.0161(15) 0.0163(15) 0.0014(12) 0.0016(12) -0.0005(12) N22 0.0150(15) 0.0186(15) 0.0230(16) -0.0022(13) 0.0010(13) 0.0011(12) N40 0.0219(17) 0.0309(18) 0.0293(18) -0.0136(15) 0.0005(14) 0.0004(14) N23 0.0176(15) 0.0163(15) 0.0214(16) -0.0028(12) 0.0008(13) 0.0033(12) N51 0.0259(19) 0.0291(19) 0.079(3) -0.003(2) -0.005(2) 0.0024(15) N44 0.036(2) 0.039(2) 0.036(2) 0.0004(18) 0.0112(18) 0.0049(17) N33 0.0341(19) 0.0274(19) 0.0312(19) -0.0006(16) -0.0046(16) 0.0049(15) N29 0.0238(18) 0.050(2) 0.036(2) 0.0159(19) 0.0027(16) -0.0095(17) N63 0.0275(18) 0.0165(15) 0.038(2) -0.0011(15) 0.0024(16) -0.0038(13) C1 0.0194(18) 0.0129(17) 0.0209(18) -0.0016(15) 0.0007(15) -0.0021(14) C2 0.0131(17) 0.0192(18) 0.0246(19) -0.0014(16) 0.0022(15) -0.0004(14) C3 0.0177(17) 0.0152(17) 0.0230(18) -0.0015(15) 0.0026(15) -0.0016(14) C4 0.0167(17) 0.0197(17) 0.0166(17) 0.0029(15) -0.0003(14) -0.0014(14) C5 0.0197(18) 0.0185(17) 0.0191(18) -0.0013(15) 0.0017(15) 0.0029(14) C6 0.0201(18) 0.0186(18) 0.0181(18) -0.0020(15) 0.0019(15) 0.0031(14) C7 0.0195(18) 0.0168(18) 0.0235(19) -0.0054(15) 0.0008(15) 0.0029(15) C8 0.0179(18) 0.0176(17) 0.028(2) -0.0036(16) -0.0011(16) 0.0028(14) C9 0.0238(19) 0.0153(17) 0.0200(18) -0.0030(15) 0.0002(16) 0.0016(15) C10 0.0213(19) 0.0131(17) 0.029(2) -0.0065(16) 0.0013(16) -0.0008(14) C11 0.0211(19) 0.0182(18) 0.023(2) -0.0039(16) 0.0002(16) -0.0019(15) C13 0.0172(18) 0.0186(18) 0.032(2) -0.0025(16) -0.0041(16) 0.0017(15) C14 0.0198(18) 0.0185(18) 0.0248(19) -0.0004(15) -0.0005(16) 0.0034(15) C15 0.0192(18) 0.0146(17) 0.026(2) -0.0017(15) -0.0010(15) 0.0011(14) C16 0.0184(17) 0.0156(17) 0.0179(17) 0.0014(14) 0.0029(15) -0.0009(13) C17 0.0207(18) 0.0122(16) 0.026(2) 0.0015(15) 0.0049(16) -0.0002(13) C18 0.0220(19) 0.0108(16) 0.0201(17) -0.0002(14) 0.0027(15) -0.0002(14) C19 0.0144(16) 0.0156(17) 0.0212(18) -0.0024(14) 0.0019(14) -0.0027(13) C20 0.0179(17) 0.0187(18) 0.0214(19) -0.0014(15) 0.0024(15) 0.0002(14) C25 0.0190(18) 0.0205(19) 0.031(2) -0.0055(16) 0.0014(16) -0.0032(15) C26 0.0186(18) 0.0185(17) 0.031(2) 0.0050(17) 0.0020(16) 0.0004(14) C27 0.022(2) 0.023(2) 0.034(2) 0.0005(17) 0.0044(17) -0.0028(15) C30 0.0208(18) 0.0179(17) 0.0265(19) -0.0032(16) -0.0023(16) -0.0021(15) C31 0.0190(19) 0.030(2) 0.030(2) 0.0015(18) -0.0021(17) -0.0012(16) C32 0.0180(19) 0.029(2) 0.039(2) -0.0054(19) -0.0096(18) 0.0042(16) C35 0.0182(19) 0.027(2) 0.036(2) -0.0103(18) 0.0032(18) 0.0012(16) C36 0.0222(19) 0.0216(19) 0.030(2) -0.0035(17) 0.0005(16) 0.0044(16) C37 0.025(2) 0.0191(19) 0.025(2) -0.0041(16) -0.0010(17) 0.0040(15) C38 0.025(2) 0.025(2) 0.0202(19) -0.0050(16) -0.0010(16) 0.0037(16) C41 0.0218(19) 0.0187(17) 0.030(2) -0.0031(16) 0.0026(16) 0.0036(14) C42 0.026(2) 0.029(2) 0.041(3) 0.008(2) 0.0063(19) 0.0019(17) C43 0.033(2) 0.033(2) 0.035(2) 0.002(2) 0.008(2) 0.0029(19) C46 0.032(2) 0.047(3) 0.036(2) -0.016(2) -0.009(2) 0.010(2) C47 0.0163(19) 0.023(2) 0.068(3) -0.014(2) -0.002(2) 0.0010(16) C48 0.0194(19) 0.026(2) 0.035(2) -0.0039(18) 0.0025(17) -0.0016(15) C49 0.020(2) 0.031(2) 0.050(3) -0.004(2) 0.0049(19) -0.0014(17) C50 0.019(2) 0.028(2) 0.064(3) -0.002(2) 0.006(2) 0.0012(16) C53 0.0180(18) 0.0199(19) 0.045(2) -0.0046(18) -0.0070(18) 0.0026(15) C54 0.029(2) 0.0184(18) 0.023(2) 0.0033(16) 0.0055(16) 0.0012(15) C55 0.0185(18) 0.0151(17) 0.030(2) -0.0005(16) 0.0019(16) 0.0033(14) C56 0.024(2) 0.0181(18) 0.028(2) 0.0017(16) 0.0034(17) 0.0070(15) C57 0.026(2) 0.0174(18) 0.026(2) 0.0044(16) 0.0039(17) 0.0002(15) C60 0.0224(19) 0.0197(19) 0.024(2) -0.0010(16) 0.0046(16) 0.0010(15) C61 0.0162(17) 0.0151(17) 0.0265(19) -0.0025(15) -0.0039(15) -0.0009(14) PR1 0.027(2) 0.0224(19) 0.025(2) 0.0011(17) 0.0046(16) 0.0079(16) PR2 0.0216(18) 0.0176(17) 0.0235(19) 0.0007(16) -0.0016(16) 0.0040(14) PR3 0.027(2) 0.025(2) 0.027(2) -0.0023(17) 0.0013(17) 0.0073(16) R3 0.024(2) 0.0127(17) 0.026(2) -0.0008(15) 0.0086(16) 0.0005(14) R4 0.023(2) 0.0212(19) 0.031(2) -0.0043(17) 0.0012(17) 0.0071(16) R1 0.0205(18) 0.0165(17) 0.0257(19) 0.0021(15) 0.0052(16) 0.0007(14) R2 0.0245(19) 0.0176(18) 0.0188(18) 0.0006(15) 0.0001(15) 0.0030(15) R5 0.024(2) 0.039(3) 0.049(3) -0.014(2) 0.009(2) -0.0005(18) B2 0.0185(18) 0.0151(17) 0.0220(18) -0.0043(15) 0.0019(15) 0.0015(13) B9 0.0216(19) 0.0139(16) 0.0190(18) -0.0030(14) 0.0030(15) -0.0021(14) B4 0.0204(18) 0.0179(18) 0.025(2) -0.0046(16) 0.0011(16) -0.0023(14) B5 0.029(2) 0.0197(19) 0.029(2) 0.0016(17) -0.0039(17) 0.0051(16) B6 0.031(2) 0.022(2) 0.035(2) -0.0003(18) 0.0026(19) 0.0073(16) B7 0.032(2) 0.0170(17) 0.028(2) 0.0043(16) 0.0058(18) 0.0019(16) B8 0.0242(19) 0.0113(16) 0.028(2) 0.0000(15) 0.0001(16) -0.0001(14) B10 0.032(2) 0.042(3) 0.034(2) 0.000(2) 0.002(2) 0.013(2) B11 0.064(4) 0.054(3) 0.044(3) 0.024(3) 0.012(3) 0.030(3) L1 0.0210(18) 0.0186(17) 0.025(2) -0.0026(15) 0.0002(16) 0.0018(15) L2 0.043(3) 0.030(2) 0.021(2) -0.0026(18) -0.0002(19) -0.0065(19) L3 0.084(4) 0.036(3) 0.025(2) -0.005(2) 0.005(2) -0.025(3) L4 0.096(5) 0.050(3) 0.044(3) 0.009(3) 0.016(3) 0.017(3) L5 0.095(5) 0.048(3) 0.061(4) 0.008(3) 0.018(4) 0.018(3) L6 0.095(5) 0.046(3) 0.039(3) 0.002(3) 0.014(3) -0.003(3) L7 0.062(4) 0.091(5) 0.033(3) -0.001(3) 0.005(3) 0.007(3) L8 0.055(3) 0.071(4) 0.041(3) 0.018(3) 0.011(3) 0.012(3) L9 0.122(4) 0.064(3) 0.048(2) 0.005(2) 0.017(3) -0.013(3) L10 0.168(10) 0.083(6) 0.081(6) 0.042(5) 0.037(6) 0.019(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 L1 1.865(4) . ? Co1 N21 1.879(3) . ? Co1 N24 1.890(3) . ? Co1 N23 1.915(3) . ? Co1 N22 1.916(3) . ? Co1 B3 2.074(3) . ? P1 O5 1.488(3) . ? P1 O4 1.490(3) . ? P1 O3 1.573(3) . ? P1 O2 1.599(3) . ? R6 R1 1.413(5) . ? R6 R4 1.437(5) . ? O2 R3 1.422(4) . ? O3 PR2 1.454(5) . ? O58 C57 1.227(5) . ? O62 C61 1.238(5) . ? O28 C27 1.242(5) . ? O34 C32 1.246(5) . ? O39 C38 1.248(5) . ? O52 C50 1.238(6) . ? R7 R2 1.403(5) . ? O83A C80A 1.221(8) . ? R8 R5 1.407(6) . ? O45 C43 1.234(6) . ? O73A C70A 1.223(11) . ? B3 B2 1.323(5) . ? B3 B9 1.397(5) . ? B1 B2 1.345(5) . ? B1 B8 1.398(5) . ? B1 R1 1.440(5) . ? N59 C57 1.338(5) . ? N59 PR1 1.447(5) . ? N24 C16 1.301(5) . ? N24 C19 1.491(4) . ? N21 C4 1.303(5) . ? N21 C1 1.488(5) . ? N22 C9 1.329(5) . ? N22 C6 1.398(5) . ? N40 C38 1.330(5) . ? N23 C11 1.337(5) . ? N23 C14 1.390(5) . ? N51 C50 1.347(6) . ? N44 C43 1.325(6) . ? N33 C32 1.298(6) . ? N29 C27 1.302(6) . ? N63 C61 1.320(5) . ? C1 C20 1.528(5) . ? C1 C19 1.538(5) . ? C1 C2 1.588(5) . ? C2 C25 1.530(5) . ? C2 C26 1.540(5) . ? C2 C3 1.563(5) . ? C3 C4 1.508(5) . ? C3 C30 1.529(5) . ? C4 C5 1.432(5) . ? C5 C6 1.367(5) . ? C5 C35 1.527(5) . ? C6 C7 1.528(5) . ? C7 C36 1.537(5) . ? C7 C8 1.565(5) . ? C7 C37 1.567(5) . ? C8 C9 1.504(5) . ? C8 C41 1.558(6) . ? C9 C10 1.373(6) . ? C10 C11 1.388(5) . ? C11 C12 1.512(6) . ? C13 C14 1.524(5) . ? C13 C12 1.533(6) . ? C13 C48 1.554(6) . ? C14 C15 1.371(5) . ? C15 C16 1.443(5) . ? C15 C53 1.528(5) . ? C16 C17 1.538(5) . ? C17 C55 1.542(5) . ? C17 C54 1.543(5) . ? C17 C18 1.556(5) . ? C18 C60 1.520(5) . ? C18 C19 1.531(5) . ? C26 C27 1.531(5) . ? C30 C31 1.529(5) . ? C31 C32 1.523(6) . ? C37 C38 1.500(5) . ? C41 C42 1.522(6) . ? C42 C43 1.504(6) . ? C46 C12 1.537(6) . ? C47 C12 1.531(6) . ? C48 C49 1.542(5) . ? C49 C50 1.491(7) . ? C55 C56 1.529(5) . ? C56 C57 1.524(5) . ? C60 C61 1.527(5) . ? PR1 PR2 1.513(5) . ? PR2 PR3 1.518(5) . ? R3 R2 1.528(5) . ? R3 R4 1.527(6) . ? R4 R5 1.543(6) . ? R1 R2 1.544(5) . ? B9 B4 1.388(5) . ? B9 B8 1.388(6) . ? B4 B5 1.378(6) . ? B5 B6 1.410(6) . ? B5 B10 1.517(6) . ? B6 B7 1.392(6) . ? B6 B11 1.503(6) . ? B7 B8 1.400(6) . ? L1 L2 1.214(6) . ? L2 L3 1.425(6) . ? L3 L8 1.340(8) . ? L3 L4 1.448(9) . ? L4 L5 1.385(9) . ? L5 L6 1.359(9) . ? L6 L9 1.364(7) . ? L6 L7 1.420(10) . ? L7 L8 1.407(8) . ? L9 L10 1.459(10) . ? C80A C82A 1.441(10) . ? C80A C81A 1.490(9) . ? C70A C71A 1.479(16) . ? C70A C72A 1.637(19) . ? O78A C75A 1.319(17) . ? C75A C76A 1.44(2) . ? C75A C77A 1.439(18) . ? 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 L1 Co1 N21 90.28(15) . . ? L1 Co1 N24 86.83(14) . . ? N21 Co1 N24 83.39(13) . . ? L1 Co1 N23 91.68(15) . . ? N21 Co1 N23 173.39(13) . . ? N24 Co1 N23 90.42(13) . . ? L1 Co1 N22 89.26(15) . . ? N21 Co1 N22 90.20(13) . . ? N24 Co1 N22 172.46(13) . . ? N23 Co1 N22 96.14(13) . . ? L1 Co1 B3 178.36(15) . . ? N21 Co1 B3 90.82(13) . . ? N24 Co1 B3 94.51(13) . . ? N23 Co1 B3 87.37(13) . . ? N22 Co1 B3 89.51(13) . . ? O5 P1 O4 116.54(16) . . ? O5 P1 O3 112.39(15) . . ? O4 P1 O3 106.64(15) . . ? O5 P1 O2 109.15(15) . . ? O4 P1 O2 110.38(16) . . ? O3 P1 O2 100.57(14) . . ? R1 R6 R4 109.4(3) . . ? R3 O2 P1 118.3(2) . . ? PR2 O3 P1 120.9(2) . . ? B2 B3 B9 105.5(3) . . ? B2 B3 Co1 121.9(3) . . ? B9 B3 Co1 132.7(2) . . ? B2 B1 B8 106.6(3) . . ? B2 B1 R1 125.5(3) . . ? B8 B1 R1 125.7(3) . . ? C57 N59 PR1 123.6(3) . . ? C16 N24 C19 111.3(3) . . ? C16 N24 Co1 132.6(3) . . ? C19 N24 Co1 113.4(2) . . ? C4 N21 C1 112.8(3) . . ? C4 N21 Co1 129.9(3) . . ? C1 N21 Co1 116.8(2) . . ? C9 N22 C6 110.7(3) . . ? C9 N22 Co1 122.6(2) . . ? C6 N22 Co1 126.2(3) . . ? C11 N23 C14 110.2(3) . . ? C11 N23 Co1 123.7(3) . . ? C14 N23 Co1 126.1(3) . . ? N21 C1 C20 110.7(3) . . ? N21 C1 C19 102.7(3) . . ? C20 C1 C19 109.5(3) . . ? N21 C1 C2 102.1(3) . . ? C20 C1 C2 113.1(3) . . ? C19 C1 C2 117.8(3) . . ? C25 C2 C26 110.0(3) . . ? C25 C2 C3 113.7(3) . . ? C26 C2 C3 107.8(3) . . ? C25 C2 C1 113.4(3) . . ? C26 C2 C1 110.0(3) . . ? C3 C2 C1 101.4(3) . . ? C4 C3 C30 109.4(3) . . ? C4 C3 C2 101.6(3) . . ? C30 C3 C2 119.6(3) . . ? N21 C4 C5 124.5(3) . . ? N21 C4 C3 111.7(3) . . ? C5 C4 C3 123.7(3) . . ? C6 C5 C4 121.4(3) . . ? C6 C5 C35 121.6(3) . . ? C4 C5 C35 117.0(3) . . ? C5 C6 N22 124.1(3) . . ? C5 C6 C7 127.8(3) . . ? N22 C6 C7 108.1(3) . . ? C6 C7 C36 116.6(3) . . ? C6 C7 C8 101.1(3) . . ? C36 C7 C8 111.9(3) . . ? C6 C7 C37 106.4(3) . . ? C36 C7 C37 110.9(3) . . ? C8 C7 C37 109.3(3) . . ? C9 C8 C41 111.1(3) . . ? C9 C8 C7 100.4(3) . . ? C41 C8 C7 112.1(3) . . ? N22 C9 C10 126.3(3) . . ? N22 C9 C8 111.0(3) . . ? C10 C9 C8 122.6(3) . . ? C9 C10 C11 125.7(4) . . ? N23 C11 C10 124.7(4) . . ? N23 C11 C12 111.3(3) . . ? C10 C11 C12 123.9(4) . . ? C14 C13 C12 101.8(3) . . ? C14 C13 C48 106.6(3) . . ? C12 C13 C48 117.6(3) . . ? C15 C14 N23 126.7(4) . . ? C15 C14 C13 124.3(3) . . ? N23 C14 C13 108.7(3) . . ? C14 C15 C16 121.0(3) . . ? C14 C15 C53 118.8(3) . . ? C16 C15 C53 120.1(3) . . ? N24 C16 C15 122.6(3) . . ? N24 C16 C17 110.7(3) . . ? C15 C16 C17 126.6(3) . . ? C16 C17 C55 116.8(3) . . ? C16 C17 C54 106.9(3) . . ? C55 C17 C54 108.3(3) . . ? C16 C17 C18 101.1(3) . . ? C55 C17 C18 111.5(3) . . ? C54 C17 C18 112.2(3) . . ? C60 C18 C19 112.9(3) . . ? C60 C18 C17 116.4(3) . . ? C19 C18 C17 101.6(3) . . ? N24 C19 C18 101.9(3) . . ? N24 C19 C1 105.9(3) . . ? C18 C19 C1 123.4(3) . . ? C27 C26 C2 116.2(3) . . ? O28 C27 N29 121.4(4) . . ? O28 C27 C26 122.9(4) . . ? N29 C27 C26 115.8(4) . . ? C31 C30 C3 114.6(3) . . ? C32 C31 C30 110.4(3) . . ? O34 C32 N33 122.8(4) . . ? O34 C32 C31 120.1(4) . . ? N33 C32 C31 117.0(4) . . ? C38 C37 C7 112.2(3) . . ? O39 C38 N40 121.9(4) . . ? O39 C38 C37 120.4(4) . . ? N40 C38 C37 117.6(4) . . ? C42 C41 C8 113.5(3) . . ? C43 C42 C41 112.9(4) . . ? O45 C43 N44 122.3(4) . . ? O45 C43 C42 122.5(4) . . ? N44 C43 C42 115.1(4) . . ? C49 C48 C13 116.6(4) . . ? C50 C49 C48 114.3(4) . . ? O52 C50 N51 122.9(5) . . ? O52 C50 C49 121.4(4) . . ? N51 C50 C49 115.7(4) . . ? C56 C55 C17 115.5(3) . . ? C57 C56 C55 111.1(3) . . ? O58 C57 N59 123.0(4) . . ? O58 C57 C56 121.2(4) . . ? N59 C57 C56 115.8(4) . . ? C18 C60 C61 114.9(3) . . ? O62 C61 N63 123.6(4) . . ? O62 C61 C60 120.5(3) . . ? N63 C61 C60 115.8(3) . . ? N59 PR1 PR2 112.6(3) . . ? O3 PR2 PR1 107.3(3) . . ? O3 PR2 PR3 108.3(3) . . ? PR1 PR2 PR3 112.0(3) . . ? O2 R3 R2 113.1(3) . . ? O2 R3 R4 110.1(3) . . ? R2 R3 R4 104.1(3) . . ? R6 R4 R3 106.4(3) . . ? R6 R4 R5 107.5(3) . . ? R3 R4 R5 112.5(4) . . ? R6 R1 B1 107.2(3) . . ? R6 R1 R2 106.9(3) . . ? B1 R1 R2 112.3(3) . . ? R7 R2 R3 112.5(3) . . ? R7 R2 R1 110.0(3) . . ? R3 R2 R1 99.4(3) . . ? R8 R5 R4 113.3(4) . . ? B3 B2 B1 113.0(3) . . ? B4 B9 B8 118.7(4) . . ? B4 B9 B3 132.4(3) . . ? B8 B9 B3 108.9(3) . . ? B5 B4 B9 119.5(4) . . ? B4 B5 B6 121.3(4) . . ? B4 B5 B10 119.2(4) . . ? B6 B5 B10 119.5(4) . . ? B7 B6 B5 120.3(4) . . ? B7 B6 B11 118.9(4) . . ? B5 B6 B11 120.8(4) . . ? B6 B7 B8 116.7(4) . . ? B9 B8 B1 106.0(3) . . ? B9 B8 B7 123.5(4) . . ? B1 B8 B7 130.5(4) . . ? L2 L1 Co1 175.0(4) . . ? L1 L2 L3 179.4(5) . . ? L8 L3 L2 122.9(5) . . ? L8 L3 L4 118.0(5) . . ? L2 L3 L4 118.9(5) . . ? L5 L4 L3 120.5(6) . . ? L6 L5 L4 119.9(6) . . ? L5 L6 L9 125.8(6) . . ? L5 L6 L7 120.7(6) . . ? L9 L6 L7 113.5(6) . . ? L8 L7 L6 118.3(6) . . ? L3 L8 L7 122.2(6) . . ? L6 L9 L10 115.2(6) . . ? O83A C80A C82A 122.9(6) . . ? O83A C80A C81A 121.4(6) . . ? C82A C80A C81A 115.7(6) . . ? O73A C70A C71A 122.6(10) . . ? O73A C70A C72A 118.9(10) . . ? C71A C70A C72A 118.5(10) . . ? O78A C75A C76A 123.8(14) . . ? O78A C75A C77A 114.1(12) . . ? C76A C75A C77A 121.7(14) . . ? C11 C12 C47 112.7(3) . . ? C11 C12 C13 101.5(3) . . ? C47 C12 C13 117.0(3) . . ? C11 C12 C46 107.0(3) . . ? C47 C12 C46 109.1(4) . . ? C13 C12 C46 108.9(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 67.54 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.986 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.099 _database_code_depnum_ccdc_archive 'CCDC 961229' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z:\aga\niemoje\dorota\al6_b\aga\bez_sq\final _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H131 Co N13 O27 P' _chemical_formula_weight 1784.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _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 15.8504(3) _cell_length_b 21.6765(4) _cell_length_c 26.2587(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9022.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9926 _cell_measurement_theta_min 3.37 _cell_measurement_theta_max 67.11 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3816 _exptl_absorpt_coefficient_mu 2.346 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7824 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47545 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 66.59 _reflns_number_total 14949 _reflns_number_gt 13305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0598P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(3) _refine_ls_number_reflns 14949 _refine_ls_number_parameters 1084 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.018 _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 C1 C 0.85436(18) 0.81726(11) 0.29488(10) 0.0152(5) Uani 1 1 d . . . C2 C 0.95082(18) 0.80194(11) 0.28618(10) 0.0158(6) Uani 1 1 d . . . C3 C 0.98996(18) 0.86788(11) 0.28276(10) 0.0162(5) Uani 1 1 d . . . H3 H 1.0373 0.8672 0.2576 0.019 Uiso 1 1 calc R . . C4 C 0.91805(17) 0.90498(12) 0.26082(9) 0.0154(5) Uani 1 1 d . . . C5 C 0.92901(18) 0.96321(12) 0.23508(10) 0.0173(6) Uani 1 1 d . . . C6 C 0.86077(19) 1.00011(11) 0.22423(10) 0.0165(6) Uani 1 1 d . . . C7 C 0.86258(19) 1.06418(12) 0.19954(10) 0.0172(6) Uani 1 1 d . . . C8 C 0.77437(19) 1.08911(11) 0.21545(10) 0.0179(6) Uani 1 1 d . . . H8 H 0.7501 1.1153 0.1877 0.021 Uiso 1 1 calc R . . C9 C 0.72585(19) 1.02996(11) 0.22020(10) 0.0164(6) Uani 1 1 d . . . C10 C 0.6397(2) 1.02579(12) 0.21172(11) 0.0200(6) Uani 1 1 d . . . C11 C 0.59305(19) 0.97216(12) 0.21441(10) 0.0173(6) Uani 1 1 d . . . C12 C 0.50264(19) 0.96684(12) 0.19513(11) 0.0207(6) Uani 1 1 d . . . C13 C 0.47398(18) 0.90713(12) 0.22146(10) 0.0180(6) Uani 1 1 d . . . H13 H 0.4370 0.8827 0.1981 0.022 Uiso 1 1 calc R . . C14 C 0.55723(18) 0.87383(12) 0.22955(10) 0.0163(5) Uani 1 1 d . . . C15 C 0.56452(18) 0.81191(11) 0.23915(10) 0.0167(6) Uani 1 1 d . . . C16 C 0.64418(17) 0.78538(11) 0.25392(10) 0.0152(5) Uani 1 1 d . . . C17 C 0.66379(18) 0.71581(11) 0.25994(10) 0.0172(6) Uani 1 1 d . . . C18 C 0.75060(18) 0.71892(11) 0.28771(10) 0.0169(6) Uani 1 1 d . . . H18 H 0.7400 0.7246 0.3250 0.020 Uiso 1 1 calc R . . C19 C 0.78764(17) 0.77879(11) 0.26655(10) 0.0153(5) Uani 1 1 d . . . H19 H 0.8098 0.7700 0.2316 0.018 Uiso 1 1 calc R . . C20 C 0.82985(19) 0.82187(12) 0.35100(10) 0.0179(6) Uani 1 1 d . . . H20A H 0.8713 0.8473 0.3691 0.027 Uiso 1 1 calc R . . H20B H 0.8286 0.7805 0.3660 0.027 Uiso 1 1 calc R . . H20C H 0.7739 0.8408 0.3539 0.027 Uiso 1 1 calc R . . C25 C 0.98873(19) 0.76204(12) 0.32785(10) 0.0190(6) Uani 1 1 d . . . H25A H 0.9816 0.7825 0.3608 0.029 Uiso 1 1 calc R . . H25B H 1.0490 0.7559 0.3211 0.029 Uiso 1 1 calc R . . H25C H 0.9601 0.7220 0.3285 0.029 Uiso 1 1 calc R . . C26 C 0.96292(18) 0.77107(12) 0.23379(10) 0.0182(6) Uani 1 1 d . . . H26A H 0.9320 0.7314 0.2340 0.022 Uiso 1 1 calc R . . H26B H 0.9363 0.7977 0.2077 0.022 Uiso 1 1 calc R . . C27 C 1.05421(19) 0.75837(12) 0.21734(10) 0.0201(6) Uani 1 1 d . . . C30 C 1.02088(18) 0.89986(12) 0.33217(10) 0.0184(6) Uani 1 1 d . . . H30A H 1.0150 0.9451 0.3280 0.022 Uiso 1 1 calc R . . H30B H 0.9839 0.8871 0.3607 0.022 Uiso 1 1 calc R . . C31 C 1.1128(2) 0.88518(13) 0.34627(11) 0.0230(6) Uani 1 1 d . . . H31A H 1.1187 0.8406 0.3535 0.028 Uiso 1 1 calc R . . H31B H 1.1503 0.8956 0.3174 0.028 Uiso 1 1 calc R . . C32 C 1.1378(2) 0.92243(13) 0.39292(12) 0.0253(7) Uani 1 1 d . . . C35 C 1.0183(2) 0.98205(13) 0.22143(12) 0.0249(6) Uani 1 1 d . . . H35A H 1.0576 0.9495 0.2318 0.037 Uiso 1 1 calc R . . H35B H 1.0326 1.0205 0.2391 0.037 Uiso 1 1 calc R . . H35C H 1.0224 0.9883 0.1846 0.037 Uiso 1 1 calc R . . C36 C 0.9336(2) 1.10760(12) 0.21548(11) 0.0212(6) Uani 1 1 d . . . H36A H 0.9275 1.1470 0.1976 0.032 Uiso 1 1 calc R . . H36B H 0.9881 1.0891 0.2068 0.032 Uiso 1 1 calc R . . H36C H 0.9308 1.1146 0.2523 0.032 Uiso 1 1 calc R . . C37 C 0.8637(2) 1.05188(12) 0.14073(10) 0.0210(6) Uani 1 1 d . . . H37A H 0.9176 1.0318 0.1314 0.025 Uiso 1 1 calc R . . H37B H 0.8173 1.0232 0.1319 0.025 Uiso 1 1 calc R . . C38 C 0.85403(19) 1.11016(13) 0.11052(10) 0.0203(6) Uani 1 1 d . . . C41 C 0.77503(19) 1.12482(12) 0.26617(11) 0.0205(6) Uani 1 1 d . . . H41A H 0.8060 1.1003 0.2919 0.025 Uiso 1 1 calc R . . H41B H 0.8059 1.1641 0.2613 0.025 Uiso 1 1 calc R . . C42 C 0.6874(2) 1.13903(14) 0.28641(12) 0.0267(7) Uani 1 1 d . . . H42A H 0.6547 1.1601 0.2594 0.032 Uiso 1 1 calc R . . H42B H 0.6585 1.0997 0.2943 0.032 Uiso 1 1 calc R . . C43 C 0.6875(2) 1.17867(13) 0.33325(12) 0.0288(7) Uani 1 1 d . . . C46 C 0.4508(2) 1.02434(13) 0.20470(13) 0.0290(7) Uani 1 1 d . . . H46A H 0.3935 1.0182 0.1917 0.044 Uiso 1 1 calc R . . H46B H 0.4769 1.0595 0.1872 0.044 Uiso 1 1 calc R . . H46C H 0.4486 1.0326 0.2414 0.044 Uiso 1 1 calc R . . C47 C 0.5074(2) 0.95481(15) 0.13764(12) 0.0301(7) Uani 1 1 d . . . H47A H 0.5418 0.9180 0.1313 0.045 Uiso 1 1 calc R . . H47B H 0.5331 0.9905 0.1207 0.045 Uiso 1 1 calc R . . H47C H 0.4504 0.9482 0.1242 0.045 Uiso 1 1 calc R . . C48 C 0.43164(19) 0.91335(13) 0.27439(11) 0.0202(6) Uani 1 1 d . . . H48A H 0.4356 0.8730 0.2919 0.024 Uiso 1 1 calc R . . H48B H 0.4646 0.9434 0.2947 0.024 Uiso 1 1 calc R . . C49 C 0.33829(19) 0.93385(13) 0.27485(11) 0.0235(6) Uani 1 1 d . . . H49A H 0.3156 0.9292 0.3098 0.028 Uiso 1 1 calc R . . H49B H 0.3351 0.9781 0.2657 0.028 Uiso 1 1 calc R . . C50 C 0.28402(19) 0.89744(12) 0.23854(11) 0.0222(6) Uani 1 1 d . . . C60 C 0.80894(19) 0.66302(12) 0.28079(11) 0.0209(6) Uani 1 1 d . . . H05A H 0.8139 0.6540 0.2440 0.025 Uiso 1 1 calc R . . H05B H 0.8659 0.6740 0.2934 0.025 Uiso 1 1 calc R . . C53 C 0.48710(19) 0.77150(12) 0.23290(11) 0.0228(6) Uani 1 1 d . . . H53A H 0.5007 0.7365 0.2107 0.034 Uiso 1 1 calc R . . H53B H 0.4414 0.7957 0.2176 0.034 Uiso 1 1 calc R . . H53C H 0.4692 0.7562 0.2663 0.034 Uiso 1 1 calc R . . C54 C 0.6727(2) 0.68867(12) 0.20584(10) 0.0211(6) Uani 1 1 d . . . H54A H 0.7144 0.7126 0.1866 0.032 Uiso 1 1 calc R . . H54B H 0.6181 0.6905 0.1884 0.032 Uiso 1 1 calc R . . H54C H 0.6914 0.6456 0.2081 0.032 Uiso 1 1 calc R . . C55 C 0.59884(19) 0.67759(11) 0.28982(11) 0.0185(6) Uani 1 1 d . . . H55A H 0.5484 0.6718 0.2681 0.022 Uiso 1 1 calc R . . H55B H 0.6232 0.6363 0.2963 0.022 Uiso 1 1 calc R . . C56 C 0.5705(2) 0.70499(13) 0.34057(11) 0.0224(6) Uani 1 1 d . . . H56A H 0.6167 0.7010 0.3658 0.027 Uiso 1 1 calc R . . H56B H 0.5581 0.7494 0.3361 0.027 Uiso 1 1 calc R . . C57 C 0.49220(19) 0.67218(12) 0.36039(11) 0.0207(6) Uani 1 1 d . . . C61 C 0.77942(18) 0.60455(12) 0.30827(11) 0.0191(6) Uani 1 1 d . . . PR1 C 0.4314(2) 0.61042(13) 0.42939(11) 0.0229(6) Uani 1 1 d . . . HR1A H 0.4508 0.5703 0.4430 0.027 Uiso 1 1 calc R . . HR1B H 0.3853 0.6023 0.4049 0.027 Uiso 1 1 calc R . . PR2 C 0.39778(19) 0.64929(12) 0.47266(10) 0.0202(6) Uani 1 1 d . . . HR2 H 0.3715 0.6876 0.4586 0.024 Uiso 1 1 calc R . . PR3 C 0.3341(2) 0.61513(14) 0.50442(11) 0.0250(6) Uani 1 1 d . . . HR3A H 0.3145 0.6418 0.5321 0.038 Uiso 1 1 calc R . . HR3B H 0.3602 0.5780 0.5188 0.038 Uiso 1 1 calc R . . HR3C H 0.2861 0.6032 0.4831 0.038 Uiso 1 1 calc R . . B2 C 0.63814(18) 0.91440(11) 0.34424(10) 0.0158(6) Uani 1 1 d . . . B4 C 0.8273(2) 0.99983(11) 0.35331(11) 0.0185(6) Uani 1 1 d . . . H4 H 0.8603 0.9976 0.3232 0.022 Uiso 1 1 calc R . . B5 C 0.8556(2) 1.03314(12) 0.39504(11) 0.0221(6) Uani 1 1 d . . . B6 C 0.8062(2) 1.03666(13) 0.43999(11) 0.0235(6) Uani 1 1 d . . . B7 C 0.7296(2) 1.00727(12) 0.44262(10) 0.0207(6) Uani 1 1 d . . . H7 H 0.6959 1.0097 0.4725 0.025 Uiso 1 1 calc R . . B8 C 0.70264(18) 0.97387(12) 0.40034(10) 0.0172(6) Uani 1 1 d . . . B9 C 0.75024(18) 0.96978(11) 0.35600(10) 0.0159(6) Uani 1 1 d . . . B10 C 0.9395(2) 1.06596(15) 0.39222(13) 0.0322(7) Uani 1 1 d . . . H10A H 0.9319 1.1095 0.4012 0.048 Uiso 1 1 calc R . . H10B H 0.9619 1.0629 0.3575 0.048 Uiso 1 1 calc R . . H10C H 0.9791 1.0468 0.4161 0.048 Uiso 1 1 calc R . . B11 C 0.8400(2) 1.07072(16) 0.48575(13) 0.0368(8) Uani 1 1 d . . . H11A H 0.8957 1.0543 0.4947 0.055 Uiso 1 1 calc R . . H11B H 0.8014 1.0652 0.5146 0.055 Uiso 1 1 calc R . . H11C H 0.8449 1.1147 0.4777 0.055 Uiso 1 1 calc R . . R1 C 0.57085(18) 0.91847(12) 0.42986(10) 0.0173(6) Uani 1 1 d . . . H1 H 0.5660 0.9501 0.4574 0.021 Uiso 1 1 calc R . . L1 C 0.75931(19) 0.87666(11) 0.18126(10) 0.0184(6) Uani 1 1 d . . . L2 C 0.7689(2) 0.85570(13) 0.13908(11) 0.0253(6) Uani 1 1 d . . . R2 C 0.59351(18) 0.85530(12) 0.45300(10) 0.0172(6) Uani 1 1 d . . . H2 H 0.6311 0.8598 0.4833 0.021 Uiso 1 1 calc R . . L3 C 0.7788(2) 0.82794(15) 0.08972(11) 0.0321(7) Uani 1 1 d . . . R3 C 0.50562(19) 0.83358(12) 0.46817(10) 0.0189(6) Uani 1 1 d . . . H3A H 0.4904 0.8511 0.5022 0.023 Uiso 1 1 calc R . . L4 C 0.7332(3) 0.77518(16) 0.07680(13) 0.0413(9) Uani 1 1 d . . . H4A H 0.6948 0.7579 0.1007 0.050 Uiso 1 1 calc R . . R4 C 0.44690(19) 0.85967(12) 0.42761(10) 0.0193(6) Uani 1 1 d . . . H9 H 0.4363 0.8276 0.4010 0.023 Uiso 1 1 calc R . . L5 C 0.7431(3) 0.74766(18) 0.02944(14) 0.0514(10) Uani 1 1 d . . . H5 H 0.7137 0.7107 0.0217 0.062 Uiso 1 1 calc R . . R5 C 0.3638(2) 0.88293(14) 0.44805(12) 0.0277(7) Uani 1 1 d . . . H5A H 0.3292 0.8984 0.4194 0.033 Uiso 1 1 calc R . . H5B H 0.3331 0.8482 0.4640 0.033 Uiso 1 1 calc R . . L6 C 0.7945(3) 0.7732(2) -0.00558(15) 0.0576(12) Uani 1 1 d . . . H6 H 0.8004 0.7546 -0.0381 0.069 Uiso 1 1 calc R . . L7 C 0.8392(3) 0.8270(2) 0.00581(15) 0.0584(12) Uani 1 1 d . . . H7A H 0.8746 0.8454 -0.0191 0.070 Uiso 1 1 calc R . . L8 C 0.8318(3) 0.85315(18) 0.05340(13) 0.0426(9) Uani 1 1 d . . . H8A H 0.8636 0.8890 0.0614 0.051 Uiso 1 1 calc R . . N21 N 0.84582(15) 0.87859(9) 0.26916(8) 0.0151(5) Uani 1 1 d . . . N22 N 0.77720(15) 0.98302(9) 0.23195(8) 0.0148(5) Uani 1 1 d . . . N23 N 0.62193(15) 0.91707(9) 0.22998(8) 0.0159(5) Uani 1 1 d . . . N24 N 0.71190(14) 0.81825(9) 0.26103(8) 0.0147(5) Uani 1 1 d . . . N29 N 1.06217(17) 0.72468(11) 0.17537(9) 0.0266(6) Uani 1 1 d . . . H29A H 1.1127 0.7154 0.1638 0.032 Uiso 1 1 calc R . . H29B H 1.0169 0.7117 0.1592 0.032 Uiso 1 1 calc R . . N63 N 0.78380(16) 0.55324(10) 0.28090(10) 0.0228(5) Uani 1 1 d . . . H63A H 0.7704 0.5176 0.2947 0.027 Uiso 1 1 calc R . . H63B H 0.8001 0.5548 0.2489 0.027 Uiso 1 1 calc R . . N34 N 1.12844(18) 0.89563(13) 0.43760(9) 0.0308(6) Uani 1 1 d . . . H34A H 1.1412 0.9158 0.4656 0.037 Uiso 1 1 calc R . . H34B H 1.1094 0.8576 0.4394 0.037 Uiso 1 1 calc R . . N40 N 0.92509(17) 1.13841(11) 0.09575(9) 0.0250(5) Uani 1 1 d . . . H40A H 0.9224 1.1733 0.0787 0.030 Uiso 1 1 calc R . . H40B H 0.9744 1.1221 0.1031 0.030 Uiso 1 1 calc R . . N45 N 0.6163(2) 1.17445(13) 0.36108(10) 0.0363(7) Uani 1 1 d . . . H45A H 0.6101 1.1973 0.3885 0.044 Uiso 1 1 calc R . . H45B H 0.5761 1.1488 0.3519 0.044 Uiso 1 1 calc R . . N52 N 0.27327(16) 0.83813(10) 0.24921(10) 0.0252(5) Uani 1 1 d . . . H52A H 0.2434 0.8146 0.2286 0.030 Uiso 1 1 calc R . . H52B H 0.2960 0.8223 0.2769 0.030 Uiso 1 1 calc R . . N59 N 0.50088(16) 0.64031(10) 0.40303(9) 0.0203(5) Uani 1 1 d . . . H59 H 0.5517 0.6370 0.4162 0.024 Uiso 1 1 calc R . . NB1 N 0.63064(16) 0.93899(10) 0.39150(8) 0.0171(5) Uani 1 1 d . . . NB3 N 0.70703(15) 0.93237(9) 0.32095(8) 0.0161(5) Uani 1 1 d . . . O62 O 0.75729(14) 0.60627(8) 0.35307(7) 0.0244(4) Uani 1 1 d . . . O28 O 1.11577(13) 0.77758(9) 0.24123(8) 0.0289(5) Uani 1 1 d . . . O33 O 1.16460(18) 0.97634(10) 0.38865(9) 0.0395(6) Uani 1 1 d . . . O39 O 0.78323(14) 1.13123(9) 0.10112(8) 0.0292(5) Uani 1 1 d . . . O44 O 0.74548(17) 1.21366(10) 0.34441(9) 0.0394(6) Uani 1 1 d . . . O51 O 0.25339(15) 0.92190(9) 0.20016(8) 0.0283(5) Uani 1 1 d . . . O58 O 0.42468(14) 0.67476(9) 0.33652(8) 0.0273(5) Uani 1 1 d . . . OP2 O 0.49933(14) 0.76758(8) 0.46971(7) 0.0212(4) Uani 1 1 d . . . OP3 O 0.46931(13) 0.66577(8) 0.50456(7) 0.0196(4) Uani 1 1 d . . . OP4 O 0.40777(13) 0.76100(8) 0.54747(7) 0.0208(4) Uani 1 1 d . . . OP5 O 0.56275(13) 0.73350(9) 0.55372(7) 0.0235(4) Uani 1 1 d . . . OR6 O 0.49234(13) 0.91115(9) 0.40516(7) 0.0214(4) Uani 1 1 d . . . OR7 O 0.63034(14) 0.81818(8) 0.41559(7) 0.0198(4) Uani 1 1 d . . . HR7 H 0.6675 0.7958 0.4289 0.030 Uiso 1 1 calc R . . OR8 O 0.37389(17) 0.93092(10) 0.48453(8) 0.0354(5) Uani 1 1 d . . . HR8 H 0.3742 0.9157 0.5140 0.053 Uiso 1 1 calc R . . P1 P 0.48386(5) 0.73394(3) 0.52290(3) 0.01760(15) Uani 1 1 d . . . Co01 Co 0.73714(3) 0.902026(17) 0.248003(15) 0.01348(10) Uani 1 1 d . . . O1W O 0.73906(14) 0.73984(9) 0.46695(7) 0.0267(5) Uani 1 1 d . . . O2W O 0.39388(14) 0.87768(10) 0.58254(8) 0.0269(5) Uani 1 1 d . . . O3W O 0.77124(14) 1.24978(9) 0.07197(8) 0.0281(5) Uani 1 1 d . . . O4W O 0.32772(15) 0.78151(10) 0.34190(8) 0.0320(5) Uani 1 1 d . . . O5W O 1.16942(16) 0.87488(11) 0.55534(10) 0.0410(6) Uani 1 1 d . . . O6W O 0.86145(18) 0.56458(11) 0.18407(9) 0.0436(6) Uani 1 1 d . . . O7W O 0.89452(18) 0.68030(13) 0.12659(10) 0.0481(7) Uani 1 1 d . . . O8W O 0.2821(3) 0.83532(14) 0.11802(11) 0.0921(15) Uani 1 1 d . . . O9W O 0.8532(2) 0.59344(15) 0.05774(13) 0.0715(9) Uani 1 1 d . . . O10W O 1.2086(5) 0.9785(3) 0.5153(2) 0.0626(16) Uiso 0.50 1 d P A 1 O11W O 1.3415(6) 0.9006(4) 0.0392(3) 0.085(2) Uiso 0.50 1 d P B 1 O1A O 0.4798(2) 1.08051(14) 0.34352(11) 0.0582(8) Uani 1 1 d . . . C1A C 0.3511(3) 1.0506(2) 0.38173(17) 0.0520(11) Uani 1 1 d . . . H1A1 H 0.3323 1.0453 0.3464 0.078 Uiso 1 1 calc R . . H1A2 H 0.3186 1.0838 0.3978 0.078 Uiso 1 1 calc R . . H1A3 H 0.3423 1.0121 0.4006 0.078 Uiso 1 1 calc R . . C2A C 0.4430(3) 1.06686(15) 0.38231(15) 0.0402(9) Uani 1 1 d . . . C3A C 0.4846(3) 1.06744(16) 0.43324(15) 0.0451(9) Uani 1 1 d . . . H3A1 H 0.5458 1.0634 0.4289 0.068 Uiso 1 1 calc R . . H3A2 H 0.4634 1.0329 0.4537 0.068 Uiso 1 1 calc R . . H3A3 H 0.4720 1.1064 0.4506 0.068 Uiso 1 1 calc R . . O2A O 0.4905(2) 1.21991(15) 0.43975(12) 0.0673(9) Uani 1 1 d D . . C4A1 C 0.4958(7) 1.2654(5) 0.4738(4) 0.049(3) Uiso 0.50 1 d PD C 1 C5A1 C 0.4613(5) 1.2540(4) 0.5235(3) 0.0354(15) Uiso 0.50 1 d PD C 1 H5A1 H 0.4427 1.2110 0.5258 0.053 Uiso 0.50 1 calc PR C 1 H5A2 H 0.4130 1.2815 0.5293 0.053 Uiso 0.50 1 calc PR C 1 H5A3 H 0.5045 1.2619 0.5494 0.053 Uiso 0.50 1 calc PR C 1 C6A1 C 0.5243(7) 1.3283(4) 0.4611(4) 0.058(2) Uiso 0.50 1 d PD C 1 H6A1 H 0.5583 1.3271 0.4300 0.087 Uiso 0.50 1 calc PR C 1 H6A2 H 0.5584 1.3446 0.4892 0.087 Uiso 0.50 1 calc PR C 1 H6A3 H 0.4751 1.3549 0.4558 0.087 Uiso 0.50 1 calc PR C 1 C4A2 C 0.4825(6) 1.2639(5) 0.4614(4) 0.040(3) Uiso 0.50 1 d PD C 2 C5A2 C 0.4891(12) 1.2789(9) 0.5200(7) 0.123(6) Uiso 0.50 1 d PD C 2 H5A4 H 0.4666 1.3202 0.5264 0.184 Uiso 0.50 1 calc PR C 2 H5A5 H 0.5484 1.2772 0.5305 0.184 Uiso 0.50 1 calc PR C 2 H5A6 H 0.4566 1.2485 0.5394 0.184 Uiso 0.50 1 calc PR C 2 C6A2 C 0.4838(9) 1.3209(5) 0.4324(5) 0.085(3) Uiso 0.50 1 d PD C 2 H6A4 H 0.5113 1.3533 0.4524 0.127 Uiso 0.50 1 calc PR C 2 H6A5 H 0.4258 1.3334 0.4244 0.127 Uiso 0.50 1 calc PR C 2 H6A6 H 0.5151 1.3145 0.4006 0.127 Uiso 0.50 1 calc PR C 2 O3A O 0.9844(5) 0.9631(3) 0.0691(2) 0.0655(16) Uiso 0.50 1 d PD D 1 C7A C 1.0399(7) 0.9332(4) 0.0848(3) 0.060(2) Uiso 0.50 1 d PD D 1 C8A C 1.1232(5) 0.9388(3) 0.0749(3) 0.275(19) Uiso 0.50 1 d PD D 1 H8A1 H 1.1374 0.9148 0.0445 0.413 Uiso 0.50 1 calc PR D 1 H8A2 H 1.1557 0.9235 0.1040 0.413 Uiso 0.50 1 calc PR D 1 H8A3 H 1.1369 0.9823 0.0690 0.413 Uiso 0.50 1 calc PR D 1 C9A C 1.0215(9) 0.8816(6) 0.1206(4) 0.085(3) Uiso 0.50 1 d PD D 1 H9A1 H 0.9691 0.8902 0.1390 0.127 Uiso 0.50 1 calc PR D 1 H9A2 H 1.0680 0.8774 0.1449 0.127 Uiso 0.50 1 calc PR D 1 H9A3 H 1.0154 0.8431 0.1013 0.127 Uiso 0.50 1 calc PR D 1 O4A O 1.2053(4) 0.8992(2) 0.00620(19) 0.0463(12) Uiso 0.50 1 d PD E 2 C10A C 1.2009(5) 0.9301(3) 0.0448(3) 0.0411(17) Uiso 0.50 1 d PD E 2 C11A C 1.2712(6) 0.9685(4) 0.0623(3) 0.0492(19) Uiso 0.50 1 d PD E 2 H11D H 1.3226 0.9571 0.0437 0.074 Uiso 0.50 1 calc PR E 2 H11E H 1.2801 0.9619 0.0989 0.074 Uiso 0.50 1 calc PR E 2 H11F H 1.2582 1.0120 0.0561 0.074 Uiso 0.50 1 calc PR E 2 C12A C 1.1232(5) 0.9388(3) 0.0749(3) 0.050(2) Uiso 0.50 1 d P E 2 H12A H 1.0740 0.9352 0.0525 0.075 Uiso 0.50 1 calc PR E 2 H12B H 1.1238 0.9798 0.0906 0.075 Uiso 0.50 1 calc PR E 2 H12C H 1.1202 0.9072 0.1015 0.075 Uiso 0.50 1 calc PR E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0096(14) 0.0115(12) 0.0245(13) 0.0003(10) -0.0011(11) 0.0003(10) C2 0.0102(14) 0.0141(12) 0.0233(13) -0.0008(10) 0.0000(11) 0.0009(11) C3 0.0099(14) 0.0136(12) 0.0252(13) 0.0009(10) 0.0021(11) 0.0014(10) C4 0.0115(14) 0.0153(12) 0.0193(12) -0.0024(10) 0.0012(10) 0.0000(11) C5 0.0116(14) 0.0163(12) 0.0241(13) -0.0008(10) 0.0009(11) -0.0017(11) C6 0.0167(16) 0.0127(12) 0.0202(13) -0.0003(10) 0.0019(11) -0.0015(11) C7 0.0157(15) 0.0115(12) 0.0245(13) 0.0023(10) 0.0020(11) -0.0025(11) C8 0.0189(16) 0.0113(11) 0.0235(13) 0.0013(10) 0.0027(12) -0.0037(11) C9 0.0155(15) 0.0142(12) 0.0197(12) 0.0010(10) 0.0023(11) 0.0001(11) C10 0.0178(16) 0.0152(13) 0.0268(14) 0.0002(11) 0.0013(12) 0.0003(11) C11 0.0146(16) 0.0152(12) 0.0220(13) 0.0010(10) 0.0003(11) -0.0003(11) C12 0.0132(16) 0.0171(13) 0.0317(15) 0.0043(11) -0.0039(12) -0.0007(11) C13 0.0131(15) 0.0126(12) 0.0282(14) -0.0004(11) -0.0032(11) -0.0009(11) C14 0.0125(15) 0.0153(12) 0.0210(12) -0.0010(10) 0.0009(11) -0.0038(11) C15 0.0135(15) 0.0141(12) 0.0226(13) 0.0005(10) -0.0019(11) -0.0023(10) C16 0.0133(14) 0.0135(11) 0.0189(12) -0.0023(10) 0.0008(11) -0.0006(10) C17 0.0115(14) 0.0104(11) 0.0297(14) 0.0008(10) 0.0001(11) -0.0010(10) C18 0.0140(15) 0.0102(11) 0.0265(13) -0.0008(10) 0.0002(11) 0.0006(11) C19 0.0111(14) 0.0116(11) 0.0233(12) 0.0000(10) -0.0007(11) 0.0016(10) C20 0.0136(15) 0.0152(12) 0.0249(14) 0.0010(10) -0.0002(11) 0.0002(11) C25 0.0148(15) 0.0156(12) 0.0266(13) 0.0005(11) 0.0006(11) 0.0015(11) C26 0.0121(15) 0.0165(12) 0.0261(13) -0.0014(11) 0.0007(11) -0.0008(11) C27 0.0191(17) 0.0158(12) 0.0254(14) -0.0007(11) 0.0007(12) 0.0024(12) C30 0.0129(14) 0.0164(12) 0.0259(13) 0.0001(11) -0.0003(11) 0.0007(11) C31 0.0144(15) 0.0252(14) 0.0294(14) -0.0041(12) -0.0017(12) 0.0008(12) C32 0.0125(15) 0.0252(15) 0.0382(16) -0.0036(13) -0.0039(13) -0.0026(12) C35 0.0145(16) 0.0234(14) 0.0367(16) 0.0088(12) 0.0037(13) 0.0008(12) C36 0.0193(16) 0.0164(13) 0.0278(14) 0.0011(11) 0.0000(12) -0.0031(11) C37 0.0205(16) 0.0177(13) 0.0248(14) 0.0012(11) 0.0011(12) -0.0027(12) C38 0.0171(16) 0.0232(14) 0.0205(13) 0.0010(11) -0.0007(11) -0.0008(12) C41 0.0199(16) 0.0124(11) 0.0293(14) -0.0016(10) 0.0019(12) -0.0034(11) C42 0.0232(19) 0.0238(14) 0.0332(16) -0.0032(12) 0.0059(13) -0.0018(13) C43 0.032(2) 0.0209(14) 0.0331(16) -0.0005(12) 0.0073(14) -0.0028(14) C46 0.0167(17) 0.0179(14) 0.0526(19) 0.0107(13) 0.0016(15) 0.0014(13) C47 0.0256(19) 0.0310(16) 0.0336(16) 0.0096(13) -0.0064(14) -0.0062(14) C48 0.0104(15) 0.0207(13) 0.0297(14) -0.0027(11) -0.0017(12) 0.0000(11) C49 0.0153(16) 0.0235(14) 0.0317(15) -0.0001(12) 0.0006(13) 0.0004(12) C50 0.0147(15) 0.0212(13) 0.0309(15) 0.0010(12) 0.0039(12) 0.0021(11) C60 0.0162(16) 0.0122(12) 0.0343(16) 0.0013(11) 0.0025(13) 0.0014(11) C53 0.0150(15) 0.0146(12) 0.0388(15) 0.0025(11) -0.0059(12) -0.0033(11) C54 0.0178(16) 0.0177(13) 0.0279(14) -0.0025(11) -0.0012(12) -0.0037(12) C55 0.0133(15) 0.0119(12) 0.0305(14) 0.0009(11) -0.0006(12) -0.0003(11) C56 0.0156(16) 0.0210(13) 0.0306(14) -0.0011(12) 0.0028(12) -0.0053(12) C57 0.0164(17) 0.0175(13) 0.0281(14) -0.0058(11) 0.0041(13) -0.0027(12) C61 0.0108(15) 0.0129(12) 0.0337(15) 0.0024(11) -0.0071(12) 0.0003(11) PR1 0.0193(16) 0.0199(13) 0.0296(14) -0.0001(11) 0.0041(12) -0.0065(12) PR2 0.0167(15) 0.0192(12) 0.0246(14) 0.0004(11) -0.0033(12) -0.0038(11) PR3 0.0211(17) 0.0267(14) 0.0274(14) 0.0003(12) 0.0027(13) -0.0058(13) B2 0.0145(15) 0.0116(12) 0.0214(13) 0.0028(10) 0.0007(11) 0.0017(11) B4 0.0177(16) 0.0134(12) 0.0243(14) 0.0005(10) 0.0027(12) 0.0014(11) B5 0.0182(16) 0.0178(13) 0.0303(15) -0.0006(11) 0.0012(13) -0.0013(12) B6 0.0253(18) 0.0184(13) 0.0268(15) -0.0033(11) 0.0001(13) -0.0006(12) B7 0.0246(17) 0.0156(12) 0.0218(13) -0.0008(10) 0.0024(12) 0.0001(12) B8 0.0125(15) 0.0128(12) 0.0263(14) -0.0005(10) 0.0000(12) -0.0017(10) B9 0.0151(15) 0.0114(11) 0.0212(12) 0.0009(10) -0.0005(11) 0.0016(11) B10 0.0259(19) 0.0342(16) 0.0364(17) -0.0073(14) 0.0022(15) -0.0100(15) B11 0.033(2) 0.0406(18) 0.0373(18) -0.0139(15) 0.0047(16) -0.0125(16) R1 0.0132(15) 0.0179(12) 0.0210(13) -0.0004(10) 0.0028(11) -0.0015(11) L1 0.0146(15) 0.0143(11) 0.0262(14) 0.0007(11) -0.0006(12) -0.0009(11) L2 0.0252(18) 0.0255(14) 0.0253(15) 0.0003(12) -0.0011(13) 0.0048(13) R2 0.0156(15) 0.0170(12) 0.0189(13) -0.0012(10) -0.0015(11) 0.0005(11) L3 0.037(2) 0.0332(16) 0.0259(15) -0.0032(13) -0.0024(14) 0.0070(15) R3 0.0212(17) 0.0131(12) 0.0224(13) 0.0006(10) 0.0030(12) -0.0021(11) L4 0.047(2) 0.0395(18) 0.0371(17) -0.0094(14) -0.0034(17) -0.0029(18) R4 0.0155(15) 0.0195(13) 0.0229(13) 0.0005(11) 0.0013(12) -0.0050(11) L5 0.059(3) 0.049(2) 0.046(2) -0.0146(17) -0.004(2) -0.009(2) R5 0.0171(17) 0.0303(15) 0.0357(16) 0.0079(13) 0.0048(13) 0.0004(13) L6 0.064(3) 0.070(3) 0.039(2) -0.023(2) 0.005(2) 0.001(2) L7 0.065(3) 0.071(3) 0.039(2) -0.011(2) 0.018(2) -0.002(2) L8 0.045(2) 0.048(2) 0.0346(18) -0.0055(16) 0.0071(17) -0.0046(18) N21 0.0140(13) 0.0109(10) 0.0204(10) -0.0005(8) 0.0015(9) 0.0003(9) N22 0.0098(12) 0.0132(10) 0.0215(10) 0.0009(8) -0.0002(9) 0.0002(9) N23 0.0132(12) 0.0125(10) 0.0220(10) 0.0003(9) -0.0005(9) 0.0001(9) N24 0.0091(12) 0.0135(10) 0.0214(11) -0.0028(8) 0.0007(9) 0.0022(9) N29 0.0173(14) 0.0319(13) 0.0305(13) -0.0083(11) 0.0030(11) 0.0037(11) N63 0.0197(14) 0.0127(10) 0.0361(13) 0.0003(9) 0.0003(11) -0.0009(10) N34 0.0289(16) 0.0351(14) 0.0283(13) -0.0056(11) -0.0020(11) -0.0111(12) N40 0.0170(14) 0.0272(12) 0.0307(12) 0.0121(10) 0.0020(11) 0.0015(11) N45 0.0333(18) 0.0395(15) 0.0361(14) -0.0060(12) 0.0099(13) -0.0028(14) N52 0.0177(13) 0.0209(11) 0.0370(13) 0.0011(10) -0.0040(12) -0.0025(10) N59 0.0145(14) 0.0212(11) 0.0253(12) -0.0019(9) 0.0022(10) -0.0046(10) NB1 0.0135(13) 0.0153(10) 0.0225(11) 0.0000(9) 0.0032(10) -0.0017(9) NB3 0.0152(13) 0.0122(10) 0.0210(11) 0.0000(8) 0.0007(10) 0.0003(9) O62 0.0226(12) 0.0226(9) 0.0279(10) 0.0034(8) -0.0031(9) -0.0012(9) O28 0.0147(11) 0.0274(10) 0.0444(12) -0.0063(9) 0.0028(10) -0.0022(9) O33 0.0440(16) 0.0282(12) 0.0463(13) -0.0025(10) -0.0120(12) -0.0159(11) O39 0.0187(13) 0.0315(11) 0.0374(11) 0.0127(9) -0.0026(9) -0.0009(9) O44 0.0406(16) 0.0328(11) 0.0447(12) -0.0114(10) 0.0142(12) -0.0121(11) O51 0.0278(13) 0.0206(9) 0.0366(11) 0.0004(8) -0.0072(10) 0.0026(9) O58 0.0155(12) 0.0283(10) 0.0381(11) 0.0045(9) 0.0015(10) -0.0026(9) OP2 0.0277(12) 0.0126(8) 0.0235(9) -0.0030(7) 0.0039(8) -0.0048(8) OP3 0.0154(11) 0.0191(9) 0.0241(9) 0.0015(8) -0.0029(8) -0.0005(8) OP4 0.0161(11) 0.0222(9) 0.0242(9) -0.0019(8) 0.0020(8) -0.0015(8) OP5 0.0173(11) 0.0275(10) 0.0258(10) -0.0037(8) -0.0032(8) -0.0012(9) OR6 0.0112(10) 0.0242(9) 0.0288(10) 0.0092(8) 0.0017(8) -0.0009(8) OR7 0.0180(11) 0.0150(9) 0.0264(9) -0.0009(8) 0.0051(8) 0.0023(8) OR8 0.0405(15) 0.0297(11) 0.0359(12) 0.0027(9) 0.0119(11) 0.0116(10) P1 0.0151(4) 0.0171(3) 0.0206(3) 0.0005(3) 0.0008(3) -0.0021(3) Co01 0.0106(2) 0.01001(18) 0.0198(2) 0.00007(16) 0.00012(18) -0.00062(16) O1W 0.0209(12) 0.0242(9) 0.0350(10) -0.0001(8) -0.0010(9) 0.0023(9) O2W 0.0190(12) 0.0305(10) 0.0313(10) -0.0036(9) 0.0032(9) -0.0010(9) O3W 0.0182(12) 0.0291(10) 0.0369(11) 0.0051(9) -0.0020(9) 0.0014(9) O4W 0.0277(13) 0.0325(11) 0.0360(11) 0.0048(9) -0.0010(10) -0.0021(10) O5W 0.0214(13) 0.0384(13) 0.0631(16) -0.0115(12) 0.0017(12) -0.0028(11) O6W 0.0457(17) 0.0411(13) 0.0442(13) 0.0013(11) 0.0130(12) 0.0060(12) O7W 0.0359(17) 0.0500(15) 0.0583(15) 0.0032(12) -0.0013(13) -0.0020(13) O8W 0.187(5) 0.0412(15) 0.0482(16) 0.0054(13) 0.020(2) -0.004(2) O9W 0.074(3) 0.0560(18) 0.084(2) 0.0112(17) -0.0108(19) -0.0009(18) O1A 0.0504(19) 0.0657(18) 0.0584(17) 0.0081(14) 0.0111(15) -0.0020(15) C1A 0.045(3) 0.049(2) 0.062(2) 0.0107(19) -0.011(2) -0.0142(19) C2A 0.039(2) 0.0274(16) 0.054(2) 0.0039(15) 0.0036(19) 0.0014(16) C3A 0.045(2) 0.0288(17) 0.062(2) 0.0018(16) -0.007(2) 0.0037(17) O2A 0.075(3) 0.0604(18) 0.0664(18) -0.0127(16) 0.0056(18) 0.0199(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N21 1.497(3) . ? C1 C20 1.527(4) . ? C1 C19 1.539(4) . ? C1 C2 1.581(4) . ? C2 C25 1.519(4) . ? C2 C26 1.542(4) . ? C2 C3 1.561(4) . ? C3 C4 1.509(4) . ? C3 C30 1.550(4) . ? C4 N21 1.298(4) . ? C4 C5 1.442(4) . ? C5 C6 1.375(4) . ? C5 C35 1.516(4) . ? C6 N22 1.390(4) . ? C6 C7 1.533(3) . ? C7 C36 1.526(4) . ? C7 C8 1.556(4) . ? C7 C37 1.567(4) . ? C8 C9 1.500(4) . ? C8 C41 1.541(4) . ? C9 N22 1.339(3) . ? C9 C10 1.387(4) . ? C10 C11 1.379(4) . ? C11 N23 1.343(3) . ? C11 C12 1.524(4) . ? C12 C46 1.514(4) . ? C12 C47 1.534(4) . ? C12 C13 1.536(4) . ? C13 C14 1.519(4) . ? C13 C48 1.549(4) . ? C14 C15 1.371(4) . ? C14 N23 1.389(4) . ? C15 C16 1.441(4) . ? C15 C53 1.517(4) . ? C16 N24 1.302(4) . ? C16 C17 1.548(3) . ? C17 C55 1.537(4) . ? C17 C54 1.544(4) . ? C17 C18 1.559(4) . ? C18 C19 1.529(3) . ? C18 C60 1.535(4) . ? C19 N24 1.481(3) . ? C26 C27 1.535(4) . ? C27 O28 1.233(4) . ? C27 N29 1.328(4) . ? C30 C31 1.536(4) . ? C31 C32 1.520(4) . ? C32 O33 1.249(4) . ? C32 N34 1.318(4) . ? C37 C38 1.500(4) . ? C38 O39 1.237(4) . ? C38 N40 1.339(4) . ? C41 C42 1.518(4) . ? C42 C43 1.500(4) . ? C43 O44 1.227(4) . ? C43 N45 1.348(4) . ? C48 C49 1.545(4) . ? C49 C50 1.507(4) . ? C50 O51 1.238(3) . ? C50 N52 1.327(4) . ? C60 C61 1.532(4) . ? C55 C56 1.527(4) . ? C56 C57 1.523(4) . ? C57 O58 1.242(4) . ? C57 N59 1.323(4) . ? C61 O62 1.228(4) . ? C61 N63 1.326(4) . ? PR1 N59 1.454(4) . ? PR1 PR2 1.511(4) . ? PR2 OP3 1.454(3) . ? PR2 PR3 1.504(4) . ? B2 NB3 1.311(4) . ? B2 NB1 1.356(3) . ? B4 B9 1.386(4) . ? B4 B5 1.387(4) . ? B5 B6 1.418(4) . ? B5 B10 1.510(5) . ? B6 B7 1.373(5) . ? B6 B11 1.509(4) . ? B7 B8 1.393(4) . ? B8 NB1 1.388(4) . ? B8 B9 1.390(4) . ? B9 NB3 1.405(3) . ? R1 OR6 1.412(3) . ? R1 NB1 1.453(4) . ? R1 R2 1.541(4) . ? L1 L2 1.207(4) . ? L1 Co01 1.870(3) . ? L2 L3 1.437(4) . ? R2 OR7 1.398(3) . ? R2 R3 1.523(4) . ? L3 L8 1.384(5) . ? L3 L4 1.395(5) . ? R3 OP2 1.435(3) . ? R3 R4 1.523(4) . ? L4 L5 1.388(5) . ? R4 OR6 1.453(3) . ? R4 R5 1.508(4) . ? L5 L6 1.348(6) . ? R5 OR8 1.423(4) . ? L6 L7 1.396(7) . ? L7 L8 1.377(5) . ? N21 Co01 1.880(2) . ? N22 Co01 1.914(2) . ? N23 Co01 1.914(2) . ? N24 Co01 1.891(2) . ? NB3 Co01 2.081(2) . ? OP2 P1 1.5945(19) . ? OP3 P1 1.5711(19) . ? OP4 P1 1.488(2) . ? OP5 P1 1.490(2) . ? O1A C2A 1.211(5) . ? C1A C2A 1.498(6) . ? C2A C3A 1.491(6) . ? O2A C4A2 1.117(10) . ? O2A C4A1 1.334(12) . ? C4A1 C5A1 1.436(14) . ? C4A1 C6A1 1.474(14) . ? C4A2 C6A2 1.452(15) . ? C4A2 C5A2 1.575(19) . ? O3A C7A 1.169(12) . ? C7A C8A 1.351(13) . ? C7A C9A 1.490(15) . ? O4A C10A 1.218(9) . ? C10A C11A 1.465(12) . ? 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 N21 C1 C20 110.7(2) . . ? N21 C1 C19 101.6(2) . . ? C20 C1 C19 109.1(2) . . ? N21 C1 C2 102.0(2) . . ? C20 C1 C2 113.5(2) . . ? C19 C1 C2 118.7(2) . . ? C25 C2 C26 110.3(2) . . ? C25 C2 C3 113.9(2) . . ? C26 C2 C3 107.3(2) . . ? C25 C2 C1 113.5(2) . . ? C26 C2 C1 109.9(2) . . ? C3 C2 C1 101.6(2) . . ? C4 C3 C30 108.7(2) . . ? C4 C3 C2 102.1(2) . . ? C30 C3 C2 119.1(2) . . ? N21 C4 C5 124.8(3) . . ? N21 C4 C3 111.5(2) . . ? C5 C4 C3 123.7(2) . . ? C6 C5 C4 120.8(3) . . ? C6 C5 C35 121.9(2) . . ? C4 C5 C35 117.3(2) . . ? C5 C6 N22 124.3(2) . . ? C5 C6 C7 126.9(3) . . ? N22 C6 C7 108.7(2) . . ? C36 C7 C6 117.2(2) . . ? C36 C7 C8 112.0(2) . . ? C6 C7 C8 100.6(2) . . ? C36 C7 C37 111.5(2) . . ? C6 C7 C37 105.2(2) . . ? C8 C7 C37 109.5(2) . . ? C9 C8 C41 111.2(2) . . ? C9 C8 C7 100.7(2) . . ? C41 C8 C7 113.6(2) . . ? N22 C9 C10 125.9(2) . . ? N22 C9 C8 110.9(2) . . ? C10 C9 C8 123.2(2) . . ? C11 C10 C9 125.1(3) . . ? N23 C11 C10 125.6(3) . . ? N23 C11 C12 110.8(2) . . ? C10 C11 C12 123.4(2) . . ? C46 C12 C11 113.1(2) . . ? C46 C12 C47 109.3(3) . . ? C11 C12 C47 107.1(3) . . ? C46 C12 C13 117.3(2) . . ? C11 C12 C13 101.1(2) . . ? C47 C12 C13 108.3(2) . . ? C14 C13 C12 101.9(2) . . ? C14 C13 C48 107.0(2) . . ? C12 C13 C48 117.3(2) . . ? C15 C14 N23 126.7(3) . . ? C15 C14 C13 124.4(3) . . ? N23 C14 C13 108.8(2) . . ? C14 C15 C16 121.0(3) . . ? C14 C15 C53 118.5(3) . . ? C16 C15 C53 120.5(2) . . ? N24 C16 C15 122.9(2) . . ? N24 C16 C17 110.7(2) . . ? C15 C16 C17 126.3(2) . . ? C55 C17 C54 109.0(2) . . ? C55 C17 C16 116.3(2) . . ? C54 C17 C16 107.2(2) . . ? C55 C17 C18 112.1(2) . . ? C54 C17 C18 111.5(2) . . ? C16 C17 C18 100.54(19) . . ? C19 C18 C60 113.3(2) . . ? C19 C18 C17 101.9(2) . . ? C60 C18 C17 116.2(2) . . ? N24 C19 C18 102.4(2) . . ? N24 C19 C1 106.94(19) . . ? C18 C19 C1 123.2(2) . . ? C27 C26 C2 116.5(2) . . ? O28 C27 N29 122.2(3) . . ? O28 C27 C26 122.9(2) . . ? N29 C27 C26 114.9(3) . . ? C31 C30 C3 114.1(2) . . ? C32 C31 C30 109.4(2) . . ? O33 C32 N34 122.1(3) . . ? O33 C32 C31 120.9(3) . . ? N34 C32 C31 117.0(3) . . ? C38 C37 C7 112.1(2) . . ? O39 C38 N40 122.4(3) . . ? O39 C38 C37 120.6(3) . . ? N40 C38 C37 116.9(3) . . ? C42 C41 C8 113.5(2) . . ? C43 C42 C41 113.7(3) . . ? O44 C43 N45 122.6(3) . . ? O44 C43 C42 123.4(3) . . ? N45 C43 C42 113.9(3) . . ? C49 C48 C13 116.5(2) . . ? C50 C49 C48 113.0(2) . . ? O51 C50 N52 122.4(3) . . ? O51 C50 C49 121.0(2) . . ? N52 C50 C49 116.6(3) . . ? C61 C60 C18 114.4(2) . . ? C56 C55 C17 115.6(2) . . ? C57 C56 C55 110.9(2) . . ? O58 C57 N59 122.7(3) . . ? O58 C57 C56 120.6(3) . . ? N59 C57 C56 116.6(3) . . ? O62 C61 N63 124.0(2) . . ? O62 C61 C60 120.9(2) . . ? N63 C61 C60 115.0(2) . . ? N59 PR1 PR2 112.1(2) . . ? OP3 PR2 PR3 108.9(2) . . ? OP3 PR2 PR1 107.2(2) . . ? PR3 PR2 PR1 112.3(2) . . ? NB3 B2 NB1 112.5(2) . . ? B9 B4 B5 119.3(3) . . ? B4 B5 B6 120.5(3) . . ? B4 B5 B10 119.4(3) . . ? B6 B5 B10 120.1(3) . . ? B7 B6 B5 120.3(3) . . ? B7 B6 B11 120.1(3) . . ? B5 B6 B11 119.6(3) . . ? B6 B7 B8 118.2(3) . . ? NB1 B8 B9 105.7(2) . . ? NB1 B8 B7 132.0(3) . . ? B9 B8 B7 122.3(3) . . ? B4 B9 B8 119.4(2) . . ? B4 B9 NB3 131.9(2) . . ? B8 B9 NB3 108.7(2) . . ? OR6 R1 NB1 106.9(2) . . ? OR6 R1 R2 106.7(2) . . ? NB1 R1 R2 113.2(2) . . ? L2 L1 Co01 174.0(3) . . ? L1 L2 L3 177.2(3) . . ? OR7 R2 R3 112.8(2) . . ? OR7 R2 R1 109.4(2) . . ? R3 R2 R1 99.5(2) . . ? L8 L3 L4 118.1(3) . . ? L8 L3 L2 121.5(3) . . ? L4 L3 L2 120.4(3) . . ? OP2 R3 R4 110.3(2) . . ? OP2 R3 R2 112.3(2) . . ? R4 R3 R2 105.1(2) . . ? L5 L4 L3 120.7(4) . . ? OR6 R4 R5 108.7(2) . . ? OR6 R4 R3 105.4(2) . . ? R5 R4 R3 114.1(2) . . ? L6 L5 L4 120.2(4) . . ? OR8 R5 R4 112.7(3) . . ? L5 L6 L7 120.2(3) . . ? L8 L7 L6 119.7(4) . . ? L7 L8 L3 120.9(4) . . ? C4 N21 C1 112.8(2) . . ? C4 N21 Co01 129.73(18) . . ? C1 N21 Co01 117.13(17) . . ? C9 N22 C6 110.1(2) . . ? C9 N22 Co01 123.10(19) . . ? C6 N22 Co01 126.34(17) . . ? C11 N23 C14 110.2(2) . . ? C11 N23 Co01 123.51(19) . . ? C14 N23 Co01 126.23(18) . . ? C16 N24 C19 111.5(2) . . ? C16 N24 Co01 132.40(19) . . ? C19 N24 Co01 113.63(17) . . ? C57 N59 PR1 123.9(3) . . ? B2 NB1 B8 107.2(2) . . ? B2 NB1 R1 124.9(2) . . ? B8 NB1 R1 125.9(2) . . ? B2 NB3 B9 105.8(2) . . ? B2 NB3 Co01 121.78(18) . . ? B9 NB3 Co01 132.35(19) . . ? R3 OP2 P1 119.43(16) . . ? PR2 OP3 P1 121.47(17) . . ? R1 OR6 R4 109.67(19) . . ? OP4 P1 OP5 116.57(11) . . ? OP4 P1 OP3 112.62(11) . . ? OP5 P1 OP3 106.48(11) . . ? OP4 P1 OP2 108.91(11) . . ? OP5 P1 OP2 110.47(12) . . ? OP3 P1 OP2 100.62(10) . . ? L1 Co01 N21 91.45(11) . . ? L1 Co01 N24 85.81(10) . . ? N21 Co01 N24 83.16(9) . . ? L1 Co01 N22 90.05(10) . . ? N21 Co01 N22 90.51(9) . . ? N24 Co01 N22 172.35(10) . . ? L1 Co01 N23 89.86(11) . . ? N21 Co01 N23 173.29(9) . . ? N24 Co01 N23 90.37(9) . . ? N22 Co01 N23 96.06(9) . . ? L1 Co01 NB3 177.14(11) . . ? N21 Co01 NB3 91.35(9) . . ? N24 Co01 NB3 95.07(9) . . ? N22 Co01 NB3 89.36(9) . . ? N23 Co01 NB3 87.42(9) . . ? O1A C2A C3A 122.6(4) . . ? O1A C2A C1A 121.1(4) . . ? C3A C2A C1A 116.2(4) . . ? C4A2 O2A C4A1 15.2(7) . . ? O2A C4A1 C5A1 117.4(9) . . ? O2A C4A1 C6A1 123.4(9) . . ? C5A1 C4A1 C6A1 118.7(9) . . ? O2A C4A2 C6A2 117.2(9) . . ? O2A C4A2 C5A2 131.7(11) . . ? C6A2 C4A2 C5A2 109.7(10) . . ? O3A C7A C8A 128.2(9) . . ? O3A C7A C9A 119.4(11) . . ? C8A C7A C9A 112.4(9) . . ? O4A C10A C11A 122.0(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.581 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.066 _database_code_depnum_ccdc_archive 'CCDC 961230'