# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_1 #TrackingRef 'web_deposit_cif_file_0_NeilChampness_1364485153.Champness.cif' _nottingham_internal_coll_name BWNRCC _nottingham_internal_coll_number 11445 _nottingham_internal_coll_client BW/NRC _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_time 15 _nottingham_internal_coll_frame_width 1.0 _nottingham_internal_coll_frame_method omega _nottingham_internal_coll_user 'Dr Peter N. Horton, NCS' _nottingham_internal_coll_date 12/06/2012 _nottingham_internal_coll_location SOTON _nottingham_internal_NCS_number 2012ncs0369 _nottingham_internal_process_user 'Dr Peter N. Horton, NCS' _nottingham_internal_process_date 12/06.2012 _nottingham_internal_solution_user 'Dr Peter N. Horton, NCS' _nottingham_internal_solution_date 12/06/2012 _nottingham_internal_refinement_user SPA/AGS _nottingham_internal_refinement_date 20/06/2012 _nottingham_internal_validation_user AJB _nottingham_internal_validation_date 20/6/2012 _nottingham_internal_archive_date ? _refine_special_details ; Rigid bond and similarity restraints (DELU, SIMU) have been applied to the anisotropic displacement parameters of all atoms in the structure owing to weak data arising from poor crystallinity. All hydrogen atoms were observed in the electron difference map before being geometrically placed and refined using a riding model. The C-C 1,2 and 1,3 distances in the butyl chains have all been constrained (DFIX) to have values of 1.50 and 2.50 respectively. The P-C distances, C-O carbonyl distances, C-N imide distances and C-C imide-perylene distances have all been restrained (SADI) to have similar values to their chemically identical equivalents. The terminal phenyl ring has been constrained to have regular hexagonal geometry (AFIX 66). A residual electron density peak of 3.46 e \%A^-3^ is observed 0.83 \%A from Pt1. This peak is likely to be artefact caused by deficiencies in the adsorption correction for the heavy-metal- containing platey crystal. A further electron density peak of 2.33 e \%A^-3^ is observed 1.54 \%A from C6. Although this is within the range of a chemical bond to the perylene core, the peak is in a chemically nonsensical position above the aromatic plane and likely to be a result of unresolved disorder or other experimental artefact. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H146 N2 O4 P4 Pt2' _chemical_formula_sum 'C104 H146 N2 O4 P4 Pt2' _chemical_formula_weight 2002.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 33.88(3) _cell_length_b 14.178(13) _cell_length_c 20.595(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9893(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18733 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 30.4 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method ? _exptl_crystal_F_000 4128 _exptl_absorpt_coefficient_mu 2.939 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.599 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source_power 2.5 _diffrn_source_voltage 45.0 _diffrn_source_current 55.0 _diffrn_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_specimen_support Mitegen _diffrn_detector CCD _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_details ; scan: Number of images: 180 Slice: -115.0000 - 65.0000 Image width: 1.0000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 15.0000 Phi: 135.0000 XTD: 55.6855 2theta: -24.3627 scan: Number of images: 117 Slice: -67.0000 - 50.0000 Image width: 1.0000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 60.0000 Phi: 45.0000 XTD: 55.6875 2theta: -23.0865 ; _diffrn_reflns_number 36399 _diffrn_reflns_av_R_equivalents 0.096 _diffrn_reflns_av_sigmaI/netI 0.073 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8315 _reflns_number_gt 6542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 3.1 b5 (Rigaku, 2011) ; _computing_cell_refinement ; CrystalClear-SM Expert 3.1 b5 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 3.1 b5 (Rigaku, 2011) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.165P)^2^+160.4P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8315 _refine_ls_number_parameters 511 _refine_ls_number_restraints 586 _refine_ls_R_factor_all 0.172 _refine_ls_R_factor_gt 0.149 _refine_ls_wR_factor_ref 0.385 _refine_ls_wR_factor_gt 0.364 _refine_ls_goodness_of_fit_ref 1.16 _refine_ls_restrained_S_all 1.13 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.40914(2) 0.73112(6) 0.55183(4) 0.0691(4) Uani 1 1 d U . . C1 C 0.5029(4) 0.7879(11) 0.3887(9) 0.056(3) Uani 1 1 d U . . C2 C 0.5404(5) 0.7856(11) 0.4179(9) 0.058(3) Uani 1 1 d U . . H2 H 0.5417 0.7802 0.4639 0.070 Uiso 1 1 calc R . . C3 C 0.5761(4) 0.7906(10) 0.3834(8) 0.054(3) Uani 1 1 d DU . . C4 C 0.6105(4) 0.8122(13) 0.2819(9) 0.063(3) Uani 1 1 d DU . . C5 C 0.6091(5) 0.8231(14) 0.2145(9) 0.068(4) Uani 1 1 d U . . H5 H 0.6329 0.8301 0.1906 0.081 Uiso 1 1 calc R . . C6 C 0.5732(4) 0.8238(14) 0.1825(10) 0.068(4) Uani 1 1 d U . . H6 H 0.5732 0.8325 0.1368 0.082 Uiso 1 1 calc R . . C14 C 0.5002(4) 0.8015(11) 0.3211(8) 0.054(3) Uani 1 1 d U . . C15 C 0.5374(4) 0.8068(12) 0.2829(9) 0.055(3) Uani 1 1 d U . . C16 C 0.5748(4) 0.8023(11) 0.3167(8) 0.053(3) Uani 1 1 d U . . C17 C 0.5374(4) 0.8124(13) 0.2137(9) 0.060(3) Uani 1 1 d U . . C21 C 0.6146(4) 0.7807(11) 0.4201(8) 0.059(3) Uani 1 1 d DU . . O22 O 0.6154(3) 0.7706(9) 0.4787(6) 0.070(3) Uani 1 1 d DU . . N23 N 0.6493(3) 0.7846(10) 0.3829(6) 0.067(3) Uani 1 1 d DU . . C24 C 0.6499(4) 0.8038(13) 0.3160(8) 0.067(3) Uani 1 1 d DU . . O25 O 0.6812(3) 0.8134(10) 0.2871(6) 0.076(3) Uani 1 1 d DU . . C31 C 0.6876(5) 0.7654(10) 0.4186(11) 0.075(4) Uani 1 1 d DU . . H31 H 0.6796 0.7495 0.4641 0.090 Uiso 1 1 calc R . . C32 C 0.7136(5) 0.8528(14) 0.4249(11) 0.082(4) Uani 1 1 d DU . . H32A H 0.6982 0.9048 0.4448 0.099 Uiso 1 1 calc R . . H32B H 0.7224 0.8735 0.3814 0.099 Uiso 1 1 calc R . . C33 C 0.7497(5) 0.8306(15) 0.4673(11) 0.091(5) Uani 1 1 d DU . . H33A H 0.7679 0.8853 0.4662 0.109 Uiso 1 1 calc R . . H33B H 0.7409 0.8223 0.5128 0.109 Uiso 1 1 calc R . . C34 C 0.7718(6) 0.7443(11) 0.4467(11) 0.096(5) Uani 1 1 d DU . . H34A H 0.7922 0.7296 0.4797 0.115 Uiso 1 1 calc R . . H34B H 0.7855 0.7574 0.4052 0.115 Uiso 1 1 calc R . . C35 C 0.7456(5) 0.6601(14) 0.4383(9) 0.081(4) Uani 1 1 d DU . . H35A H 0.7361 0.6396 0.4815 0.097 Uiso 1 1 calc R . . H35B H 0.7613 0.6079 0.4196 0.097 Uiso 1 1 calc R . . C36 C 0.7097(5) 0.6785(14) 0.3942(10) 0.079(4) Uani 1 1 d DU . . H36A H 0.7186 0.6890 0.3490 0.094 Uiso 1 1 calc R . . H36B H 0.6920 0.6231 0.3947 0.094 Uiso 1 1 calc R . . C50 C 0.4703(5) 0.7709(14) 0.4330(10) 0.068(4) Uani 1 1 d U . . C51 C 0.4464(6) 0.7548(14) 0.4780(11) 0.079(5) Uani 1 1 d U . . C52 C 0.3786(5) 0.7069(12) 0.6353(9) 0.062(3) Uani 1 1 d U . . C53 C 0.3619(5) 0.6945(13) 0.6820(10) 0.068(4) Uani 1 1 d U . . C54 C 0.3380(3) 0.6833(11) 0.7468(5) 0.078(4) Uani 1 1 d GU . . C55 C 0.3552(3) 0.7014(11) 0.8068(6) 0.087(4) Uani 1 1 d GU . . H55 H 0.3824 0.7169 0.8096 0.104 Uiso 1 1 calc R . . C56 C 0.3324(4) 0.6967(12) 0.8629(5) 0.098(5) Uani 1 1 d GU . . H56 H 0.3441 0.7090 0.9040 0.118 Uiso 1 1 calc R . . C57 C 0.2926(4) 0.6739(13) 0.8589(5) 0.097(5) Uani 1 1 d GU . . H57 H 0.2771 0.6707 0.8973 0.116 Uiso 1 1 calc R . . C58 C 0.2755(3) 0.6558(12) 0.7989(6) 0.091(5) Uani 1 1 d GU . . H58 H 0.2483 0.6403 0.7962 0.109 Uiso 1 1 calc R . . C59 C 0.2982(3) 0.6606(11) 0.7428(5) 0.082(4) Uani 1 1 d GU . . H59 H 0.2865 0.6482 0.7017 0.099 Uiso 1 1 calc R . . P60 P 0.41506(15) 0.8909(4) 0.5750(3) 0.0777(14) Uani 1 1 d DU . . C61A C 0.4661(4) 0.9354(16) 0.5738(9) 0.089(5) Uani 1 1 d DU . . H61A H 0.4792 0.9113 0.5342 0.107 Uiso 1 1 calc R . . H61B H 0.4652 1.0050 0.5704 0.107 Uiso 1 1 calc R . . C62A C 0.4909(4) 0.9095(17) 0.6315(8) 0.100(5) Uani 1 1 d DU . . H62A H 0.4884 0.8409 0.6394 0.120 Uiso 1 1 calc R . . H62B H 0.4806 0.9427 0.6702 0.120 Uiso 1 1 calc R . . C63A C 0.5337(3) 0.9337(17) 0.6231(8) 0.095(5) Uani 1 1 d DU . . H63A H 0.5450 0.8939 0.5882 0.114 Uiso 1 1 calc R . . H63B H 0.5359 1.0003 0.6092 0.114 Uiso 1 1 calc R . . C64A C 0.5572(5) 0.920(2) 0.6840(10) 0.126(9) Uani 1 1 d DU . . H64A H 0.5851 0.9336 0.6753 0.189 Uiso 1 1 calc R . . H64B H 0.5546 0.8542 0.6985 0.189 Uiso 1 1 calc R . . H64C H 0.5474 0.9621 0.7179 0.189 Uiso 1 1 calc R . . C61B C 0.3935(3) 0.9343(14) 0.6512(7) 0.078(4) Uani 1 1 d DU . . H61C H 0.4034 0.8946 0.6872 0.094 Uiso 1 1 calc R . . H61D H 0.4032 0.9993 0.6588 0.094 Uiso 1 1 calc R . . C62B C 0.3492(3) 0.9356(14) 0.6543(6) 0.075(4) Uani 1 1 d DU . . H62C H 0.3393 0.9899 0.6288 0.091 Uiso 1 1 calc R . . H62D H 0.3389 0.8774 0.6340 0.091 Uiso 1 1 calc R . . C63B C 0.3334(3) 0.9426(15) 0.7223(6) 0.081(5) Uani 1 1 d DU . . H63C H 0.3445 0.8905 0.7486 0.097 Uiso 1 1 calc R . . H63D H 0.3423 1.0028 0.7417 0.097 Uiso 1 1 calc R . . C64B C 0.2892(3) 0.9380(18) 0.7251(10) 0.098(7) Uani 1 1 d DU . . H64D H 0.2780 0.9856 0.6960 0.147 Uiso 1 1 calc R . . H64E H 0.2804 0.9502 0.7697 0.147 Uiso 1 1 calc R . . H64F H 0.2804 0.8752 0.7116 0.147 Uiso 1 1 calc R . . C61C C 0.3940(5) 0.9598(14) 0.5077(9) 0.093(5) Uani 1 1 d DU . . H61E H 0.3924 1.0263 0.5221 0.112 Uiso 1 1 calc R . . H61F H 0.4130 0.9577 0.4713 0.112 Uiso 1 1 calc R . . C62C C 0.3543(5) 0.9332(13) 0.4810(10) 0.095(5) Uani 1 1 d DU . . H62E H 0.3556 0.8682 0.4636 0.115 Uiso 1 1 calc R . . H62F H 0.3347 0.9336 0.5168 0.115 Uiso 1 1 calc R . . C63C C 0.3403(5) 0.9983(16) 0.4283(10) 0.113(6) Uani 1 1 d DU . . H63E H 0.3404 1.0638 0.4449 0.136 Uiso 1 1 calc R . . H63F H 0.3590 0.9952 0.3914 0.136 Uiso 1 1 calc R . . C64C C 0.2997(6) 0.975(2) 0.4045(12) 0.149(10) Uani 1 1 d DU . . H64G H 0.3010 0.9570 0.3586 0.224 Uiso 1 1 calc R . . H64H H 0.2825 1.0296 0.4097 0.224 Uiso 1 1 calc R . . H64I H 0.2892 0.9217 0.4298 0.224 Uiso 1 1 calc R . . P70 P 0.39860(14) 0.5753(4) 0.5215(3) 0.0806(16) Uani 1 1 d DU . . C71A C 0.3861(8) 0.4947(17) 0.5872(10) 0.159(9) Uani 1 1 d DU . . H71A H 0.3621 0.5176 0.6097 0.191 Uiso 1 1 calc R . . H71B H 0.3803 0.4316 0.5691 0.191 Uiso 1 1 calc R . . C72A C 0.4194(7) 0.487(2) 0.6350(11) 0.170(9) Uani 1 1 d DU . . H72A H 0.4401 0.4459 0.6167 0.204 Uiso 1 1 calc R . . H72B H 0.4311 0.5506 0.6415 0.204 Uiso 1 1 calc R . . C73A C 0.4067(8) 0.449(3) 0.6996(10) 0.197(11) Uani 1 1 d DU . . H73A H 0.3870 0.4920 0.7189 0.237 Uiso 1 1 calc R . . H73B H 0.3937 0.3870 0.6929 0.237 Uiso 1 1 calc R . . C74A C 0.4403(10) 0.437(3) 0.7460(13) 0.237(14) Uani 1 1 d DU . . H74A H 0.4563 0.3823 0.7330 0.355 Uiso 1 1 calc R . . H74B H 0.4300 0.4265 0.7899 0.355 Uiso 1 1 calc R . . H74C H 0.4568 0.4936 0.7456 0.355 Uiso 1 1 calc R . . C71B C 0.3560(7) 0.5609(19) 0.4687(13) 0.158(8) Uani 1 1 d DU . . H71C H 0.3524 0.4929 0.4597 0.189 Uiso 1 1 calc R . . H71D H 0.3322 0.5829 0.4923 0.189 Uiso 1 1 calc R . . C72B C 0.3581(7) 0.612(2) 0.4051(15) 0.192(9) Uani 1 1 d DU . . H72C H 0.3554 0.6809 0.4131 0.230 Uiso 1 1 calc R . . H72D H 0.3844 0.6015 0.3854 0.230 Uiso 1 1 calc R . . C73B C 0.3269(10) 0.5818(18) 0.3580(13) 0.217(11) Uani 1 1 d DU . . H73C H 0.3397 0.5559 0.3186 0.261 Uiso 1 1 calc R . . H73D H 0.3111 0.5307 0.3779 0.261 Uiso 1 1 calc R . . C74B C 0.2998(9) 0.660(2) 0.338(2) 0.200(14) Uani 1 1 d DU . . H74D H 0.2870 0.6865 0.3771 0.300 Uiso 1 1 calc R . . H74E H 0.2797 0.6363 0.3086 0.300 Uiso 1 1 calc R . . H74F H 0.3151 0.7100 0.3168 0.300 Uiso 1 1 calc R . . C71C C 0.4397(5) 0.5198(11) 0.4785(11) 0.083(5) Uani 1 1 d DU . . H71E H 0.4491 0.5641 0.4447 0.100 Uiso 1 1 calc R . . H71F H 0.4616 0.5108 0.5098 0.100 Uiso 1 1 calc R . . C72C C 0.4314(4) 0.4266(13) 0.4466(11) 0.102(6) Uani 1 1 d DU . . H72E H 0.4159 0.3869 0.4769 0.123 Uiso 1 1 calc R . . H72F H 0.4151 0.4374 0.4075 0.123 Uiso 1 1 calc R . . C73C C 0.4681(6) 0.3745(15) 0.4274(11) 0.133(8) Uani 1 1 d DU . . H73E H 0.4913 0.4081 0.4453 0.160 Uiso 1 1 calc R . . H73F H 0.4675 0.3107 0.4469 0.160 Uiso 1 1 calc R . . C74C C 0.4729(10) 0.365(3) 0.3554(12) 0.210(14) Uani 1 1 d DU . . H74G H 0.4514 0.3989 0.3335 0.316 Uiso 1 1 calc R . . H74H H 0.4721 0.2985 0.3433 0.316 Uiso 1 1 calc R . . H74I H 0.4983 0.3925 0.3423 0.316 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0554(5) 0.0538(6) 0.0981(7) 0.0034(4) 0.0184(3) -0.0043(3) C1 0.043(5) 0.041(7) 0.083(6) -0.003(6) -0.001(4) 0.002(6) C2 0.048(5) 0.038(8) 0.090(8) 0.005(7) -0.008(5) 0.004(6) C3 0.046(4) 0.035(7) 0.081(6) -0.001(6) -0.013(4) -0.002(6) C4 0.035(4) 0.064(8) 0.089(6) -0.004(7) -0.004(4) 0.004(6) C5 0.034(5) 0.081(10) 0.088(6) -0.004(8) 0.002(5) -0.002(7) C6 0.035(5) 0.083(10) 0.086(8) 0.001(8) 0.000(5) 0.000(7) C14 0.039(5) 0.044(7) 0.080(6) -0.013(6) -0.004(5) -0.005(6) C15 0.033(5) 0.050(7) 0.083(6) 0.002(7) -0.008(4) 0.000(6) C16 0.036(4) 0.040(7) 0.083(5) 0.001(6) -0.010(4) -0.004(6) C17 0.028(5) 0.069(9) 0.084(6) 0.000(8) -0.006(5) 0.000(6) C21 0.046(5) 0.043(8) 0.088(6) -0.003(7) -0.011(4) -0.001(6) O22 0.049(6) 0.073(8) 0.089(6) -0.003(7) -0.019(5) 0.001(6) N23 0.040(4) 0.065(8) 0.096(6) -0.011(6) -0.012(4) 0.000(5) C24 0.036(5) 0.070(9) 0.096(6) -0.012(8) -0.007(4) -0.001(7) O25 0.035(5) 0.094(9) 0.098(8) -0.009(7) -0.006(5) 0.002(6) C31 0.043(6) 0.081(8) 0.102(9) -0.011(8) -0.012(6) 0.004(5) C32 0.048(7) 0.090(9) 0.109(11) 0.002(9) -0.020(8) -0.007(6) C33 0.051(8) 0.105(10) 0.117(12) 0.006(9) -0.024(8) -0.002(7) C34 0.049(9) 0.114(11) 0.125(13) 0.010(10) -0.022(8) 0.006(6) C35 0.053(8) 0.103(10) 0.088(11) 0.002(9) -0.012(7) 0.013(7) C36 0.051(7) 0.089(9) 0.096(11) -0.002(8) -0.011(7) 0.017(6) C50 0.052(7) 0.065(9) 0.088(8) 0.004(8) 0.003(6) -0.002(7) C51 0.078(11) 0.064(9) 0.096(11) 0.004(8) 0.019(7) -0.015(8) C52 0.043(8) 0.051(8) 0.092(8) 0.012(6) 0.006(6) 0.001(6) C53 0.054(8) 0.063(9) 0.086(7) 0.005(8) 0.004(6) -0.001(7) C54 0.061(6) 0.091(10) 0.083(6) -0.003(8) 0.006(5) -0.007(8) C55 0.068(8) 0.106(12) 0.087(7) -0.006(10) 0.003(6) -0.012(9) C56 0.086(9) 0.126(13) 0.083(8) -0.001(10) 0.005(7) -0.009(10) C57 0.087(8) 0.131(13) 0.072(8) -0.006(10) 0.020(8) -0.013(10) C58 0.077(9) 0.124(13) 0.072(8) 0.000(10) 0.018(6) -0.012(10) C59 0.062(7) 0.116(12) 0.069(8) 0.004(9) 0.010(6) -0.015(9) P60 0.070(3) 0.063(3) 0.100(4) -0.004(3) 0.009(3) -0.011(2) C61A 0.072(6) 0.079(11) 0.116(13) 0.003(10) 0.020(6) -0.017(8) C62A 0.074(8) 0.096(12) 0.130(13) 0.004(10) 0.009(7) -0.015(9) C63A 0.075(8) 0.091(13) 0.120(13) 0.009(11) 0.017(8) -0.013(10) C64A 0.089(13) 0.15(2) 0.137(18) 0.021(17) -0.002(11) -0.027(16) C61B 0.069(7) 0.062(9) 0.104(8) -0.008(7) 0.009(7) -0.013(8) C62B 0.070(7) 0.057(9) 0.099(10) 0.003(8) 0.009(7) 0.004(8) C63B 0.073(8) 0.068(11) 0.102(10) -0.008(9) 0.011(8) -0.002(9) C64B 0.076(8) 0.105(17) 0.114(16) -0.013(13) 0.016(10) -0.007(12) C61C 0.096(10) 0.072(9) 0.112(10) 0.011(9) 0.007(8) -0.007(10) C62C 0.091(10) 0.096(12) 0.099(11) 0.008(9) 0.008(8) 0.002(9) C63C 0.110(12) 0.133(16) 0.097(13) 0.022(11) 0.016(9) 0.016(12) C64C 0.139(16) 0.22(3) 0.084(17) 0.018(18) -0.017(13) 0.001(19) P70 0.052(3) 0.044(3) 0.145(5) 0.002(3) 0.028(3) -0.004(2) C71A 0.27(3) 0.060(9) 0.145(15) -0.004(11) 0.112(11) -0.001(17) C72A 0.32(3) 0.060(12) 0.125(15) 0.020(12) 0.095(12) 0.012(17) C73A 0.37(3) 0.083(15) 0.138(16) 0.024(14) 0.111(15) -0.003(19) C74A 0.47(4) 0.11(2) 0.14(2) 0.02(2) 0.05(2) -0.01(3) C71B 0.100(11) 0.086(16) 0.29(2) -0.058(15) -0.064(14) 0.035(12) C72B 0.158(16) 0.130(18) 0.29(2) -0.041(15) -0.113(16) 0.040(14) C73B 0.176(19) 0.16(2) 0.31(2) -0.055(19) -0.124(17) 0.029(16) C74B 0.14(2) 0.17(3) 0.29(3) 0.01(3) -0.10(2) -0.002(19) C71C 0.060(8) 0.071(10) 0.118(13) -0.014(9) 0.017(8) -0.002(7) C72C 0.069(10) 0.088(11) 0.150(15) -0.039(10) 0.005(10) 0.008(8) C73C 0.091(12) 0.141(16) 0.168(16) -0.063(14) 0.023(13) 0.024(11) C74C 0.19(3) 0.27(3) 0.168(18) -0.02(3) 0.05(2) 0.08(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 Pt1 C51 2.00(2) . ? Pt1 C52 2.036(18) . ? Pt1 P60 2.323(6) . ? Pt1 P70 2.323(6) . ? C1 C2 1.41(2) . ? C1 C14 1.41(2) . ? C1 C50 1.45(2) . ? C2 C3 1.41(2) . ? C2 H2 0.9500 . ? C3 C16 1.38(2) . ? C3 C21 1.511(16) . ? C4 C5 1.40(2) . ? C4 C16 1.41(2) . ? C4 C24 1.514(16) . ? C5 C6 1.38(2) . ? C5 H5 0.9500 . ? C6 C17 1.38(2) . ? C6 H6 0.9500 . ? C14 C17 1.47(2) 4_655 ? C14 C15 1.49(2) . ? C15 C17 1.43(2) . ? C15 C16 1.45(2) . ? C17 C14 1.47(2) 4_655 ? C21 O22 1.218(16) . ? C21 N23 1.404(15) . ? N23 C24 1.404(15) . ? N23 C31 1.52(2) . ? C24 O25 1.223(15) . ? C31 C32 1.526(17) . ? C31 C36 1.527(17) . ? C31 H31 1.0000 . ? C32 C33 1.536(19) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.50(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.50(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.539(19) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C50 C51 1.25(3) . ? C52 C53 1.13(2) . ? C53 C54 1.57(2) . ? C54 C55 1.3900 . ? C54 C59 1.3900 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 C57 1.3900 . ? C56 H56 0.9500 . ? C57 C58 1.3900 . ? C57 H57 0.9500 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? P60 C61B 1.839(12) . ? P60 C61C 1.840(13) . ? P60 C61A 1.841(12) . ? C61A C62A 1.501(3) . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? C62A C63A 1.501(4) . ? C62A H62A 0.9900 . ? C62A H62B 0.9900 . ? C63A C64A 1.499(4) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A H64A 0.9800 . ? C64A H64B 0.9800 . ? C64A H64C 0.9800 . ? C61B C62B 1.502(4) . ? C61B H61C 0.9900 . ? C61B H61D 0.9900 . ? C62B C63B 1.500(4) . ? C62B H62C 0.9900 . ? C62B H62D 0.9900 . ? C63B C64B 1.500(4) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B H64D 0.9800 . ? C64B H64E 0.9800 . ? C64B H64F 0.9800 . ? C61C C62C 1.501(4) . ? C61C H61E 0.9900 . ? C61C H61F 0.9900 . ? C62C C63C 1.501(3) . ? C62C H62E 0.9900 . ? C62C H62F 0.9900 . ? C63C C64C 1.498(5) . ? C63C H63E 0.9900 . ? C63C H63F 0.9900 . ? C64C H64G 0.9800 . ? C64C H64H 0.9800 . ? C64C H64I 0.9800 . ? P70 C71B 1.819(14) . ? P70 C71A 1.822(14) . ? P70 C71C 1.827(12) . ? C71A C72A 1.501(3) . ? C71A H71A 0.9900 . ? C71A H71B 0.9900 . ? C72A C73A 1.501(4) . ? C72A H72A 0.9900 . ? C72A H72B 0.9900 . ? C73A C74A 1.499(4) . ? C73A H73A 0.9900 . ? C73A H73B 0.9900 . ? C74A H74A 0.9800 . ? C74A H74B 0.9800 . ? C74A H74C 0.9800 . ? C71B C72B 1.501(4) . ? C71B H71C 0.9900 . ? C71B H71D 0.9900 . ? C72B C73B 1.501(3) . ? C72B H72C 0.9900 . ? C72B H72D 0.9900 . ? C73B C74B 1.498(4) . ? C73B H73C 0.9900 . ? C73B H73D 0.9900 . ? C74B H74D 0.9800 . ? C74B H74E 0.9800 . ? C74B H74F 0.9800 . ? C71C C72C 1.501(4) . ? C71C H71E 0.9900 . ? C71C H71F 0.9900 . ? C72C C73C 1.500(3) . ? C72C H72E 0.9900 . ? C72C H72F 0.9900 . ? C73C C74C 1.498(4) . ? C73C H73E 0.9900 . ? C73C H73F 0.9900 . ? C74C H74G 0.9800 . ? C74C H74H 0.9800 . ? C74C H74I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C51 Pt1 C52 171.5(8) . . ? C51 Pt1 P60 86.4(6) . . ? C52 Pt1 P60 92.0(5) . . ? C51 Pt1 P70 93.0(6) . . ? C52 Pt1 P70 89.4(5) . . ? P60 Pt1 P70 174.5(2) . . ? C2 C1 C14 119.1(15) . . ? C2 C1 C50 114.4(16) . . ? C14 C1 C50 126.4(15) . . ? C3 C2 C1 124.0(17) . . ? C3 C2 H2 118.0 . . ? C1 C2 H2 118.0 . . ? C16 C3 C2 118.6(13) . . ? C16 C3 C21 122.4(15) . . ? C2 C3 C21 119.0(15) . . ? C5 C4 C16 119.0(14) . . ? C5 C4 C24 120.0(15) . . ? C16 C4 C24 120.8(15) . . ? C6 C5 C4 120.3(16) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C17 C6 C5 123.3(18) . . ? C17 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? C1 C14 C17 123.5(14) . 4_655 ? C1 C14 C15 118.4(14) . . ? C17 C14 C15 118.2(15) 4_655 . ? C17 C15 C16 118.9(14) . . ? C17 C15 C14 122.1(13) . . ? C16 C15 C14 119.0(15) . . ? C3 C16 C4 119.1(14) . . ? C3 C16 C15 120.8(14) . . ? C4 C16 C15 120.0(15) . . ? C6 C17 C15 118.1(14) . . ? C6 C17 C14 123.2(17) . 4_655 ? C15 C17 C14 118.6(14) . 4_655 ? O22 C21 N23 121.8(13) . . ? O22 C21 C3 121.7(14) . . ? N23 C21 C3 116.5(13) . . ? C24 N23 C21 123.7(14) . . ? C24 N23 C31 119.8(13) . . ? C21 N23 C31 116.5(13) . . ? O25 C24 N23 120.8(14) . . ? O25 C24 C4 121.9(15) . . ? N23 C24 C4 117.3(13) . . ? N23 C31 C32 112.9(13) . . ? N23 C31 C36 113.9(13) . . ? C32 C31 C36 113.6(16) . . ? N23 C31 H31 105.1 . . ? C32 C31 H31 105.1 . . ? C36 C31 H31 105.1 . . ? C31 C32 C33 110.0(14) . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C32 113.9(16) . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C32 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 112.9(19) . . ? C33 C34 H34A 109.0 . . ? C35 C34 H34A 109.0 . . ? C33 C34 H34B 109.0 . . ? C35 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C34 C35 C36 113.7(15) . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C31 C36 C35 109.3(14) . . ? C31 C36 H36A 109.8 . . ? C35 C36 H36A 109.8 . . ? C31 C36 H36B 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? C51 C50 C1 171(2) . . ? C50 C51 Pt1 178(2) . . ? C53 C52 Pt1 179.1(19) . . ? C52 C53 C54 177(2) . . ? C55 C54 C59 120.0 . . ? C55 C54 C53 121.6(10) . . ? C59 C54 C53 118.3(10) . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C57 C56 C55 120.0 . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C59 C58 C57 120.0 . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C54 120.0 . . ? C58 C59 H59 120.0 . . ? C54 C59 H59 120.0 . . ? C61B P60 C61C 108.1(10) . . ? C61B P60 C61A 105.7(9) . . ? C61C P60 C61A 99.9(8) . . ? C61B P60 Pt1 117.9(7) . . ? C61C P60 Pt1 109.3(8) . . ? C61A P60 Pt1 114.4(8) . . ? C62A C61A P60 115.5(10) . . ? C62A C61A H61A 108.4 . . ? P60 C61A H61A 108.4 . . ? C62A C61A H61B 108.4 . . ? P60 C61A H61B 108.4 . . ? H61A C61A H61B 107.5 . . ? C61A C62A C63A 113.1(6) . . ? C61A C62A H62A 108.9 . . ? C63A C62A H62A 108.9 . . ? C61A C62A H62B 108.9 . . ? C63A C62A H62B 108.9 . . ? H62A C62A H62B 107.8 . . ? C64A C63A C62A 112.8(6) . . ? C64A C63A H63A 109.0 . . ? C62A C63A H63A 109.0 . . ? C64A C63A H63B 109.0 . . ? C62A C63A H63B 109.0 . . ? H63A C63A H63B 107.8 . . ? C63A C64A H64A 109.5 . . ? C63A C64A H64B 109.5 . . ? H64A C64A H64B 109.5 . . ? C63A C64A H64C 109.5 . . ? H64A C64A H64C 109.5 . . ? H64B C64A H64C 109.5 . . ? C62B C61B P60 116.0(9) . . ? C62B C61B H61C 108.3 . . ? P60 C61B H61C 108.3 . . ? C62B C61B H61D 108.3 . . ? P60 C61B H61D 108.3 . . ? H61C C61B H61D 107.4 . . ? C63B C62B C61B 113.3(6) . . ? C63B C62B H62C 108.9 . . ? C61B C62B H62C 108.9 . . ? C63B C62B H62D 108.9 . . ? C61B C62B H62D 108.9 . . ? H62C C62B H62D 107.7 . . ? C64B C63B C62B 112.9(6) . . ? C64B C63B H63C 109.0 . . ? C62B C63B H63C 109.0 . . ? C64B C63B H63D 109.0 . . ? C62B C63B H63D 109.0 . . ? H63C C63B H63D 107.8 . . ? C63B C64B H64D 109.5 . . ? C63B C64B H64E 109.5 . . ? H64D C64B H64E 109.5 . . ? C63B C64B H64F 109.5 . . ? H64D C64B H64F 109.5 . . ? H64E C64B H64F 109.5 . . ? C62C C61C P60 119.4(10) . . ? C62C C61C H61E 107.5 . . ? P60 C61C H61E 107.5 . . ? C62C C61C H61F 107.5 . . ? P60 C61C H61F 107.5 . . ? H61E C61C H61F 107.0 . . ? C63C C62C C61C 113.1(6) . . ? C63C C62C H62E 109.0 . . ? C61C C62C H62E 109.0 . . ? C63C C62C H62F 109.0 . . ? C61C C62C H62F 109.0 . . ? H62E C62C H62F 107.8 . . ? C64C C63C C62C 112.8(7) . . ? C64C C63C H63E 109.0 . . ? C62C C63C H63E 109.0 . . ? C64C C63C H63F 109.0 . . ? C62C C63C H63F 109.0 . . ? H63E C63C H63F 107.8 . . ? C63C C64C H64G 109.5 . . ? C63C C64C H64H 109.5 . . ? H64G C64C H64H 109.5 . . ? C63C C64C H64I 109.5 . . ? H64G C64C H64I 109.5 . . ? H64H C64C H64I 109.5 . . ? C71B P70 C71A 100.9(14) . . ? C71B P70 C71C 105.5(12) . . ? C71A P70 C71C 105.4(11) . . ? C71B P70 Pt1 112.9(9) . . ? C71A P70 Pt1 115.6(9) . . ? C71C P70 Pt1 115.0(5) . . ? C72A C71A P70 110.9(14) . . ? C72A C71A H71A 109.5 . . ? P70 C71A H71A 109.5 . . ? C72A C71A H71B 109.5 . . ? P70 C71A H71B 109.5 . . ? H71A C71A H71B 108.0 . . ? C73A C72A C71A 113.0(7) . . ? C73A C72A H72A 109.0 . . ? C71A C72A H72A 109.0 . . ? C73A C72A H72B 109.0 . . ? C71A C72A H72B 109.0 . . ? H72A C72A H72B 107.8 . . ? C74A C73A C72A 112.8(7) . . ? C74A C73A H73A 109.0 . . ? C72A C73A H73A 109.0 . . ? C74A C73A H73B 109.0 . . ? C72A C73A H73B 109.0 . . ? H73A C73A H73B 107.8 . . ? C73A C74A H74A 109.5 . . ? C73A C74A H74B 109.5 . . ? H74A C74A H74B 109.5 . . ? C73A C74A H74C 109.5 . . ? H74A C74A H74C 109.5 . . ? H74B C74A H74C 109.5 . . ? C72B C71B P70 115.3(16) . . ? C72B C71B H71C 108.4 . . ? P70 C71B H71C 108.4 . . ? C72B C71B H71D 108.4 . . ? P70 C71B H71D 108.4 . . ? H71C C71B H71D 107.5 . . ? C73B C72B C71B 112.9(7) . . ? C73B C72B H72C 109.0 . . ? C71B C72B H72C 109.0 . . ? C73B C72B H72D 109.0 . . ? C71B C72B H72D 109.0 . . ? H72C C72B H72D 107.8 . . ? C74B C73B C72B 113.0(7) . . ? C74B C73B H73C 109.0 . . ? C72B C73B H73C 109.0 . . ? C74B C73B H73D 109.0 . . ? C72B C73B H73D 109.0 . . ? H73C C73B H73D 107.8 . . ? C73B C74B H74D 109.5 . . ? C73B C74B H74E 109.5 . . ? H74D C74B H74E 109.5 . . ? C73B C74B H74F 109.5 . . ? H74D C74B H74F 109.5 . . ? H74E C74B H74F 109.5 . . ? C72C C71C P70 116.6(10) . . ? C72C C71C H71E 108.1 . . ? P70 C71C H71E 108.1 . . ? C72C C71C H71F 108.1 . . ? P70 C71C H71F 108.1 . . ? H71E C71C H71F 107.3 . . ? C73C C72C C71C 113.2(7) . . ? C73C C72C H72E 108.9 . . ? C71C C72C H72E 108.9 . . ? C73C C72C H72F 108.9 . . ? C71C C72C H72F 108.9 . . ? H72E C72C H72F 107.8 . . ? C74C C73C C72C 113.2(7) . . ? C74C C73C H73E 108.9 . . ? C72C C73C H73E 108.9 . . ? C74C C73C H73F 108.9 . . ? C72C C73C H73F 108.9 . . ? H73E C73C H73F 107.7 . . ? C73C C74C H74G 109.5 . . ? C73C C74C H74H 109.5 . . ? H74G C74C H74H 109.5 . . ? C73C C74C H74I 109.5 . . ? H74G C74C H74I 109.5 . . ? H74H C74C H74I 109.5 . . ? 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 C14 C1 C2 C3 -4(2) . . . . ? C50 C1 C2 C3 173.3(15) . . . . ? C1 C2 C3 C16 3(2) . . . . ? C1 C2 C3 C21 -175.9(14) . . . . ? C16 C4 C5 C6 0(3) . . . . ? C24 C4 C5 C6 175.1(17) . . . . ? C4 C5 C6 C17 -1(3) . . . . ? C2 C1 C14 C17 -175.1(15) . . . 4_655 ? C50 C1 C14 C17 8(3) . . . 4_655 ? C2 C1 C14 C15 4(2) . . . . ? C50 C1 C14 C15 -172.9(16) . . . . ? C1 C14 C15 C17 174.6(15) . . . . ? C17 C14 C15 C17 -6(2) 4_655 . . . ? C1 C14 C15 C16 -3(2) . . . . ? C17 C14 C15 C16 176.1(15) 4_655 . . . ? C2 C3 C16 C4 176.8(14) . . . . ? C21 C3 C16 C4 -5(2) . . . . ? C2 C3 C16 C15 -2(2) . . . . ? C21 C3 C16 C15 176.9(14) . . . . ? C5 C4 C16 C3 179.4(16) . . . . ? C24 C4 C16 C3 4(2) . . . . ? C5 C4 C16 C15 -2(2) . . . . ? C24 C4 C16 C15 -177.5(16) . . . . ? C17 C15 C16 C3 -175.8(15) . . . . ? C14 C15 C16 C3 2(2) . . . . ? C17 C15 C16 C4 6(2) . . . . ? C14 C15 C16 C4 -176.6(15) . . . . ? C5 C6 C17 C15 5(3) . . . . ? C5 C6 C17 C14 -172.3(17) . . . 4_655 ? C16 C15 C17 C6 -7(3) . . . . ? C14 C15 C17 C6 175.5(16) . . . . ? C16 C15 C17 C14 170.2(15) . . . 4_655 ? C14 C15 C17 C14 -7(2) . . . 4_655 ? C16 C3 C21 O22 179.9(15) . . . . ? C2 C3 C21 O22 -2(2) . . . . ? C16 C3 C21 N23 0(2) . . . . ? C2 C3 C21 N23 178.9(14) . . . . ? O22 C21 N23 C24 -174.7(16) . . . . ? C3 C21 N23 C24 5(2) . . . . ? O22 C21 N23 C31 6(2) . . . . ? C3 C21 N23 C31 -174.3(12) . . . . ? C21 N23 C24 O25 174.3(16) . . . . ? C31 N23 C24 O25 -7(3) . . . . ? C21 N23 C24 C4 -5(2) . . . . ? C31 N23 C24 C4 173.8(14) . . . . ? C5 C4 C24 O25 6(3) . . . . ? C16 C4 C24 O25 -178.9(17) . . . . ? C5 C4 C24 N23 -174.5(17) . . . . ? C16 C4 C24 N23 1(2) . . . . ? C24 N23 C31 C32 70(2) . . . . ? C21 N23 C31 C32 -111.0(19) . . . . ? C24 N23 C31 C36 -62(2) . . . . ? C21 N23 C31 C36 117.5(19) . . . . ? N23 C31 C32 C33 174.3(16) . . . . ? C36 C31 C32 C33 -54(3) . . . . ? C31 C32 C33 C34 51(3) . . . . ? C32 C33 C34 C35 -51(3) . . . . ? C33 C34 C35 C36 52(3) . . . . ? N23 C31 C36 C35 -174.2(15) . . . . ? C32 C31 C36 C35 55(2) . . . . ? C34 C35 C36 C31 -53(2) . . . . ? C2 C1 C50 C51 -1(13) . . . . ? C14 C1 C50 C51 176(12) . . . . ? C1 C50 C51 Pt1 32(75) . . . . ? C52 Pt1 C51 C50 -29(70) . . . . ? P60 Pt1 C51 C50 51(67) . . . . ? P70 Pt1 C51 C50 -135(67) . . . . ? C51 Pt1 C52 C53 59(100) . . . . ? P60 Pt1 C52 C53 -20(100) . . . . ? P70 Pt1 C52 C53 165(100) . . . . ? Pt1 C52 C53 C54 42(100) . . . . ? C52 C53 C54 C55 -85(35) . . . . ? C52 C53 C54 C59 91(35) . . . . ? C59 C54 C55 C56 0.0 . . . . ? C53 C54 C55 C56 175.8(15) . . . . ? C54 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C58 0.0 . . . . ? C56 C57 C58 C59 0.0 . . . . ? C57 C58 C59 C54 0.0 . . . . ? C55 C54 C59 C58 0.0 . . . . ? C53 C54 C59 C58 -176.0(14) . . . . ? C51 Pt1 P60 C61B -171.0(9) . . . . ? C52 Pt1 P60 C61B 0.6(8) . . . . ? P70 Pt1 P60 C61B 105(2) . . . . ? C51 Pt1 P60 C61C 65.2(10) . . . . ? C52 Pt1 P60 C61C -123.2(9) . . . . ? P70 Pt1 P60 C61C -19(2) . . . . ? C51 Pt1 P60 C61A -45.9(9) . . . . ? C52 Pt1 P60 C61A 125.7(8) . . . . ? P70 Pt1 P60 C61A -130(2) . . . . ? C61B P60 C61A C62A 56(2) . . . . ? C61C P60 C61A C62A 167.9(18) . . . . ? Pt1 P60 C61A C62A -75.5(19) . . . . ? P60 C61A C62A C63A 170.5(17) . . . . ? C61A C62A C63A C64A 172(2) . . . . ? C61C P60 C61B C62B 54.3(16) . . . . ? C61A P60 C61B C62B 160.6(14) . . . . ? Pt1 P60 C61B C62B -70.1(16) . . . . ? P60 C61B C62B C63B 162.3(14) . . . . ? C61B C62B C63B C64B -176.6(18) . . . . ? C61B P60 C61C C62C -82(2) . . . . ? C61A P60 C61C C62C 168(2) . . . . ? Pt1 P60 C61C C62C 47(2) . . . . ? P60 C61C C62C C63C 177.6(19) . . . . ? C61C C62C C63C C64C -177(2) . . . . ? C51 Pt1 P70 C71B -92.8(13) . . . . ? C52 Pt1 P70 C71B 95.4(12) . . . . ? P60 Pt1 P70 C71B -9(2) . . . . ? C51 Pt1 P70 C71A 151.7(12) . . . . ? C52 Pt1 P70 C71A -20.1(11) . . . . ? P60 Pt1 P70 C71A -125(2) . . . . ? C51 Pt1 P70 C71C 28.4(11) . . . . ? C52 Pt1 P70 C71C -143.4(10) . . . . ? P60 Pt1 P70 C71C 112(2) . . . . ? C71B P70 C71A C72A 175(2) . . . . ? C71C P70 C71A C72A 65(2) . . . . ? Pt1 P70 C71A C72A -63(2) . . . . ? P70 C71A C72A C73A 161(2) . . . . ? C71A C72A C73A C74A 177(3) . . . . ? C71A P70 C71B C72B -175(2) . . . . ? C71C P70 C71B C72B -65(2) . . . . ? Pt1 P70 C71B C72B 61(2) . . . . ? P70 C71B C72B C73B 167.5(18) . . . . ? C71B C72B C73B C74B 119(3) . . . . ? C71B P70 C71C C72C -43(2) . . . . ? C71A P70 C71C C72C 63(2) . . . . ? Pt1 P70 C71C C72C -168.3(16) . . . . ? P70 C71C C72C C73C -165.4(15) . . . . ? C71C C72C C73C C74C -113(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 3.46 _refine_diff_density_min -3.89 _refine_diff_density_rms 0.19 _database_code_depnum_ccdc_archive 'CCDC 931600' ####################################################################### # # 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_BWNRCB #TrackingRef 'web_deposit_cif_file_0_NeilChampness_1364485153.Champness.cif' _nottingham_internal_coll_name BWNRCB _nottingham_internal_coll_number 11067 _nottingham_internal_coll_client BW/NRC _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_time 40 _nottingham_internal_coll_frame_width 1.0 _nottingham_internal_coll_frame_method omega _nottingham_internal_coll_user 'Dr Peter N. Horton, NCS' _nottingham_internal_coll_date 8/2/2012 _nottingham_internal_coll_location SOTON _nottingham_internal_NCS_number 2012ncs0010 _nottingham_internal_process_user 'Dr Peter N. Horton, NCS' _nottingham_internal_process_date 8/2/2012 _nottingham_internal_solution_user 'Dr Peter N. Horton, NCS' _nottingham_internal_solution_date 8/2/2012 _nottingham_internal_refinement_user SPA/AGS _nottingham_internal_refinement_date 02/06/2012 _nottingham_internal_validation_user ? _nottingham_internal_validation_date ? _nottingham_internal_archive_date ? _refine_special_details ; Rigid bond and similarity restraints (DELU, SIMU) have been applied to the anisotropic displacement parameters of all atoms in the structure owing to weak data arising from poor crystallinity. The anisotropic displacement parameters of the isopropyl groups have been restrained to be more isotropic (ISOR). Disorder was observed in the conformation of cyclohexyl ring C41-c46. The occupancies of the two components have been refined and constrained to sum to unity (major component occupancy 0.55(1)). Geometric similarity restraints (SAME) have been applied to the 1,2 and 1,3 bond lengths of the disordered and ordered cyclohexyl groups reflecting their 2-fold symmetry. The atoms of the two disordered rings have been refined with isotropic displacement parameters. Disorder was observed in the orientation of isopropyl group C88-C90. The two components share the position of the methine carbon (C88A/C88B) and one methyl carbon (C89A/C89B), these atoms have been fixed to have the same positions and displacement parameters. The occupancies of the two components have been refined and constrained to sum to unity (major component occupancy 0.55(2)). The atoms of the two disordered groups have been refined with isotropic displacement parameters. The CH-CH3 bonds of the disordered group have been constrained (DFIX) to have a bond length of 1.55(0.01) A. Geometric similarity restraints (SADI) have been applied to the 1,2 bond lengths of the two entire triisopropylacetylene groups and additionally the 1,3 bond lengths of the isopropyl groups. All hydrogen atoms were observed in the electron density map before being geometrically placed and refined using a riding model. A residual electron density peak of 1.11 e A-3 is observed 1.56 A from C86. This peak is likely to be a result of further unresolved disorder in the triisopropylsilyl group. A short contact (1.98 A) is observed between H42A and H87C. This is a result of a clash between a disordered group (cyclohexyl ring C41-C46) and a methyl hydrogen which has been modelled in an idealised rather than refined postion as a result of poor convergence. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H68 N2 O4 Si2' _chemical_formula_sum 'C58 H68 N2 O4 Si2' _chemical_formula_weight 913.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.734(8) _cell_length_b 12.986(5) _cell_length_c 23.8022(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.456(7) _cell_angle_gamma 90.00 _cell_volume 5102(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13505 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 31.4 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_specimen_support Mitegen _diffrn_detector CCD _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 28020 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 24.71 _diffrn_measurement_details ; scan: Number of images: 164 Slice: -94.0000 - 70.0000 Image width: 1.0000 Exp time: 40.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 15.0000 Phi: 45.0000 XTD: 44.8717 2theta: -19.6488 scan: Number of images: 48 Slice: -58.0000 - -10.0000 Image width: 1.0000 Exp time: 40.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 70.0000 Phi: 315.0000 XTD: 44.8717 2theta: -19.6488 scan: Number of images: 53 Slice: -58.0000 - -5.0000 Image width: 1.0000 Exp time: 40.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 70.0000 Phi: 45.0000 XTD: 44.8717 2theta: -19.6488 scan: Number of images: 38 Slice: -80.0000 - -42.0000 Image width: 1.0000 Exp time: 40.0000 Rotation axis: Omega Omega: 0.0000 Kappa: -70.0000 Phi: 270.0000 XTD: 44.8717 2theta: -19.6488 ; _reflns_number_total 8667 _reflns_number_gt 6226 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8667 _refine_ls_number_parameters 580 _refine_ls_number_restraints 807 _refine_ls_R_factor_all 0.2130 _refine_ls_R_factor_gt 0.1845 _refine_ls_wR_factor_ref 0.5150 _refine_ls_wR_factor_gt 0.4952 _refine_ls_goodness_of_fit_ref 1.906 _refine_ls_restrained_S_all 1.972 _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 0.3478(4) 0.4192(5) 0.8976(3) 0.0681(15) Uani 1 1 d DU . . C2 C 0.2719(4) 0.4648(5) 0.8680(3) 0.0736(16) Uani 1 1 d U . . H2 H 0.2247 0.4294 0.8673 0.088 Uiso 1 1 calc R . . C3 C 0.2634(4) 0.5588(6) 0.8401(3) 0.0777(16) Uani 1 1 d U . . C4 C 0.3225(5) 0.7022(5) 0.8068(3) 0.0800(17) Uani 1 1 d U . . C5 C 0.3908(5) 0.7520(6) 0.8060(3) 0.0828(18) Uani 1 1 d U . . H5 H 0.3856 0.8174 0.7871 0.099 Uiso 1 1 calc R . . C6 C 0.4654(5) 0.7092(5) 0.8318(3) 0.0827(18) Uani 1 1 d U . . H6 H 0.5108 0.7461 0.8302 0.099 Uiso 1 1 calc R . . C7 C 0.6268(4) 0.5978(5) 0.8710(3) 0.0781(17) Uani 1 1 d DU . . C8 C 0.7045(5) 0.5531(6) 0.9012(3) 0.0843(18) Uani 1 1 d U . . H8 H 0.7491 0.5748 0.8911 0.101 Uiso 1 1 calc R . . C9 C 0.7155(4) 0.4805(6) 0.9438(3) 0.0756(16) Uani 1 1 d U . . C10 C 0.6612(4) 0.3638(5) 1.0002(3) 0.0667(14) Uani 1 1 d U . . C11 C 0.5957(4) 0.3233(5) 1.0111(3) 0.0686(15) Uani 1 1 d U . . H11 H 0.6044 0.2708 1.0405 0.082 Uiso 1 1 calc R . . C12 C 0.5173(4) 0.3579(5) 0.9799(2) 0.0649(14) Uani 1 1 d U . . H12 H 0.4735 0.3280 0.9880 0.078 Uiso 1 1 calc R . . C13 C 0.5020(4) 0.4360(4) 0.9367(2) 0.0621(14) Uani 1 1 d U . . C14 C 0.4202(4) 0.4689(4) 0.9010(2) 0.0596(13) Uani 1 1 d U . . C15 C 0.4114(4) 0.5634(4) 0.8656(2) 0.0629(14) Uani 1 1 d U . . C16 C 0.3321(4) 0.6081(5) 0.8376(3) 0.0723(15) Uani 1 1 d U . . C17 C 0.4783(4) 0.6145(5) 0.8603(2) 0.0686(15) Uani 1 1 d U . . C18 C 0.5592(4) 0.5671(5) 0.8869(3) 0.0687(14) Uani 1 1 d U . . C19 C 0.5693(4) 0.4837(4) 0.9270(3) 0.0625(13) Uani 1 1 d U . . C20 C 0.6477(4) 0.4421(5) 0.9578(3) 0.0640(14) Uani 1 1 d U . . C21 C 0.1819(5) 0.6032(7) 0.8118(3) 0.0889(19) Uani 1 1 d U A . O22 O 0.1236(3) 0.5646(5) 0.8179(3) 0.1086(18) Uani 1 1 d U . . N23 N 0.1747(4) 0.6941(5) 0.7816(3) 0.106(2) Uani 1 1 d U . . C24 C 0.2419(5) 0.7459(6) 0.7764(3) 0.0891(19) Uani 1 1 d U A . O25 O 0.2326(4) 0.8286(5) 0.7483(2) 0.1083(18) Uani 1 1 d U . . C26 C 0.7966(4) 0.4334(6) 0.9721(3) 0.0814(18) Uani 1 1 d U . . O27 O 0.8513(3) 0.4556(5) 0.9544(2) 0.1012(17) Uani 1 1 d U . . N28 N 0.8083(3) 0.3633(5) 1.0197(2) 0.0815(15) Uani 1 1 d U . . C29 C 0.7446(4) 0.3235(5) 1.0339(3) 0.0729(16) Uani 1 1 d U . . O30 O 0.7560(3) 0.2579(4) 1.0724(2) 0.0801(13) Uani 1 1 d U . . C31 C 0.8919(5) 0.3241(6) 1.0523(3) 0.100(2) Uani 1 1 d DU . . C36 C 0.9532(5) 0.4099(8) 1.0760(4) 0.126(3) Uani 1 1 d DU . . H36A H 0.9349 0.4581 1.1006 0.151 Uiso 1 1 calc R . . H36B H 0.9584 0.4489 1.0418 0.151 Uiso 1 1 calc R . . C35 C 1.0362(5) 0.3628(10) 1.1150(5) 0.141(3) Uani 1 1 d DU . . H35A H 1.0772 0.4182 1.1291 0.170 Uiso 1 1 calc R . . H35B H 1.0318 0.3289 1.1509 0.170 Uiso 1 1 calc R . . C34 C 1.0626(7) 0.2866(10) 1.0797(6) 0.170(4) Uani 1 1 d DU . . H34A H 1.1150 0.2566 1.1059 0.204 Uiso 1 1 calc R . . H34B H 1.0713 0.3222 1.0458 0.204 Uiso 1 1 calc R . . C33 C 1.0030(6) 0.2019(9) 1.0551(5) 0.147(4) Uani 1 1 d DU . . H33A H 0.9989 0.1607 1.0888 0.176 Uiso 1 1 calc R . . H33B H 1.0222 0.1560 1.0299 0.176 Uiso 1 1 calc R . . C32 C 0.9175(6) 0.2453(8) 1.0161(4) 0.122(3) Uani 1 1 d DU . . H32A H 0.9195 0.2776 0.9790 0.146 Uiso 1 1 calc R . . H32B H 0.8776 0.1884 1.0041 0.146 Uiso 1 1 calc R . . C41A C 0.0993(8) 0.7553(11) 0.7394(6) 0.094(4) Uiso 0.554(14) 1 d PDU A 2 C42A C 0.0299(8) 0.6902(11) 0.6989(7) 0.101(5) Uiso 0.554(14) 1 d PDU A 2 H42A H 0.0170 0.6331 0.7214 0.121 Uiso 0.554(14) 1 calc PR A 2 H42B H 0.0416 0.6618 0.6643 0.121 Uiso 0.554(14) 1 calc PR A 2 C43A C -0.0397(9) 0.7715(13) 0.6779(8) 0.102(6) Uiso 0.554(14) 1 d PDU A 2 H43A H -0.0457 0.7904 0.6362 0.122 Uiso 0.554(14) 1 calc PR A 2 H43B H -0.0897 0.7338 0.6746 0.122 Uiso 0.554(14) 1 calc PR A 2 C44A C -0.0428(12) 0.8694(13) 0.7085(6) 0.122(6) Uiso 0.554(14) 1 d PDU A 2 H44A H -0.1005 0.8868 0.6992 0.146 Uiso 0.554(14) 1 calc PR A 2 H44B H -0.0198 0.9240 0.6906 0.146 Uiso 0.554(14) 1 calc PR A 2 C45A C -0.0007(8) 0.8732(12) 0.7747(7) 0.101(5) Uiso 0.554(14) 1 d PDU A 2 H45A H -0.0353 0.8444 0.7954 0.121 Uiso 0.554(14) 1 calc PR A 2 H45B H 0.0139 0.9449 0.7885 0.121 Uiso 0.554(14) 1 calc PR A 2 C46A C 0.0765(9) 0.8066(16) 0.7876(7) 0.104(6) Uiso 0.554(14) 1 d PDU A 2 H46A H 0.1229 0.8508 0.8108 0.125 Uiso 0.554(14) 1 calc PR A 2 H46B H 0.0737 0.7513 0.8154 0.125 Uiso 0.554(14) 1 calc PR A 2 C41B C 0.0859(9) 0.7293(10) 0.7674(5) 0.077(5) Uiso 0.446(14) 1 d PDU A 1 C42B C 0.0542(8) 0.7344(13) 0.6992(5) 0.071(4) Uiso 0.446(14) 1 d PDU A 1 H42C H 0.0714 0.6715 0.6837 0.085 Uiso 0.446(14) 1 calc PR A 1 H42D H 0.0792 0.7941 0.6869 0.085 Uiso 0.446(14) 1 calc PR A 1 C43B C -0.0398(8) 0.7441(19) 0.6693(8) 0.093(7) Uiso 0.446(14) 1 d PDU A 1 H43C H -0.0554 0.7729 0.6281 0.112 Uiso 0.446(14) 1 calc PR A 1 H43D H -0.0656 0.6757 0.6666 0.112 Uiso 0.446(14) 1 calc PR A 1 C44B C -0.0658(10) 0.8141(18) 0.7083(9) 0.120(7) Uiso 0.446(14) 1 d PDU A 1 H44C H -0.1112 0.8572 0.6822 0.143 Uiso 0.446(14) 1 calc PR A 1 H44D H -0.0863 0.7720 0.7343 0.143 Uiso 0.446(14) 1 calc PR A 1 C45B C -0.0006(10) 0.8826(13) 0.7471(11) 0.114(7) Uiso 0.446(14) 1 d PDU A 1 H45C H -0.0237 0.9232 0.7721 0.137 Uiso 0.446(14) 1 calc PR A 1 H45D H 0.0123 0.9319 0.7201 0.137 Uiso 0.446(14) 1 calc PR A 1 C46B C 0.0814(9) 0.8368(12) 0.7905(7) 0.071(5) Uiso 0.446(14) 1 d PDU A 1 H46C H 0.1274 0.8791 0.7897 0.085 Uiso 0.446(14) 1 calc PR A 1 H46D H 0.0827 0.8343 0.8324 0.085 Uiso 0.446(14) 1 calc PR A 1 C51 C 0.3441(4) 0.3175(5) 0.9209(3) 0.0783(17) Uani 1 1 d DU . . C52 C 0.3277(4) 0.2342(5) 0.9360(4) 0.0865(19) Uani 1 1 d DU . . Si61 Si 0.30042(12) 0.10624(16) 0.95556(10) 0.0862(8) Uani 1 1 d DU . . C62 C 0.3943(5) 0.0431(6) 1.0047(4) 0.120(3) Uani 1 1 d DU . . H62 H 0.4282 0.0299 0.9798 0.143 Uiso 1 1 calc R . . C63 C 0.3749(7) -0.0644(7) 1.0269(6) 0.167(5) Uani 1 1 d DU . . H63A H 0.3427 -0.1059 0.9920 0.251 Uiso 1 1 calc R . . H63B H 0.3442 -0.0540 1.0533 0.251 Uiso 1 1 calc R . . H63C H 0.4256 -0.1003 1.0492 0.251 Uiso 1 1 calc R . . C64 C 0.4468(7) 0.1102(7) 1.0611(5) 0.139(4) Uani 1 1 d DU . . H64A H 0.4539 0.1796 1.0475 0.208 Uiso 1 1 calc R . . H64B H 0.5000 0.0779 1.0806 0.208 Uiso 1 1 calc R . . H64C H 0.4191 0.1145 1.0898 0.208 Uiso 1 1 calc R . . C65 C 0.2131(7) 0.1281(9) 0.9762(7) 0.163(4) Uani 1 1 d DU . . H65 H 0.1738 0.1563 0.9375 0.195 Uiso 1 1 calc R . . C66 C 0.1661(9) 0.0341(11) 0.9848(8) 0.200(6) Uani 1 1 d DU . . H66A H 0.1596 -0.0156 0.9524 0.300 Uiso 1 1 calc R . . H66B H 0.1126 0.0560 0.9836 0.300 Uiso 1 1 calc R . . H66C H 0.1960 0.0020 1.0239 0.300 Uiso 1 1 calc R . . C67 C 0.2264(13) 0.2215(13) 1.0164(9) 0.244(8) Uani 1 1 d DU . . H67A H 0.2568 0.2735 1.0035 0.366 Uiso 1 1 calc R . . H67B H 0.2571 0.2017 1.0583 0.366 Uiso 1 1 calc R . . H67C H 0.1738 0.2500 1.0133 0.366 Uiso 1 1 calc R . . C68 C 0.2605(5) 0.0333(7) 0.8821(4) 0.118(3) Uani 1 1 d DU . . H68 H 0.2460 -0.0376 0.8910 0.141 Uiso 1 1 calc R . . C69 C 0.1804(6) 0.0855(9) 0.8361(5) 0.157(4) Uani 1 1 d DU . . H69A H 0.1402 0.0915 0.8552 0.235 Uiso 1 1 calc R . . H69B H 0.1585 0.0430 0.7997 0.235 Uiso 1 1 calc R . . H69C H 0.1934 0.1542 0.8251 0.235 Uiso 1 1 calc R . . C70 C 0.3261(7) 0.0227(10) 0.8529(6) 0.157(4) Uani 1 1 d DU . . H70A H 0.3755 -0.0074 0.8823 0.236 Uiso 1 1 calc R . . H70B H 0.3384 0.0908 0.8408 0.236 Uiso 1 1 calc R . . H70C H 0.3056 -0.0220 0.8174 0.236 Uiso 1 1 calc R . . C71 C 0.6236(5) 0.6671(6) 0.8235(3) 0.092(2) Uani 1 1 d DU . . C72 C 0.6308(6) 0.7202(7) 0.7847(4) 0.106(3) Uani 1 1 d DU B . Si81 Si 0.63734(19) 0.8000(2) 0.72207(12) 0.1168(10) Uani 1 1 d DU . . C82 C 0.6417(9) 0.7222(11) 0.6601(6) 0.168(4) Uani 1 1 d DU B . H82 H 0.6111 0.7697 0.6265 0.202 Uiso 1 1 calc R . . C83 C 0.5812(11) 0.6333(14) 0.6436(9) 0.248(8) Uani 1 1 d DU . . H83A H 0.5335 0.6524 0.6528 0.372 Uiso 1 1 calc R B . H83B H 0.6066 0.5721 0.6669 0.372 Uiso 1 1 calc R . . H83C H 0.5646 0.6184 0.6004 0.372 Uiso 1 1 calc R . . C84 C 0.7203(9) 0.7163(16) 0.6472(9) 0.238(8) Uani 1 1 d DU . . H84A H 0.7519 0.7792 0.6617 0.357 Uiso 1 1 calc R B . H84B H 0.7071 0.7094 0.6037 0.357 Uiso 1 1 calc R . . H84C H 0.7520 0.6565 0.6680 0.357 Uiso 1 1 calc R . . C85 C 0.5545(7) 0.8925(10) 0.7063(7) 0.163(4) Uani 1 1 d DU B . H85 H 0.5599 0.9412 0.6754 0.195 Uiso 1 1 calc R . . C86 C 0.4718(7) 0.8282(10) 0.6731(6) 0.173(5) Uani 1 1 d DU . . H86A H 0.4759 0.7905 0.6387 0.260 Uiso 1 1 calc R B . H86B H 0.4258 0.8759 0.6588 0.260 Uiso 1 1 calc R . . H86C H 0.4635 0.7794 0.7017 0.260 Uiso 1 1 calc R . . C87 C 0.5604(9) 0.9561(12) 0.7597(7) 0.197(6) Uani 1 1 d DU . . H87A H 0.6139 0.9888 0.7759 0.295 Uiso 1 1 calc R B . H87B H 0.5530 0.9121 0.7907 0.295 Uiso 1 1 calc R . . H87C H 0.5183 1.0093 0.7477 0.295 Uiso 1 1 calc R . . C88A C 0.7379(8) 0.8696(11) 0.7557(6) 0.200(6) Uiso 0.49(2) 1 d PDU B 1 H88A H 0.7416 0.8981 0.7957 0.240 Uiso 0.49(2) 1 calc PR B 1 C89A C 0.7399(9) 0.9627(11) 0.7143(6) 0.175(5) Uiso 0.49(2) 1 d PDU B 1 H89A H 0.6954 1.0101 0.7109 0.262 Uiso 0.49(2) 1 calc PR B 1 H89B H 0.7338 0.9373 0.6741 0.262 Uiso 0.49(2) 1 calc PR B 1 H89C H 0.7917 0.9990 0.7320 0.262 Uiso 0.49(2) 1 calc PR B 1 C90A C 0.802(2) 0.789(2) 0.7672(16) 0.225(17) Uiso 0.49(2) 1 d PDU B 1 H90A H 0.7949 0.7358 0.7941 0.338 Uiso 0.49(2) 1 calc PR B 1 H90B H 0.8559 0.8205 0.7862 0.338 Uiso 0.49(2) 1 calc PR B 1 H90C H 0.7985 0.7570 0.7289 0.338 Uiso 0.49(2) 1 calc PR B 1 C88B C 0.7379(8) 0.8696(11) 0.7557(6) 0.200(6) Uiso 0.51(2) 1 d PDU B 2 H88B H 0.7795 0.8201 0.7529 0.240 Uiso 0.51(2) 1 calc PR B 2 C89B C 0.7399(9) 0.9627(11) 0.7143(6) 0.175(5) Uiso 0.51(2) 1 d PDU B 2 H89D H 0.7165 0.9416 0.6719 0.262 Uiso 0.51(2) 1 calc PR B 2 H89E H 0.7960 0.9848 0.7239 0.262 Uiso 0.51(2) 1 calc PR B 2 H89F H 0.7083 1.0199 0.7212 0.262 Uiso 0.51(2) 1 calc PR B 2 C90B C 0.7675(12) 0.9026(14) 0.8235(6) 0.118(8) Uiso 0.51(2) 1 d PDU B 2 H90D H 0.7647 0.8435 0.8483 0.176 Uiso 0.51(2) 1 calc PR B 2 H90E H 0.7328 0.9580 0.8284 0.176 Uiso 0.51(2) 1 calc PR B 2 H90F H 0.8235 0.9272 0.8365 0.176 Uiso 0.51(2) 1 calc PR B 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 0.084(4) 0.062(3) 0.060(3) -0.013(3) 0.030(3) 0.002(3) C2 0.082(4) 0.072(4) 0.065(3) -0.012(3) 0.025(3) 0.002(3) C3 0.089(4) 0.077(4) 0.070(4) -0.014(3) 0.032(3) 0.012(3) C4 0.105(4) 0.070(4) 0.062(3) -0.002(3) 0.029(3) 0.016(3) C5 0.107(5) 0.072(4) 0.069(4) 0.005(3) 0.032(4) 0.005(3) C6 0.105(4) 0.065(4) 0.083(4) 0.002(3) 0.040(4) 0.004(3) C7 0.091(4) 0.077(4) 0.070(3) -0.009(3) 0.033(3) -0.014(3) C8 0.088(4) 0.090(5) 0.085(4) -0.001(3) 0.043(3) -0.006(3) C9 0.076(3) 0.082(4) 0.071(3) -0.013(3) 0.029(3) -0.001(3) C10 0.079(3) 0.061(3) 0.060(3) -0.017(3) 0.024(3) 0.002(3) C11 0.089(4) 0.059(3) 0.063(3) -0.007(3) 0.034(3) 0.009(3) C12 0.083(4) 0.060(3) 0.056(3) -0.005(3) 0.031(3) 0.000(3) C13 0.087(3) 0.045(3) 0.057(3) -0.017(2) 0.031(3) 0.001(2) C14 0.074(3) 0.055(3) 0.053(3) -0.019(2) 0.027(2) 0.003(2) C15 0.081(3) 0.056(3) 0.054(3) -0.009(2) 0.026(3) 0.005(2) C16 0.092(4) 0.066(4) 0.054(3) -0.015(3) 0.022(3) 0.000(3) C17 0.095(4) 0.064(3) 0.050(3) -0.013(3) 0.031(3) -0.004(3) C18 0.087(4) 0.065(4) 0.059(3) -0.007(3) 0.033(3) -0.001(3) C19 0.081(3) 0.054(3) 0.059(3) -0.013(2) 0.033(3) 0.001(3) C20 0.082(3) 0.057(3) 0.057(3) -0.015(2) 0.032(3) 0.004(3) C21 0.088(4) 0.089(5) 0.079(4) -0.016(4) 0.018(4) 0.019(4) O22 0.085(3) 0.139(5) 0.098(4) 0.011(3) 0.030(3) 0.026(3) N23 0.092(4) 0.082(4) 0.113(5) -0.015(3) -0.002(4) 0.018(3) C24 0.101(4) 0.080(4) 0.074(4) -0.007(4) 0.017(4) 0.024(4) O25 0.124(4) 0.093(4) 0.084(3) -0.002(3) 0.011(3) 0.021(3) C26 0.078(4) 0.097(5) 0.072(4) -0.011(3) 0.030(3) -0.002(3) O27 0.088(3) 0.131(5) 0.102(4) 0.012(3) 0.055(3) 0.009(3) N28 0.077(3) 0.106(4) 0.066(3) -0.005(3) 0.032(3) 0.010(3) C29 0.088(4) 0.070(4) 0.060(3) -0.007(3) 0.026(3) 0.009(3) O30 0.090(3) 0.077(3) 0.070(3) -0.008(2) 0.025(2) 0.011(2) C31 0.091(4) 0.133(6) 0.083(4) 0.005(4) 0.041(4) 0.017(4) C36 0.090(5) 0.182(8) 0.109(6) -0.014(6) 0.039(5) -0.005(5) C35 0.096(6) 0.203(10) 0.118(7) 0.011(7) 0.031(5) 0.008(6) C34 0.139(8) 0.211(12) 0.171(11) 0.039(9) 0.071(8) 0.054(7) C33 0.181(9) 0.143(8) 0.135(8) 0.046(6) 0.080(7) 0.071(6) C32 0.154(7) 0.123(6) 0.109(6) 0.024(5) 0.073(5) 0.055(5) C51 0.086(4) 0.061(3) 0.094(4) -0.014(3) 0.040(4) 0.003(3) C52 0.083(4) 0.074(4) 0.106(5) -0.004(4) 0.038(4) 0.020(3) Si61 0.0798(13) 0.0702(13) 0.1165(16) 0.0124(11) 0.0451(12) 0.0069(9) C62 0.117(5) 0.092(5) 0.128(6) -0.003(4) 0.020(4) 0.008(4) C63 0.179(9) 0.092(6) 0.162(9) 0.015(6) -0.019(7) 0.003(6) C64 0.144(8) 0.115(7) 0.127(7) -0.012(6) 0.014(6) 0.011(5) C65 0.157(7) 0.171(8) 0.199(8) -0.001(6) 0.110(6) 0.011(6) C66 0.177(10) 0.251(11) 0.230(13) 0.006(11) 0.142(10) -0.042(9) C67 0.282(15) 0.269(13) 0.271(15) -0.098(11) 0.209(13) -0.037(11) C68 0.117(5) 0.094(5) 0.128(5) -0.003(4) 0.029(4) -0.025(4) C69 0.143(7) 0.151(9) 0.135(7) 0.052(7) 0.002(6) -0.022(6) C70 0.183(8) 0.148(9) 0.144(8) -0.051(7) 0.064(7) -0.016(7) C71 0.103(5) 0.097(5) 0.086(4) 0.004(4) 0.046(4) -0.010(4) C72 0.116(6) 0.111(6) 0.099(5) 0.013(4) 0.050(5) -0.004(5) Si81 0.136(2) 0.127(2) 0.1010(16) 0.0352(15) 0.0604(16) 0.0059(16) C82 0.190(8) 0.180(8) 0.154(7) 0.004(6) 0.086(7) 0.009(6) C83 0.282(14) 0.222(13) 0.238(14) -0.074(11) 0.092(12) -0.053(11) C84 0.209(11) 0.286(16) 0.255(15) -0.013(12) 0.127(11) 0.066(10) C85 0.151(7) 0.161(7) 0.166(7) 0.019(6) 0.047(6) 0.009(5) C86 0.127(6) 0.183(10) 0.189(10) 0.050(8) 0.032(7) 0.002(7) C87 0.189(11) 0.184(11) 0.199(11) -0.006(8) 0.049(9) 0.063(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.402(9) . ? C1 C14 1.412(9) . ? C1 C51 1.444(9) . ? C2 C3 1.371(10) . ? C2 H2 0.9500 . ? C3 C16 1.398(10) . ? C3 C21 1.470(10) . ? C4 C5 1.379(11) . ? C4 C16 1.403(10) . ? C4 C24 1.461(11) . ? C5 C6 1.356(10) . ? C5 H5 0.9500 . ? C6 C17 1.382(9) . ? C6 H6 0.9500 . ? C7 C8 1.424(10) . ? C7 C71 1.430(9) . ? C7 C18 1.438(9) . ? C8 C9 1.346(10) . ? C8 H8 0.9500 . ? C9 C20 1.448(9) . ? C9 C26 1.479(10) . ? C10 C11 1.384(9) . ? C10 C20 1.390(9) . ? C10 C29 1.496(9) . ? C11 C12 1.388(8) . ? C11 H11 0.9500 . ? C12 C13 1.398(8) . ? C12 H12 0.9500 . ? C13 C19 1.437(9) . ? C13 C14 1.451(8) . ? C14 C15 1.465(9) . ? C15 C17 1.405(9) . ? C15 C16 1.439(9) . ? C17 C18 1.475(9) . ? C18 C19 1.411(9) . ? C19 C20 1.420(8) . ? C21 O22 1.205(10) . ? C21 N23 1.363(11) . ? N23 C24 1.413(12) . ? N23 C41B 1.553(17) . ? N23 C41A 1.562(16) . ? C24 O25 1.244(9) . ? C26 O27 1.226(8) . ? C26 N28 1.408(9) . ? N28 C29 1.392(9) . ? N28 C31 1.489(9) . ? C29 O30 1.212(8) . ? C31 C32 1.509(8) . ? C31 C36 1.515(8) . ? C36 C35 1.551(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C35 C34 1.479(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C34 C33 1.488(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C33 C32 1.564(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C41A C46A 1.504(9) . ? C41A C42A 1.515(9) . ? C42A C43A 1.561(10) . ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? C43A C44A 1.476(10) . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C44A C45A 1.478(10) . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C45A C46A 1.551(9) . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C41B C42B 1.512(9) . ? C41B C46B 1.513(9) . ? C42B C43B 1.560(10) . ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? C43B C44B 1.488(11) . ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? C44B C45B 1.483(11) . ? C44B H44C 0.9900 . ? C44B H44D 0.9900 . ? C45B C46B 1.561(10) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C51 C52 1.208(9) . ? C52 Si61 1.837(8) . ? Si61 C65 1.811(10) . ? Si61 C62 1.840(8) . ? Si61 C68 1.885(9) . ? C62 C63 1.575(11) . ? C62 C64 1.586(10) . ? C62 H62 1.0000 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C67 1.508(12) . ? C65 C66 1.533(12) . ? C65 H65 1.0000 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C70 1.563(11) . ? C68 C69 1.592(10) . ? C68 H68 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.196(9) . ? C72 Si81 1.854(8) . ? Si81 C82 1.812(11) . ? Si81 C85 1.827(11) . ? Si81 C88A 1.895(11) . ? C82 C83 1.526(12) . ? C82 C84 1.535(12) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C87 1.487(17) . ? C85 C86 1.620(16) . ? C85 H85 1.0000 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88A C90A 1.50(3) . ? C88A C89A 1.568(9) . ? C88A H88A 1.0000 . ? C89A H89A 0.9800 . ? C89A H89B 0.9800 . ? C89A H89C 0.9800 . ? C90A H90A 0.9800 . ? C90A H90B 0.9800 . ? C90A H90C 0.9800 . ? C90B H90D 0.9800 . ? C90B H90E 0.9800 . ? C90B H90F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C14 121.5(6) . . ? C2 C1 C51 114.1(6) . . ? C14 C1 C51 124.3(6) . . ? C3 C2 C1 122.3(7) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C16 119.1(6) . . ? C2 C3 C21 119.2(7) . . ? C16 C3 C21 121.7(7) . . ? C5 C4 C16 118.4(7) . . ? C5 C4 C24 121.1(7) . . ? C16 C4 C24 120.5(8) . . ? C6 C5 C4 121.1(7) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C17 123.1(8) . . ? C5 C6 H6 118.4 . . ? C17 C6 H6 118.4 . . ? C8 C7 C71 114.0(7) . . ? C8 C7 C18 120.0(6) . . ? C71 C7 C18 125.8(7) . . ? C9 C8 C7 120.8(7) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C20 120.7(6) . . ? C8 C9 C26 118.8(7) . . ? C20 C9 C26 120.3(6) . . ? C11 C10 C20 118.7(6) . . ? C11 C10 C29 120.0(6) . . ? C20 C10 C29 121.3(6) . . ? C10 C11 C12 121.4(6) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 121.1(6) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C19 118.7(6) . . ? C12 C13 C14 121.9(6) . . ? C19 C13 C14 119.4(5) . . ? C1 C14 C13 126.3(6) . . ? C1 C14 C15 116.5(5) . . ? C13 C14 C15 117.1(5) . . ? C17 C15 C16 118.8(6) . . ? C17 C15 C14 122.2(5) . . ? C16 C15 C14 119.0(6) . . ? C3 C16 C4 118.7(7) . . ? C3 C16 C15 121.0(6) . . ? C4 C16 C15 120.3(7) . . ? C6 C17 C15 118.1(6) . . ? C6 C17 C18 122.9(7) . . ? C15 C17 C18 119.0(6) . . ? C19 C18 C7 118.6(6) . . ? C19 C18 C17 118.3(6) . . ? C7 C18 C17 123.0(6) . . ? C18 C19 C20 119.9(6) . . ? C18 C19 C13 122.2(6) . . ? C20 C19 C13 117.9(6) . . ? C10 C20 C19 122.0(6) . . ? C10 C20 C9 118.8(6) . . ? C19 C20 C9 119.3(6) . . ? O22 C21 N23 120.2(7) . . ? O22 C21 C3 121.6(8) . . ? N23 C21 C3 118.0(8) . . ? C21 N23 C24 122.6(7) . . ? C21 N23 C41B 105.2(9) . . ? C24 N23 C41B 131.4(8) . . ? C21 N23 C41A 132.2(9) . . ? C24 N23 C41A 104.6(8) . . ? C41B N23 C41A 31.8(7) . . ? O25 C24 N23 120.6(7) . . ? O25 C24 C4 120.9(9) . . ? N23 C24 C4 118.4(7) . . ? O27 C26 N28 121.8(6) . . ? O27 C26 C9 120.4(7) . . ? N28 C26 C9 117.8(6) . . ? C29 N28 C26 122.8(6) . . ? C29 N28 C31 119.2(6) . . ? C26 N28 C31 117.8(6) . . ? O30 C29 N28 121.2(6) . . ? O30 C29 C10 120.7(7) . . ? N28 C29 C10 118.1(6) . . ? N28 C31 C32 112.6(6) . . ? N28 C31 C36 112.6(6) . . ? C32 C31 C36 112.7(8) . . ? C31 C36 C35 109.1(8) . . ? C31 C36 H36A 109.9 . . ? C35 C36 H36A 109.9 . . ? C31 C36 H36B 109.9 . . ? C35 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? C34 C35 C36 110.6(8) . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C34 C33 113.1(11) . . ? C35 C34 H34A 109.0 . . ? C33 C34 H34A 109.0 . . ? C35 C34 H34B 109.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C34 C33 C32 111.2(9) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C31 C32 C33 109.6(7) . . ? C31 C32 H32A 109.8 . . ? C33 C32 H32A 109.8 . . ? C31 C32 H32B 109.8 . . ? C33 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? C46A C41A C42A 110.5(13) . . ? C46A C41A N23 98.1(10) . . ? C42A C41A N23 115.5(10) . . ? C41A C42A C43A 100.9(10) . . ? C41A C42A H42A 111.6 . . ? C43A C42A H42A 111.6 . . ? C41A C42A H42B 111.6 . . ? C43A C42A H42B 111.6 . . ? H42A C42A H42B 109.4 . . ? C44A C43A C42A 126.4(12) . . ? C44A C43A H43A 105.7 . . ? C42A C43A H43A 105.7 . . ? C44A C43A H43B 105.7 . . ? C42A C43A H43B 105.7 . . ? H43A C43A H43B 106.2 . . ? C43A C44A C45A 117.3(13) . . ? C43A C44A H44A 108.0 . . ? C45A C44A H44A 108.0 . . ? C43A C44A H44B 108.0 . . ? C45A C44A H44B 108.0 . . ? H44A C44A H44B 107.2 . . ? C44A C45A C46A 104.9(11) . . ? C44A C45A H45A 110.8 . . ? C46A C45A H45A 110.8 . . ? C44A C45A H45B 110.8 . . ? C46A C45A H45B 110.8 . . ? H45A C45A H45B 108.8 . . ? C41A C46A C45A 124.1(12) . . ? C41A C46A H46A 106.3 . . ? C45A C46A H46A 106.3 . . ? C41A C46A H46B 106.3 . . ? C45A C46A H46B 106.3 . . ? H46A C46A H46B 106.4 . . ? C42B C41B C46B 107.6(11) . . ? C42B C41B N23 101.3(10) . . ? C46B C41B N23 112.1(10) . . ? C41B C42B C43B 114.2(11) . . ? C41B C42B H42C 108.7 . . ? C43B C42B H42C 108.7 . . ? C41B C42B H42D 108.7 . . ? C43B C42B H42D 108.7 . . ? H42C C42B H42D 107.6 . . ? C44B C43B C42B 106.7(12) . . ? C44B C43B H43C 110.4 . . ? C42B C43B H43C 110.4 . . ? C44B C43B H43D 110.4 . . ? C42B C43B H43D 110.4 . . ? H43C C43B H43D 108.6 . . ? C45B C44B C43B 114.0(15) . . ? C45B C44B H44C 108.8 . . ? C43B C44B H44C 108.8 . . ? C45B C44B H44D 108.8 . . ? C43B C44B H44D 108.8 . . ? H44C C44B H44D 107.7 . . ? C44B C45B C46B 120.6(13) . . ? C44B C45B H45C 107.2 . . ? C46B C45B H45C 107.2 . . ? C44B C45B H45D 107.2 . . ? C46B C45B H45D 107.2 . . ? H45C C45B H45D 106.8 . . ? C41B C46B C45B 105.8(11) . . ? C41B C46B H46C 110.6 . . ? C45B C46B H46C 110.6 . . ? C41B C46B H46D 110.6 . . ? C45B C46B H46D 110.6 . . ? H46C C46B H46D 108.7 . . ? C52 C51 C1 169.5(7) . . ? C51 C52 Si61 177.6(7) . . ? C65 Si61 C52 105.0(5) . . ? C65 Si61 C62 124.2(6) . . ? C52 Si61 C62 107.6(4) . . ? C65 Si61 C68 105.3(5) . . ? C52 Si61 C68 105.3(4) . . ? C62 Si61 C68 108.1(4) . . ? C63 C62 C64 109.6(8) . . ? C63 C62 Si61 110.5(6) . . ? C64 C62 Si61 114.1(6) . . ? C63 C62 H62 107.4 . . ? C64 C62 H62 107.4 . . ? Si61 C62 H62 107.4 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C67 C65 C66 121.5(10) . . ? C67 C65 Si61 110.3(9) . . ? C66 C65 Si61 118.2(9) . . ? C67 C65 H65 100.6 . . ? C66 C65 H65 100.6 . . ? Si61 C65 H65 100.6 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C70 C68 C69 110.8(8) . . ? C70 C68 Si61 111.6(6) . . ? C69 C68 Si61 111.2(7) . . ? C70 C68 H68 107.7 . . ? C69 C68 H68 107.7 . . ? Si61 C68 H68 107.7 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 C7 171.3(9) . . ? C71 C72 Si81 177.2(9) . . ? C82 Si81 C85 118.0(7) . . ? C82 Si81 C72 112.1(6) . . ? C85 Si81 C72 104.5(6) . . ? C82 Si81 C88A 107.2(7) . . ? C85 Si81 C88A 109.6(7) . . ? C72 Si81 C88A 104.7(5) . . ? C83 C82 C84 121.0(11) . . ? C83 C82 Si81 113.4(10) . . ? C84 C82 Si81 120.2(11) . . ? C83 C82 H82 97.8 . . ? C84 C82 H82 97.8 . . ? Si81 C82 H82 97.8 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C87 C85 C86 118.1(12) . . ? C87 C85 Si81 112.9(9) . . ? C86 C85 Si81 106.2(8) . . ? C87 C85 H85 106.3 . . ? C86 C85 H85 106.3 . . ? Si81 C85 H85 106.3 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C90A C88A C89A 117.6(17) . . ? C90A C88A Si81 106.2(17) . . ? C89A C88A Si81 109.7(9) . . ? C90A C88A H88A 107.7 . . ? C89A C88A H88A 107.7 . . ? Si81 C88A H88A 107.7 . . ? C88A C89A H89A 109.5 . . ? C88A C89A H89B 109.5 . . ? H89A C89A H89B 109.5 . . ? C88A C89A H89C 109.5 . . ? H89A C89A H89C 109.5 . . ? H89B C89A H89C 109.5 . . ? C88A C90A H90A 109.5 . . ? C88A C90A H90B 109.5 . . ? H90A C90A H90B 109.5 . . ? C88A C90A H90C 109.5 . . ? H90A C90A H90C 109.5 . . ? H90B C90A H90C 109.5 . . ? H90D C90B H90E 109.5 . . ? H90D C90B H90F 109.5 . . ? H90E C90B H90F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.067 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 931601' ####################################################################### # # 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_BWNRCA #TrackingRef 'web_deposit_cif_file_0_NeilChampness_1364485153.Champness.cif' _nottingham_internal_coll_name BWNRCA _nottingham_internal_coll_number 11066 _nottingham_internal_coll_client BW/NRC _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_time 50 _nottingham_internal_coll_frame_width 1.0 _nottingham_internal_coll_frame_method omega _nottingham_internal_coll_user 'Dr Peter N. Horton, NCS' _nottingham_internal_coll_date 19/01/2012 _nottingham_internal_coll_location SOTON _nottingham_internal_NCS_number ? _nottingham_internal_process_user 'Dr Peter N. Horton, NCS' _nottingham_internal_process_date 19/01/2012 _nottingham_internal_solution_user 'Dr Peter N. Horton, NCS' _nottingham_internal_solution_date 19/01/2012 _nottingham_internal_refinement_user SPA/AGS _nottingham_internal_refinement_date 12/04/2012 _nottingham_internal_validation_user ? _nottingham_internal_validation_date ? _nottingham_internal_archive_date ? _refine_special_details ; All hydrogen atoms were observed in the electron density map before being geometrically placed and refined using a riding model. ; _audit_creation_date 2012-04-30 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H28 Br2 N2 O4' _chemical_formula_sum 'C36 H28 Br2 N2 O4' _chemical_formula_weight 712.42 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 15.2582(4) _cell_length_b 11.8210(3) _cell_length_c 16.0098(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.389(7) _cell_angle_gamma 90.00 _cell_volume 2809.2(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 29332 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.1 _exptl_absorpt_coefficient_mu 2.933 _exptl_absorpt_correction_T_max 0.9172 _exptl_absorpt_correction_T_min 0.6674 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1440 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 33301 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 3.13 _diffrn_ambient_temperature 100.15 _diffrn_detector CCD _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support Mitegen _diffrn_radiation_monochromator Confocal _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.710747 _diffrn_source 'Rotating Anode' _diffrn_source_current 55.0 _diffrn_source_power 2.475 _diffrn_source_voltage 45.0 _reflns_number_gt 6112 _reflns_number_total 6431 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_data_collection ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.376 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 397 _refine_ls_number_reflns 6431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0223 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+2.6150P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.0555 _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.19571(10) 1.00677(13) 0.06777(10) 0.0144(3) Uani 1 1 d . . . C2 C 0.13855(10) 1.09890(13) 0.06924(10) 0.0147(3) Uani 1 1 d . . . H2 H 0.0754 1.0908 0.0477 0.018 Uiso 1 1 calc R . . C3 C 0.17353(10) 1.20078(13) 0.10175(9) 0.0134(3) Uani 1 1 d . . . C4 C 0.30275(10) 1.32078(13) 0.15843(9) 0.0138(3) Uani 1 1 d . . . C5 C 0.39431(10) 1.33654(13) 0.17957(10) 0.0146(3) Uani 1 1 d . . . H5 H 0.4185 1.4066 0.2035 0.018 Uiso 1 1 calc R . . C6 C 0.45226(10) 1.25023(13) 0.16618(10) 0.0153(3) Uani 1 1 d . . . H6 H 0.5153 1.2643 0.1792 0.018 Uiso 1 1 calc R . . C7 C 0.56873(10) 1.06144(13) 0.10986(10) 0.0149(3) Uani 1 1 d . . . C8 C 0.62264(10) 0.96752(14) 0.10364(10) 0.0158(3) Uani 1 1 d . . . H8 H 0.6818 0.9784 0.0956 0.019 Uiso 1 1 calc R . . C9 C 0.59091(10) 0.86018(13) 0.10901(10) 0.0151(3) Uani 1 1 d . . . C10 C 0.47091(10) 0.73456(13) 0.12767(10) 0.0148(3) Uani 1 1 d . . . C11 C 0.38550(10) 0.71871(13) 0.14004(10) 0.0157(3) Uani 1 1 d . . . H11 H 0.3670 0.6459 0.1543 0.019 Uiso 1 1 calc R . . C12 C 0.32610(10) 0.80999(13) 0.13151(10) 0.0154(3) Uani 1 1 d . . . H12 H 0.2665 0.7976 0.1379 0.018 Uiso 1 1 calc R . . C13 C 0.35194(10) 0.91877(13) 0.11389(9) 0.0132(3) Uani 1 1 d . . . C14 C 0.28897(10) 1.01398(13) 0.09793(9) 0.0132(3) Uani 1 1 d . . . C15 C 0.32598(10) 1.12448(12) 0.11837(9) 0.0126(3) Uani 1 1 d . . . C16 C 0.26769(10) 1.21539(13) 0.12591(9) 0.0128(3) Uani 1 1 d . . . C17 C 0.42095(10) 1.14445(13) 0.13449(9) 0.0132(3) Uani 1 1 d . . . C18 C 0.48006(10) 1.05212(13) 0.11875(9) 0.0131(3) Uani 1 1 d . . . C19 C 0.44457(10) 0.93913(13) 0.11566(9) 0.0135(3) Uani 1 1 d . . . C20 C 0.50144(10) 0.84447(13) 0.11631(9) 0.0139(3) Uani 1 1 d . . . C21 C 0.11136(10) 1.29384(13) 0.11078(9) 0.0139(3) Uani 1 1 d . . . O22 O 0.03036(7) 1.28344(10) 0.08616(7) 0.0178(2) Uani 1 1 d . . . N23 N 0.14982(9) 1.39372(11) 0.15008(8) 0.0148(3) Uani 1 1 d . . . C24 C 0.24244(10) 1.41443(13) 0.17066(10) 0.0144(3) Uani 1 1 d . . . O25 O 0.27213(7) 1.50637(9) 0.19809(7) 0.0186(2) Uani 1 1 d . . . C26 C 0.65179(10) 0.76280(14) 0.10755(10) 0.0172(3) Uani 1 1 d . . . O27 O 0.72823(8) 0.77573(10) 0.09932(9) 0.0239(3) Uani 1 1 d . . . N28 N 0.61712(9) 0.65531(11) 0.11618(9) 0.0161(3) Uani 1 1 d . . . C29 C 0.53139(10) 0.63619(13) 0.13095(10) 0.0172(3) Uani 1 1 d . . . O30 O 0.50780(8) 0.54162(10) 0.14580(10) 0.0291(3) Uani 1 1 d . . . Br31 Br 0.134393(10) 0.874842(13) 0.017145(11) 0.01947(5) Uani 1 1 d . . . Br32 Br 0.628789(10) 1.199474(13) 0.100227(11) 0.01900(5) Uani 1 1 d . . . C41 C 0.08638(10) 1.48166(13) 0.16808(10) 0.0157(3) Uani 1 1 d . . . H41 H 0.0252 1.4461 0.1543 0.019 Uiso 1 1 calc R . . C42 C 0.08025(11) 1.58479(14) 0.10966(11) 0.0192(3) Uani 1 1 d . . . H42A H 0.0666 1.5602 0.0489 0.023 Uiso 1 1 calc R . . H42B H 0.1387 1.6251 0.1220 0.023 Uiso 1 1 calc R . . C43 C 0.00601(11) 1.66454(14) 0.12454(11) 0.0215(3) Uani 1 1 d . . . H43A H 0.0057 1.7340 0.0900 0.026 Uiso 1 1 calc R . . H43B H -0.0533 1.6272 0.1051 0.026 Uiso 1 1 calc R . . C44 C 0.02007(13) 1.69636(15) 0.21894(12) 0.0267(4) Uani 1 1 d . . . H44A H -0.0315 1.7425 0.2269 0.032 Uiso 1 1 calc R . . H44B H 0.0753 1.7429 0.2363 0.032 Uiso 1 1 calc R . . C45 C 0.02886(12) 1.59186(16) 0.27600(11) 0.0245(4) Uani 1 1 d . . . H45A H -0.0286 1.5494 0.2627 0.029 Uiso 1 1 calc R . . H45B H 0.0409 1.6156 0.3369 0.029 Uiso 1 1 calc R . . C46 C 0.10508(11) 1.51483(15) 0.26269(10) 0.0205(3) Uani 1 1 d . . . H46A H 0.1635 1.5550 0.2794 0.025 Uiso 1 1 calc R . . H46B H 0.1083 1.4463 0.2988 0.025 Uiso 1 1 calc R . . C51 C 0.67401(10) 0.55371(13) 0.11395(10) 0.0155(3) Uani 1 1 d . . . H51 H 0.6353 0.4869 0.1187 0.019 Uiso 1 1 calc R . . C52 C 0.70224(11) 0.53991(14) 0.02932(10) 0.0186(3) Uani 1 1 d . . . H52A H 0.7445 0.6011 0.0228 0.022 Uiso 1 1 calc R . . H52B H 0.6487 0.5447 -0.0192 0.022 Uiso 1 1 calc R . . C53 C 0.74771(11) 0.42523(14) 0.02890(10) 0.0191(3) Uani 1 1 d . . . H53A H 0.7025 0.3648 0.0277 0.023 Uiso 1 1 calc R . . H53B H 0.7705 0.4185 -0.0239 0.023 Uiso 1 1 calc R . . C54 C 0.82534(11) 0.40787(15) 0.10657(11) 0.0224(3) Uani 1 1 d . . . H54A H 0.8754 0.4592 0.1023 0.027 Uiso 1 1 calc R . . H54B H 0.8475 0.3291 0.1066 0.027 Uiso 1 1 calc R . . C55 C 0.79787(11) 0.43053(14) 0.19083(11) 0.0209(3) Uani 1 1 d . . . H55A H 0.8517 0.4262 0.2391 0.025 Uiso 1 1 calc R . . H55B H 0.7548 0.3717 0.1998 0.025 Uiso 1 1 calc R . . C56 C 0.75438(11) 0.54692(14) 0.19035(10) 0.0187(3) Uani 1 1 d . . . H56A H 0.7344 0.5585 0.2443 0.022 Uiso 1 1 calc R . . H56B H 0.7986 0.6067 0.1860 0.022 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0143(7) 0.0132(7) 0.0150(7) -0.0024(6) 0.0021(6) -0.0035(6) C2 0.0125(6) 0.0172(7) 0.0138(7) -0.0002(6) 0.0018(5) -0.0022(6) C3 0.0140(7) 0.0149(7) 0.0110(7) 0.0010(5) 0.0022(5) -0.0005(5) C4 0.0155(7) 0.0137(7) 0.0118(7) 0.0014(5) 0.0027(5) -0.0014(6) C5 0.0163(7) 0.0133(7) 0.0134(7) 0.0002(6) 0.0018(6) -0.0040(6) C6 0.0139(7) 0.0161(7) 0.0151(7) 0.0021(6) 0.0018(6) -0.0029(6) C7 0.0155(7) 0.0137(7) 0.0147(7) 0.0016(6) 0.0016(6) -0.0038(6) C8 0.0124(6) 0.0198(8) 0.0151(7) 0.0017(6) 0.0029(6) -0.0015(6) C9 0.0138(7) 0.0162(7) 0.0143(7) 0.0019(6) 0.0016(5) -0.0008(6) C10 0.0136(7) 0.0149(7) 0.0151(7) 0.0018(6) 0.0019(5) -0.0004(6) C11 0.0157(7) 0.0136(7) 0.0173(7) 0.0007(6) 0.0027(6) -0.0032(6) C12 0.0130(7) 0.0166(7) 0.0163(7) 0.0002(6) 0.0030(6) -0.0031(6) C13 0.0130(7) 0.0142(7) 0.0119(7) -0.0007(5) 0.0017(5) -0.0019(6) C14 0.0137(7) 0.0141(7) 0.0118(7) -0.0003(5) 0.0030(5) -0.0019(6) C15 0.0133(7) 0.0140(7) 0.0103(6) 0.0017(5) 0.0023(5) -0.0015(5) C16 0.0146(7) 0.0139(7) 0.0096(6) 0.0012(5) 0.0022(5) -0.0013(6) C17 0.0131(7) 0.0147(7) 0.0113(7) 0.0017(5) 0.0018(5) -0.0016(5) C18 0.0130(7) 0.0149(7) 0.0103(6) 0.0012(5) 0.0005(5) -0.0019(5) C19 0.0138(7) 0.0147(7) 0.0113(7) 0.0007(5) 0.0014(5) -0.0021(6) C20 0.0130(7) 0.0158(7) 0.0122(7) 0.0006(6) 0.0012(5) -0.0015(6) C21 0.0163(7) 0.0137(7) 0.0119(7) 0.0015(5) 0.0038(5) -0.0017(6) O22 0.0134(5) 0.0179(5) 0.0213(6) -0.0028(4) 0.0022(4) -0.0009(4) N23 0.0148(6) 0.0136(6) 0.0158(6) -0.0011(5) 0.0030(5) -0.0008(5) C24 0.0166(7) 0.0140(7) 0.0124(7) 0.0018(6) 0.0031(5) -0.0018(6) O25 0.0182(5) 0.0143(5) 0.0231(6) -0.0027(4) 0.0042(5) -0.0028(4) C26 0.0158(7) 0.0158(7) 0.0197(8) 0.0024(6) 0.0034(6) -0.0011(6) O27 0.0145(5) 0.0188(6) 0.0402(7) 0.0030(5) 0.0099(5) -0.0006(5) N28 0.0141(6) 0.0135(6) 0.0212(7) 0.0024(5) 0.0051(5) 0.0004(5) C29 0.0159(7) 0.0155(7) 0.0205(8) 0.0015(6) 0.0047(6) -0.0003(6) O30 0.0226(6) 0.0149(6) 0.0545(9) 0.0065(6) 0.0184(6) 0.0008(5) Br31 0.01437(8) 0.01515(8) 0.02604(9) -0.00584(6) -0.00117(6) -0.00262(5) Br32 0.01791(8) 0.01500(8) 0.02599(9) -0.00037(6) 0.00894(6) -0.00567(6) C41 0.0150(7) 0.0146(7) 0.0179(7) -0.0016(6) 0.0044(6) 0.0005(6) C42 0.0212(8) 0.0184(8) 0.0185(8) 0.0017(6) 0.0059(6) 0.0025(6) C43 0.0221(8) 0.0173(8) 0.0260(9) 0.0020(7) 0.0074(7) 0.0028(6) C44 0.0317(9) 0.0192(8) 0.0307(10) -0.0055(7) 0.0102(8) 0.0030(7) C45 0.0279(9) 0.0280(9) 0.0192(8) -0.0033(7) 0.0088(7) 0.0029(7) C46 0.0224(8) 0.0221(8) 0.0174(8) -0.0004(6) 0.0052(6) 0.0018(7) C51 0.0157(7) 0.0143(7) 0.0169(7) 0.0007(6) 0.0042(6) 0.0020(6) C52 0.0205(7) 0.0209(8) 0.0146(7) 0.0011(6) 0.0042(6) -0.0015(6) C53 0.0226(8) 0.0185(8) 0.0180(8) -0.0040(6) 0.0088(6) -0.0046(6) C54 0.0189(8) 0.0188(8) 0.0298(9) -0.0040(7) 0.0059(7) 0.0022(6) C55 0.0221(8) 0.0178(8) 0.0200(8) -0.0012(6) -0.0007(6) 0.0039(6) C56 0.0224(8) 0.0177(8) 0.0146(7) -0.0016(6) 0.0011(6) 0.0036(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 C1 C2 1.399(2) . ? C1 C14 1.395(2) . ? C1 Br31 1.9008(15) . ? C2 H2 0.9500 . ? C2 C3 1.370(2) . ? C3 C16 1.409(2) . ? C3 C21 1.481(2) . ? C4 C5 1.372(2) . ? C4 C16 1.407(2) . ? C4 C24 1.481(2) . ? C5 H5 0.9500 . ? C5 C6 1.399(2) . ? C6 H6 0.9500 . ? C6 C17 1.392(2) . ? C7 C8 1.399(2) . ? C7 C18 1.397(2) . ? C7 Br32 1.8951(15) . ? C8 H8 0.9500 . ? C8 C9 1.368(2) . ? C9 C20 1.409(2) . ? C9 C26 1.483(2) . ? C10 C11 1.376(2) . ? C10 C20 1.406(2) . ? C10 C29 1.478(2) . ? C11 H11 0.9500 . ? C11 C12 1.395(2) . ? C12 H12 0.9500 . ? C12 C13 1.393(2) . ? C13 C14 1.463(2) . ? C13 C19 1.427(2) . ? C14 C15 1.431(2) . ? C15 C16 1.418(2) . ? C15 C17 1.432(2) . ? C17 C18 1.474(2) . ? C18 C19 1.438(2) . ? C19 C20 1.415(2) . ? C21 O22 1.2134(19) . ? C21 N23 1.4012(19) . ? N23 C24 1.3965(19) . ? N23 C41 1.4933(19) . ? C24 O25 1.2194(19) . ? C26 O27 1.2132(19) . ? C26 N28 1.396(2) . ? N28 C29 1.4005(19) . ? N28 C51 1.4871(19) . ? C29 O30 1.215(2) . ? C41 H41 1.0000 . ? C41 C42 1.526(2) . ? C41 C46 1.526(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 C43 1.534(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.524(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.524(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.530(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C51 H51 1.0000 . ? C51 C52 1.523(2) . ? C51 C56 1.520(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52 C53 1.523(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C53 C54 1.520(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54 C55 1.526(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C55 C56 1.527(2) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Br31 113.50(11) . . ? C14 C1 C2 122.44(14) . . ? C14 C1 Br31 124.02(11) . . ? C1 C2 H2 120.0 . . ? C3 C2 C1 120.08(14) . . ? C3 C2 H2 120.0 . . ? C2 C3 C16 119.65(14) . . ? C2 C3 C21 119.20(13) . . ? C16 C3 C21 121.16(13) . . ? C5 C4 C16 119.32(14) . . ? C5 C4 C24 119.62(14) . . ? C16 C4 C24 121.07(13) . . ? C4 C5 H5 119.8 . . ? C4 C5 C6 120.46(14) . . ? C6 C5 H5 119.8 . . ? C5 C6 H6 118.8 . . ? C17 C6 C5 122.37(14) . . ? C17 C6 H6 118.8 . . ? C8 C7 Br32 111.97(11) . . ? C18 C7 C8 122.94(14) . . ? C18 C7 Br32 125.04(12) . . ? C7 C8 H8 119.7 . . ? C9 C8 C7 120.62(14) . . ? C9 C8 H8 119.7 . . ? C8 C9 C20 119.42(14) . . ? C8 C9 C26 119.15(14) . . ? C20 C9 C26 121.43(14) . . ? C11 C10 C20 119.85(14) . . ? C11 C10 C29 119.49(14) . . ? C20 C10 C29 120.58(13) . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.74(14) . . ? C12 C11 H11 120.1 . . ? C11 C12 H12 119.1 . . ? C13 C12 C11 121.72(14) . . ? C13 C12 H12 119.1 . . ? C12 C13 C14 122.69(13) . . ? C12 C13 C19 118.49(14) . . ? C19 C13 C14 118.74(13) . . ? C1 C14 C13 126.10(14) . . ? C1 C14 C15 116.86(14) . . ? C15 C14 C13 117.00(13) . . ? C14 C15 C17 121.42(13) . . ? C16 C15 C14 119.30(13) . . ? C16 C15 C17 119.24(13) . . ? C3 C16 C15 120.23(14) . . ? C4 C16 C3 119.08(14) . . ? C4 C16 C15 120.69(13) . . ? C6 C17 C15 117.49(14) . . ? C6 C17 C18 123.75(13) . . ? C15 C17 C18 118.74(13) . . ? C7 C18 C17 127.17(14) . . ? C7 C18 C19 115.83(14) . . ? C19 C18 C17 116.95(13) . . ? C13 C19 C18 121.37(14) . . ? C20 C19 C13 118.01(14) . . ? C20 C19 C18 120.60(13) . . ? C9 C20 C19 119.97(14) . . ? C10 C20 C9 119.26(14) . . ? C10 C20 C19 120.71(13) . . ? O22 C21 C3 121.34(14) . . ? O22 C21 N23 121.36(14) . . ? N23 C21 C3 117.29(13) . . ? C21 N23 C41 116.77(12) . . ? C24 N23 C21 123.33(13) . . ? C24 N23 C41 119.88(12) . . ? N23 C24 C4 117.61(13) . . ? O25 C24 C4 121.56(14) . . ? O25 C24 N23 120.82(14) . . ? O27 C26 C9 121.70(15) . . ? O27 C26 N28 121.42(15) . . ? N28 C26 C9 116.88(13) . . ? C26 N28 C29 123.64(13) . . ? C26 N28 C51 119.75(12) . . ? C29 N28 C51 116.55(13) . . ? N28 C29 C10 117.84(13) . . ? O30 C29 C10 121.35(14) . . ? O30 C29 N28 120.82(14) . . ? N23 C41 H41 106.1 . . ? N23 C41 C42 112.85(12) . . ? N23 C41 C46 112.94(13) . . ? C42 C41 H41 106.1 . . ? C42 C41 C46 111.96(13) . . ? C46 C41 H41 106.1 . . ? C41 C42 H42A 109.7 . . ? C41 C42 H42B 109.7 . . ? C41 C42 C43 109.78(13) . . ? H42A C42 H42B 108.2 . . ? C43 C42 H42A 109.7 . . ? C43 C42 H42B 109.7 . . ? C42 C43 H43A 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C44 C43 C42 111.49(14) . . ? C44 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C43 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? C43 C44 C45 111.54(14) . . ? H44A C44 H44B 108.0 . . ? C45 C44 H44A 109.3 . . ? C45 C44 H44B 109.3 . . ? C44 C45 H45A 109.4 . . ? C44 C45 H45B 109.4 . . ? C44 C45 C46 111.29(14) . . ? H45A C45 H45B 108.0 . . ? C46 C45 H45A 109.4 . . ? C46 C45 H45B 109.4 . . ? C41 C46 C45 108.52(13) . . ? C41 C46 H46A 110.0 . . ? C41 C46 H46B 110.0 . . ? C45 C46 H46A 110.0 . . ? C45 C46 H46B 110.0 . . ? H46A C46 H46B 108.4 . . ? N28 C51 H51 106.1 . . ? N28 C51 C52 113.26(13) . . ? N28 C51 C56 112.94(13) . . ? C52 C51 H51 106.1 . . ? C56 C51 H51 106.1 . . ? C56 C51 C52 111.63(13) . . ? C51 C52 H52A 109.9 . . ? C51 C52 H52B 109.9 . . ? C51 C52 C53 108.80(13) . . ? H52A C52 H52B 108.3 . . ? C53 C52 H52A 109.9 . . ? C53 C52 H52B 109.9 . . ? C52 C53 H53A 109.1 . . ? C52 C53 H53B 109.1 . . ? H53A C53 H53B 107.8 . . ? C54 C53 C52 112.70(13) . . ? C54 C53 H53A 109.1 . . ? C54 C53 H53B 109.1 . . ? C53 C54 H54A 109.2 . . ? C53 C54 H54B 109.2 . . ? C53 C54 C55 112.21(13) . . ? H54A C54 H54B 107.9 . . ? C55 C54 H54A 109.2 . . ? C55 C54 H54B 109.2 . . ? C54 C55 H55A 109.4 . . ? C54 C55 H55B 109.4 . . ? C54 C55 C56 111.20(14) . . ? H55A C55 H55B 108.0 . . ? C56 C55 H55A 109.4 . . ? C56 C55 H55B 109.4 . . ? C51 C56 C55 108.68(13) . . ? C51 C56 H56A 110.0 . . ? C51 C56 H56B 110.0 . . ? C55 C56 H56A 110.0 . . ? C55 C56 H56B 110.0 . . ? H56A C56 H56B 108.3 . . ? 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 C1 C2 C3 C16 6.1(2) . . . . ? C1 C2 C3 C21 -173.91(14) . . . . ? C1 C14 C15 C16 14.0(2) . . . . ? C1 C14 C15 C17 -168.34(14) . . . . ? C2 C1 C14 C13 167.80(14) . . . . ? C2 C1 C14 C15 -9.5(2) . . . . ? C2 C3 C16 C4 179.39(14) . . . . ? C2 C3 C16 C15 -1.3(2) . . . . ? C2 C3 C21 O22 -3.6(2) . . . . ? C2 C3 C21 N23 175.44(13) . . . . ? C3 C21 N23 C24 8.4(2) . . . . ? C3 C21 N23 C41 -173.08(13) . . . . ? C4 C5 C6 C17 -2.5(2) . . . . ? C5 C4 C16 C3 -178.01(14) . . . . ? C5 C4 C16 C15 2.7(2) . . . . ? C5 C4 C24 N23 -178.59(14) . . . . ? C5 C4 C24 O25 1.0(2) . . . . ? C5 C6 C17 C15 -2.2(2) . . . . ? C5 C6 C17 C18 179.30(14) . . . . ? C6 C17 C18 C7 -18.6(2) . . . . ? C6 C17 C18 C19 158.61(14) . . . . ? C7 C8 C9 C20 3.4(2) . . . . ? C7 C8 C9 C26 -176.25(14) . . . . ? C7 C18 C19 C13 -172.61(14) . . . . ? C7 C18 C19 C20 8.9(2) . . . . ? C8 C7 C18 C17 173.34(14) . . . . ? C8 C7 C18 C19 -3.9(2) . . . . ? C8 C9 C20 C10 -175.72(14) . . . . ? C8 C9 C20 C19 1.7(2) . . . . ? C8 C9 C26 O27 -2.1(2) . . . . ? C8 C9 C26 N28 177.86(14) . . . . ? C9 C26 N28 C29 -3.9(2) . . . . ? C9 C26 N28 C51 179.08(13) . . . . ? C10 C11 C12 C13 -2.5(2) . . . . ? C11 C10 C20 C9 176.11(14) . . . . ? C11 C10 C20 C19 -1.3(2) . . . . ? C11 C10 C29 N28 178.63(14) . . . . ? C11 C10 C29 O30 -1.3(2) . . . . ? C11 C12 C13 C14 175.01(14) . . . . ? C11 C12 C13 C19 -8.1(2) . . . . ? C12 C13 C14 C1 -24.6(2) . . . . ? C12 C13 C14 C15 152.75(14) . . . . ? C12 C13 C19 C18 -164.85(14) . . . . ? C12 C13 C19 C20 13.7(2) . . . . ? C13 C14 C15 C16 -163.59(13) . . . . ? C13 C14 C15 C17 14.1(2) . . . . ? C13 C19 C20 C9 173.38(14) . . . . ? C13 C19 C20 C10 -9.2(2) . . . . ? C14 C1 C2 C3 -0.5(2) . . . . ? C14 C13 C19 C18 12.1(2) . . . . ? C14 C13 C19 C20 -169.32(13) . . . . ? C14 C15 C16 C3 -8.9(2) . . . . ? C14 C15 C16 C4 170.33(13) . . . . ? C14 C15 C17 C6 -170.72(14) . . . . ? C14 C15 C17 C18 7.9(2) . . . . ? C15 C17 C18 C7 162.92(15) . . . . ? C15 C17 C18 C19 -19.9(2) . . . . ? C16 C3 C21 O22 176.33(14) . . . . ? C16 C3 C21 N23 -4.6(2) . . . . ? C16 C4 C5 C6 2.2(2) . . . . ? C16 C4 C24 N23 1.0(2) . . . . ? C16 C4 C24 O25 -179.36(14) . . . . ? C16 C15 C17 C6 7.0(2) . . . . ? C16 C15 C17 C18 -174.43(13) . . . . ? C17 C15 C16 C3 173.36(13) . . . . ? C17 C15 C16 C4 -7.4(2) . . . . ? C17 C18 C19 C13 9.9(2) . . . . ? C17 C18 C19 C20 -168.63(13) . . . . ? C18 C7 C8 C9 -2.2(2) . . . . ? C18 C19 C20 C9 -8.0(2) . . . . ? C18 C19 C20 C10 169.36(14) . . . . ? C19 C13 C14 C1 158.58(15) . . . . ? C19 C13 C14 C15 -24.1(2) . . . . ? C20 C9 C26 O27 178.29(16) . . . . ? C20 C9 C26 N28 -1.8(2) . . . . ? C20 C10 C11 C12 7.3(2) . . . . ? C20 C10 C29 N28 -4.5(2) . . . . ? C20 C10 C29 O30 175.57(16) . . . . ? C21 C3 C16 C4 -0.6(2) . . . . ? C21 C3 C16 C15 178.70(13) . . . . ? C21 N23 C24 C4 -6.7(2) . . . . ? C21 N23 C24 O25 173.71(14) . . . . ? C21 N23 C41 C42 -108.65(15) . . . . ? C21 N23 C41 C46 123.11(14) . . . . ? O22 C21 N23 C24 -172.57(14) . . . . ? O22 C21 N23 C41 6.0(2) . . . . ? N23 C41 C42 C43 173.32(13) . . . . ? N23 C41 C46 C45 -172.03(13) . . . . ? C24 C4 C5 C6 -178.16(14) . . . . ? C24 C4 C16 C3 2.4(2) . . . . ? C24 C4 C16 C15 -176.88(13) . . . . ? C24 N23 C41 C42 69.96(18) . . . . ? C24 N23 C41 C46 -58.28(18) . . . . ? C26 C9 C20 C10 3.9(2) . . . . ? C26 C9 C20 C19 -178.66(14) . . . . ? C26 N28 C29 C10 7.0(2) . . . . ? C26 N28 C29 O30 -173.17(16) . . . . ? C26 N28 C51 C52 -61.68(19) . . . . ? C26 N28 C51 C56 66.46(18) . . . . ? O27 C26 N28 C29 176.06(16) . . . . ? O27 C26 N28 C51 -1.0(2) . . . . ? N28 C51 C52 C53 -171.58(13) . . . . ? N28 C51 C56 C55 169.66(13) . . . . ? C29 C10 C11 C12 -175.86(14) . . . . ? C29 C10 C20 C9 -0.7(2) . . . . ? C29 C10 C20 C19 -178.13(14) . . . . ? C29 N28 C51 C52 121.07(15) . . . . ? C29 N28 C51 C56 -110.78(16) . . . . ? Br31 C1 C2 C3 -178.24(11) . . . . ? Br31 C1 C14 C13 -14.7(2) . . . . ? Br31 C1 C14 C15 167.94(11) . . . . ? Br32 C7 C8 C9 -179.93(12) . . . . ? Br32 C7 C18 C17 -9.3(2) . . . . ? Br32 C7 C18 C19 173.52(11) . . . . ? C41 N23 C24 C4 174.84(13) . . . . ? C41 N23 C24 O25 -4.8(2) . . . . ? C41 C42 C43 C44 54.43(18) . . . . ? C42 C41 C46 C45 59.26(17) . . . . ? C42 C43 C44 C45 -54.3(2) . . . . ? C43 C44 C45 C46 56.3(2) . . . . ? C44 C45 C46 C41 -57.68(19) . . . . ? C46 C41 C42 C43 -57.92(17) . . . . ? C51 N28 C29 C10 -175.92(13) . . . . ? C51 N28 C29 O30 4.0(2) . . . . ? C51 C52 C53 C54 -54.23(17) . . . . ? C52 C51 C56 C55 -61.34(17) . . . . ? C52 C53 C54 C55 52.12(19) . . . . ? C53 C54 C55 C56 -53.12(19) . . . . ? C54 C55 C56 C51 56.91(18) . . . . ? C56 C51 C52 C53 59.59(17) . . . . ? #===END _database_code_depnum_ccdc_archive 'CCDC 931602'