# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_complex4 _database_code_depnum_ccdc_archive 'CCDC 892658' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H57 Cl N4, 1.50(C H Cl3)' _chemical_formula_sum 'C42.50 H58.50 Cl5.50 N4' _chemical_formula_weight 820.41 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.5237(3) _cell_length_b 12.7743(2) _cell_length_c 16.6305(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.6610(10) _cell_angle_gamma 90.00 _cell_volume 4668.65(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5591 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9119 _exptl_absorpt_correction_T_max 0.9608 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50959 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5357 _reflns_number_gt 4815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One partially occupied CHCl3 molecule was fixed at 50% occupancy in the asymmetric unit. 5249 Friedel pairs were merged in the final cycle of refinement. ; _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^)+(0.0778P)^2^+5.9278P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 5249 Friedel pairs' _refine_ls_abs_structure_Flack 0.08(7) _refine_ls_number_reflns 5357 _refine_ls_number_parameters 503 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.83032(16) 0.5928(3) 0.9279(2) 0.0246(7) Uani 1 1 d . . . C2 C 0.78280(17) 0.5483(3) 0.8708(2) 0.0305(8) Uani 1 1 d . . . C3 C 0.72586(18) 0.5952(3) 0.8615(3) 0.0363(9) Uani 1 1 d . . . H3 H 0.6922 0.5678 0.8225 0.044 Uiso 1 1 calc R . . C4 C 0.71783(19) 0.6813(4) 0.9083(3) 0.0374(9) Uani 1 1 d . . . H4 H 0.6785 0.7114 0.9024 0.045 Uiso 1 1 calc R . . C5 C 0.76691(19) 0.7241(3) 0.9641(3) 0.0356(9) Uani 1 1 d . . . H5 H 0.7609 0.7839 0.9954 0.043 Uiso 1 1 calc R . . C6 C 0.82459(17) 0.6807(3) 0.9748(2) 0.0309(8) Uani 1 1 d . . . C7 C 0.79082(19) 0.4543(4) 0.8180(3) 0.0397(10) Uani 1 1 d . . . H7 H 0.8339 0.4299 0.8357 0.048 Uiso 1 1 calc R . . C8 C 0.7799(3) 0.4850(5) 0.7276(4) 0.0628(15) Uani 1 1 d . . . H8A H 0.7382 0.5111 0.7091 0.094 Uiso 1 1 calc R . . H8B H 0.7858 0.4238 0.6947 0.094 Uiso 1 1 calc R . . H8C H 0.8087 0.5400 0.7207 0.094 Uiso 1 1 calc R . . C9 C 0.7495(3) 0.3640(4) 0.8299(4) 0.0652(16) Uani 1 1 d . . . H9A H 0.7535 0.3511 0.8889 0.098 Uiso 1 1 calc R . . H9B H 0.7612 0.3009 0.8036 0.098 Uiso 1 1 calc R . . H9C H 0.7072 0.3819 0.8048 0.098 Uiso 1 1 calc R . . C10 C 0.87853(19) 0.7315(3) 1.0331(3) 0.0362(9) Uani 1 1 d . . . H10 H 0.9163 0.6960 1.0249 0.043 Uiso 1 1 calc R . . C11 C 0.8839(3) 0.8483(5) 1.0142(4) 0.0619(15) Uani 1 1 d . . . H11A H 0.8473 0.8850 1.0217 0.093 Uiso 1 1 calc R . . H11B H 0.8881 0.8567 0.9571 0.093 Uiso 1 1 calc R . . H11C H 0.9197 0.8777 1.0516 0.093 Uiso 1 1 calc R . . C12 C 0.8750(3) 0.7165(5) 1.1228(3) 0.0584(14) Uani 1 1 d . . . H12A H 0.8362 0.7441 1.1312 0.088 Uiso 1 1 calc R . . H12B H 0.9087 0.7540 1.1586 0.088 Uiso 1 1 calc R . . H12C H 0.8779 0.6417 1.1364 0.088 Uiso 1 1 calc R . . C13 C 0.93196(16) 0.5599(3) 0.8991(2) 0.0221(7) Uani 1 1 d . . . H13 H 0.9272 0.6023 0.8512 0.026 Uiso 1 1 calc R . . C14 C 0.91359(17) 0.4773(3) 1.0072(2) 0.0274(7) Uani 1 1 d . . . H14 H 0.8931 0.4524 1.0476 0.033 Uiso 1 1 calc R . . C15 C 0.97102(17) 0.4551(3) 1.0023(2) 0.0273(7) Uani 1 1 d . . . H15 H 0.9988 0.4117 1.0389 0.033 Uiso 1 1 calc R . . C16 C 1.03992(15) 0.5084(3) 0.9073(2) 0.0237(7) Uani 1 1 d . . . H16A H 1.0725 0.5362 0.9522 0.028 Uiso 1 1 calc R . . H16B H 1.0364 0.5551 0.8590 0.028 Uiso 1 1 calc R . . C17 C 1.05670(15) 0.3986(3) 0.8847(2) 0.0225(7) Uani 1 1 d . . . C18 C 1.02508(19) 0.2553(3) 0.7863(2) 0.0294(8) Uani 1 1 d . . . C19 C 1.06379(19) 0.2383(3) 0.7324(2) 0.0323(8) Uani 1 1 d . . . C20 C 1.0667(3) 0.1379(4) 0.7015(3) 0.0488(12) Uani 1 1 d . . . H20 H 1.0926 0.1245 0.6646 0.059 Uiso 1 1 calc R . . C21 C 1.0328(3) 0.0574(4) 0.7233(4) 0.0594(15) Uani 1 1 d . . . H21 H 1.0351 -0.0106 0.7011 0.071 Uiso 1 1 calc R . . C22 C 0.9956(4) 0.0754(4) 0.7772(4) 0.070(2) Uani 1 1 d . . . H22 H 0.9718 0.0195 0.7909 0.084 Uiso 1 1 calc R . . C23 C 0.9918(3) 0.1745(4) 0.8125(3) 0.0491(12) Uani 1 1 d . . . C24 C 1.0993(2) 0.3270(4) 0.7051(3) 0.0380(9) Uani 1 1 d . . . H24 H 1.1085 0.3782 0.7516 0.046 Uiso 1 1 calc R . . C25 C 1.1609(2) 0.2920(5) 0.6879(4) 0.0567(14) Uani 1 1 d . . . H25A H 1.1797 0.2401 0.7290 0.085 Uiso 1 1 calc R . . H25B H 1.1879 0.3528 0.6909 0.085 Uiso 1 1 calc R . . H25C H 1.1543 0.2610 0.6327 0.085 Uiso 1 1 calc R . . C26 C 1.0633(3) 0.3843(5) 0.6320(4) 0.0609(16) Uani 1 1 d . . . H26A H 1.0538 0.3367 0.5847 0.091 Uiso 1 1 calc R . . H26B H 1.0871 0.4436 0.6188 0.091 Uiso 1 1 calc R . . H26C H 1.0254 0.4101 0.6446 0.091 Uiso 1 1 calc R . . C27 C 0.9542(4) 0.1909(5) 0.8755(4) 0.070(2) Uani 1 1 d . . . H27 H 0.9686 0.2578 0.9046 0.084 Uiso 1 1 calc R . . C28 C 0.9619(4) 0.1066(7) 0.9410(4) 0.085(2) Uani 1 1 d . . . H28A H 0.9417 0.0423 0.9171 0.127 Uiso 1 1 calc R . . H28B H 0.9438 0.1301 0.9863 0.127 Uiso 1 1 calc R . . H28C H 1.0054 0.0927 0.9620 0.127 Uiso 1 1 calc R . . C29 C 0.8886(5) 0.2059(8) 0.8366(6) 0.104(3) Uani 1 1 d . . . H29A H 0.8842 0.2631 0.7965 0.156 Uiso 1 1 calc R . . H29B H 0.8663 0.2234 0.8793 0.156 Uiso 1 1 calc R . . H29C H 0.8721 0.1413 0.8087 0.156 Uiso 1 1 calc R . . C30 C 1.14361(16) 0.3861(3) 0.9939(2) 0.0238(7) Uani 1 1 d . . . C31 C 1.14730(17) 0.3373(3) 1.0712(2) 0.0290(8) Uani 1 1 d . . . C32 C 1.19388(18) 0.3680(3) 1.1373(2) 0.0330(8) Uani 1 1 d . . . H32 H 1.1971 0.3353 1.1894 0.040 Uiso 1 1 calc R . . C33 C 1.23491(19) 0.4440(3) 1.1289(2) 0.0342(8) Uani 1 1 d . . . H33 H 1.2659 0.4637 1.1749 0.041 Uiso 1 1 calc R . . C34 C 1.23120(18) 0.4923(3) 1.0529(2) 0.0315(8) Uani 1 1 d . . . H34 H 1.2600 0.5447 1.0474 0.038 Uiso 1 1 calc R . . C35 C 1.18573(16) 0.4647(3) 0.9845(2) 0.0273(7) Uani 1 1 d . . . C36 C 1.10254(19) 0.2516(4) 1.0812(3) 0.0355(9) Uani 1 1 d . . . H36 H 1.0661 0.2590 1.0349 0.043 Uiso 1 1 calc R . . C37 C 1.0806(2) 0.2597(4) 1.1610(3) 0.0495(12) Uani 1 1 d . . . H37A H 1.0445 0.2156 1.1575 0.074 Uiso 1 1 calc R . . H37B H 1.0703 0.3326 1.1701 0.074 Uiso 1 1 calc R . . H37C H 1.1129 0.2361 1.2070 0.074 Uiso 1 1 calc R . . C38 C 1.1298(3) 0.1447(4) 1.0733(4) 0.0599(15) Uani 1 1 d . . . H38A H 1.1712 0.1421 1.1073 0.090 Uiso 1 1 calc R . . H38B H 1.1310 0.1320 1.0155 0.090 Uiso 1 1 calc R . . H38C H 1.1049 0.0909 1.0918 0.090 Uiso 1 1 calc R . . C39 C 1.18473(18) 0.5178(3) 0.9028(2) 0.0331(8) Uani 1 1 d . . . H39A H 1.1476 0.4935 0.8625 0.040 Uiso 1 1 calc R . . C40 C 1.1809(2) 0.6380(4) 0.9100(3) 0.0484(11) Uani 1 1 d . . . H40A H 1.1476 0.6563 0.9366 0.073 Uiso 1 1 calc R . . H40B H 1.1734 0.6692 0.8548 0.073 Uiso 1 1 calc R . . H40C H 1.2194 0.6648 0.9431 0.073 Uiso 1 1 calc R . . C41 C 1.2402(2) 0.4879(5) 0.8689(3) 0.0534(13) Uani 1 1 d . . . H41A H 1.2772 0.5129 0.9066 0.080 Uiso 1 1 calc R . . H41B H 1.2369 0.5201 0.8146 0.080 Uiso 1 1 calc R . . H41C H 1.2420 0.4116 0.8638 0.080 Uiso 1 1 calc R . . C42 C 0.8641(2) 0.2257(4) 1.1710(3) 0.0432(10) Uani 1 1 d . . . H42 H 0.8979 0.2781 1.1823 0.052 Uiso 1 1 calc R . . N1 N 0.89004(13) 0.5431(2) 0.94221(18) 0.0230(6) Uani 1 1 d . . . N2 N 0.98214(13) 0.5072(2) 0.93417(18) 0.0238(6) Uani 1 1 d . . . N3 N 1.01820(14) 0.3594(2) 0.81629(18) 0.0249(6) Uani 1 1 d D . . N4 N 1.10122(13) 0.3451(2) 0.92460(18) 0.0239(6) Uani 1 1 d . . . Cl1 Cl 0.95288(5) 0.56285(8) 0.71191(5) 0.0356(2) Uani 1 1 d . . . Cl2 Cl 0.83574(7) 0.21020(13) 1.26054(9) 0.0630(4) Uani 1 1 d . . . Cl3 Cl 0.80634(8) 0.27264(12) 1.09019(10) 0.0713(5) Uani 1 1 d . . . Cl4 Cl 0.89289(8) 0.10625(12) 1.14347(10) 0.0661(4) Uani 1 1 d . . . C43 C 0.0479(6) 0.1159(9) 0.4029(7) 0.060(3) Uani 0.50 1 d P . . H43 H 0.0242 0.0501 0.3864 0.072 Uiso 0.50 1 calc PR . . Cl5 Cl 0.01672(15) 0.2134(2) 0.32962(17) 0.0593(7) Uani 0.50 1 d P . . Cl6 Cl 0.0368(2) 0.1511(4) 0.49920(19) 0.0928(13) Uani 0.50 1 d P . . Cl7 Cl 0.12102(17) 0.0899(3) 0.4019(4) 0.0962(14) Uani 0.50 1 d P . . H1 H 0.996(2) 0.404(3) 0.785(3) 0.042(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0238(16) 0.0264(17) 0.0253(17) 0.0058(14) 0.0091(13) 0.0055(13) C2 0.0249(17) 0.031(2) 0.034(2) 0.0032(16) 0.0044(15) 0.0009(14) C3 0.0258(18) 0.039(2) 0.044(2) 0.0058(18) 0.0067(16) -0.0015(16) C4 0.0278(18) 0.041(2) 0.046(2) 0.0076(19) 0.0136(17) 0.0107(17) C5 0.0306(19) 0.037(2) 0.041(2) 0.0000(17) 0.0126(16) 0.0109(16) C6 0.0291(18) 0.034(2) 0.0305(18) 0.0006(16) 0.0095(15) 0.0052(15) C7 0.0285(19) 0.035(2) 0.051(3) -0.0073(19) -0.0006(17) -0.0010(16) C8 0.078(4) 0.060(4) 0.054(3) -0.013(3) 0.022(3) -0.008(3) C9 0.078(4) 0.038(3) 0.076(4) -0.007(3) 0.010(3) -0.016(3) C10 0.034(2) 0.038(2) 0.037(2) -0.0126(17) 0.0093(17) 0.0042(17) C11 0.057(3) 0.047(3) 0.073(4) -0.007(3) -0.004(3) -0.009(2) C12 0.061(3) 0.082(4) 0.031(2) -0.004(2) 0.006(2) 0.006(3) C13 0.0249(16) 0.0222(16) 0.0189(15) 0.0015(12) 0.0043(12) 0.0032(13) C14 0.0316(18) 0.0270(18) 0.0258(17) 0.0061(14) 0.0109(14) 0.0034(15) C15 0.0291(18) 0.0293(19) 0.0232(16) 0.0068(14) 0.0049(14) 0.0066(14) C16 0.0229(16) 0.0209(16) 0.0272(16) 0.0015(13) 0.0054(13) 0.0018(13) C17 0.0242(16) 0.0219(16) 0.0229(16) 0.0064(13) 0.0085(13) 0.0018(13) C18 0.040(2) 0.0234(18) 0.0244(17) 0.0008(14) 0.0073(15) 0.0001(15) C19 0.037(2) 0.031(2) 0.0299(19) 0.0043(15) 0.0099(16) 0.0061(16) C20 0.072(3) 0.035(2) 0.048(3) -0.005(2) 0.032(3) 0.007(2) C21 0.105(5) 0.029(2) 0.053(3) -0.006(2) 0.036(3) 0.001(3) C22 0.135(6) 0.030(2) 0.063(3) -0.013(2) 0.060(4) -0.025(3) C23 0.082(4) 0.036(2) 0.039(2) -0.0085(19) 0.032(2) -0.015(2) C24 0.041(2) 0.035(2) 0.045(2) 0.0006(18) 0.0241(19) 0.0007(18) C25 0.041(2) 0.064(3) 0.071(4) 0.026(3) 0.025(2) 0.013(2) C26 0.055(3) 0.057(3) 0.080(4) 0.034(3) 0.036(3) 0.019(3) C27 0.116(6) 0.041(3) 0.076(4) -0.022(3) 0.069(4) -0.034(3) C28 0.105(6) 0.111(6) 0.049(3) 0.008(4) 0.039(4) -0.025(5) C29 0.132(8) 0.117(7) 0.086(5) 0.033(5) 0.078(6) 0.043(6) C30 0.0250(16) 0.0231(17) 0.0238(16) -0.0016(13) 0.0060(13) 0.0055(13) C31 0.0323(19) 0.0305(19) 0.0260(17) 0.0040(14) 0.0106(14) 0.0070(15) C32 0.0345(19) 0.039(2) 0.0250(18) 0.0021(15) 0.0047(15) 0.0083(16) C33 0.033(2) 0.043(2) 0.0253(18) -0.0037(16) 0.0029(15) 0.0024(17) C34 0.0284(18) 0.034(2) 0.0314(19) -0.0026(16) 0.0053(15) 0.0019(15) C35 0.0254(17) 0.0299(18) 0.0271(17) 0.0007(14) 0.0068(14) 0.0048(14) C36 0.035(2) 0.040(2) 0.032(2) 0.0109(17) 0.0085(16) 0.0037(17) C37 0.054(3) 0.053(3) 0.047(3) 0.011(2) 0.024(2) 0.001(2) C38 0.074(4) 0.035(3) 0.082(4) 0.008(3) 0.041(3) -0.002(2) C39 0.033(2) 0.035(2) 0.0304(19) 0.0088(16) 0.0069(15) -0.0037(16) C40 0.052(3) 0.040(3) 0.049(3) 0.011(2) 0.002(2) -0.006(2) C41 0.053(3) 0.072(4) 0.041(3) 0.022(2) 0.024(2) 0.008(3) C42 0.051(3) 0.044(3) 0.035(2) -0.0048(18) 0.0108(19) -0.012(2) N1 0.0235(14) 0.0240(14) 0.0225(14) 0.0004(11) 0.0074(11) 0.0049(11) N2 0.0252(14) 0.0252(15) 0.0205(13) 0.0009(11) 0.0041(11) 0.0026(11) N3 0.0300(15) 0.0202(14) 0.0242(14) 0.0021(11) 0.0055(12) 0.0015(12) N4 0.0236(14) 0.0235(15) 0.0257(15) 0.0036(11) 0.0077(11) 0.0020(11) Cl1 0.0440(5) 0.0409(5) 0.0218(4) 0.0037(4) 0.0073(3) 0.0139(4) Cl2 0.0690(8) 0.0733(9) 0.0542(7) -0.0015(7) 0.0298(7) -0.0065(7) Cl3 0.0843(10) 0.0548(8) 0.0595(8) 0.0030(6) -0.0172(7) -0.0165(7) Cl4 0.0729(9) 0.0514(8) 0.0793(10) -0.0170(7) 0.0279(8) -0.0005(7) C43 0.086(8) 0.046(6) 0.059(6) -0.019(5) 0.041(6) -0.022(5) Cl5 0.0831(19) 0.0506(14) 0.0487(13) -0.0071(11) 0.0242(13) -0.0113(13) Cl6 0.108(3) 0.134(4) 0.0410(14) -0.0012(18) 0.0254(16) 0.042(3) Cl7 0.069(2) 0.071(2) 0.161(4) 0.025(2) 0.052(2) 0.0217(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.388(5) . ? C1 C6 1.390(5) . ? C1 N1 1.459(4) . ? C2 C3 1.393(6) . ? C2 C7 1.521(6) . ? C3 C4 1.382(7) . ? C3 H3 0.9500 . ? C4 C5 1.390(7) . ? C4 H4 0.9500 . ? C5 C6 1.388(5) . ? C5 H5 0.9500 . ? C6 C10 1.522(6) . ? C7 C8 1.522(8) . ? C7 C9 1.522(7) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.525(7) . ? C10 C11 1.535(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.322(5) . ? C13 N2 1.334(5) . ? C13 H13 0.9500 . ? C14 C15 1.344(5) . ? C14 N1 1.380(5) . ? C14 H14 0.9500 . ? C15 N2 1.384(5) . ? C15 H15 0.9500 . ? C16 N2 1.466(4) . ? C16 C17 1.521(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N4 1.273(5) . ? C17 N3 1.366(5) . ? C18 C19 1.398(6) . ? C18 C23 1.399(6) . ? C18 N3 1.440(5) . ? C19 C20 1.388(6) . ? C19 C24 1.512(6) . ? C20 C21 1.376(8) . ? C20 H20 0.9500 . ? C21 C22 1.373(8) . ? C21 H21 0.9500 . ? C22 C23 1.406(7) . ? C22 H22 0.9500 . ? C23 C27 1.499(7) . ? C24 C26 1.497(7) . ? C24 C25 1.543(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.490(12) . ? C27 C28 1.515(10) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.413(5) . ? C30 C31 1.415(5) . ? C30 N4 1.425(5) . ? C31 C32 1.400(6) . ? C31 C36 1.522(6) . ? C32 C33 1.368(6) . ? C32 H32 0.9500 . ? C33 C34 1.393(6) . ? C33 H33 0.9500 . ? C34 C35 1.398(5) . ? C34 H34 0.9500 . ? C35 C39 1.515(5) . ? C36 C38 1.515(7) . ? C36 C37 1.516(6) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.526(6) . ? C39 C40 1.544(7) . ? C39 H39A 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 Cl2 1.754(5) . ? C42 Cl4 1.758(5) . ? C42 Cl3 1.758(5) . ? C42 H42 1.0000 . ? N3 H1 0.857(10) . ? C43 Cl7 1.684(13) . ? C43 Cl6 1.734(11) . ? C43 Cl5 1.776(14) . ? C43 H43 1.0000 . ? 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 C6 124.3(3) . . ? C2 C1 N1 118.6(3) . . ? C6 C1 N1 117.1(3) . . ? C1 C2 C3 116.9(4) . . ? C1 C2 C7 123.2(3) . . ? C3 C2 C7 119.9(4) . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 116.7(4) . . ? C5 C6 C10 120.4(4) . . ? C1 C6 C10 122.8(3) . . ? C2 C7 C8 110.7(4) . . ? C2 C7 C9 111.7(4) . . ? C8 C7 C9 110.6(4) . . ? C2 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 111.3(4) . . ? C6 C10 C11 111.8(4) . . ? C12 C10 C11 110.2(4) . . ? C6 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 108.6(3) . . ? N1 C13 H13 125.7 . . ? N2 C13 H13 125.7 . . ? C15 C14 N1 106.9(3) . . ? C15 C14 H14 126.5 . . ? N1 C14 H14 126.5 . . ? C14 C15 N2 107.3(3) . . ? C14 C15 H15 126.4 . . ? N2 C15 H15 126.4 . . ? N2 C16 C17 110.6(3) . . ? N2 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N4 C17 N3 121.4(3) . . ? N4 C17 C16 125.1(3) . . ? N3 C17 C16 113.4(3) . . ? C19 C18 C23 122.4(4) . . ? C19 C18 N3 119.7(3) . . ? C23 C18 N3 117.9(4) . . ? C20 C19 C18 117.9(4) . . ? C20 C19 C24 120.7(4) . . ? C18 C19 C24 121.4(4) . . ? C21 C20 C19 121.2(4) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 120.0(5) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.6(5) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C18 C23 C22 116.7(4) . . ? C18 C23 C27 122.5(4) . . ? C22 C23 C27 120.8(4) . . ? C26 C24 C19 112.4(4) . . ? C26 C24 C25 109.9(4) . . ? C19 C24 C25 113.3(4) . . ? C26 C24 H24 107.0 . . ? C19 C24 H24 107.0 . . ? C25 C24 H24 107.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 112.0(6) . . ? C29 C27 C28 110.5(6) . . ? C23 C27 C28 114.2(6) . . ? C29 C27 H27 106.5 . . ? C23 C27 H27 106.5 . . ? C28 C27 H27 106.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 120.4(3) . . ? C35 C30 N4 121.3(3) . . ? C31 C30 N4 117.9(3) . . ? C32 C31 C30 118.4(4) . . ? C32 C31 C36 121.0(3) . . ? C30 C31 C36 120.6(3) . . ? C33 C32 C31 121.7(4) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C34 120.0(4) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 120.9(4) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C30 118.7(3) . . ? C34 C35 C39 118.7(4) . . ? C30 C35 C39 122.6(3) . . ? C38 C36 C37 110.7(4) . . ? C38 C36 C31 110.3(4) . . ? C37 C36 C31 113.4(4) . . ? C38 C36 H36 107.4 . . ? C37 C36 H36 107.4 . . ? C31 C36 H36 107.4 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 C41 111.5(3) . . ? C35 C39 C40 111.5(4) . . ? C41 C39 C40 109.9(4) . . ? C35 C39 H39A 107.9 . . ? C41 C39 H39A 107.9 . . ? C40 C39 H39A 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Cl2 C42 Cl4 110.3(3) . . ? Cl2 C42 Cl3 110.0(3) . . ? Cl4 C42 Cl3 110.5(3) . . ? Cl2 C42 H42 108.7 . . ? Cl4 C42 H42 108.7 . . ? Cl3 C42 H42 108.7 . . ? C13 N1 C14 109.0(3) . . ? C13 N1 C1 125.7(3) . . ? C14 N1 C1 125.1(3) . . ? C13 N2 C15 108.2(3) . . ? C13 N2 C16 125.8(3) . . ? C15 N2 C16 125.9(3) . . ? C17 N3 C18 122.0(3) . . ? C17 N3 H1 117(4) . . ? C18 N3 H1 119(4) . . ? C17 N4 C30 122.4(3) . . ? Cl7 C43 Cl6 113.5(8) . . ? Cl7 C43 Cl5 111.8(6) . . ? Cl6 C43 Cl5 109.7(7) . . ? Cl7 C43 H43 107.2 . . ? Cl6 C43 H43 107.2 . . ? Cl5 C43 H43 107.2 . . ? 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 C6 C1 C2 C3 -0.8(6) . . . . ? N1 C1 C2 C3 177.2(3) . . . . ? C6 C1 C2 C7 177.7(4) . . . . ? N1 C1 C2 C7 -4.3(6) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C7 C2 C3 C4 -179.4(4) . . . . ? C2 C3 C4 C5 1.6(7) . . . . ? C3 C4 C5 C6 -0.9(7) . . . . ? C4 C5 C6 C1 -0.6(6) . . . . ? C4 C5 C6 C10 177.0(4) . . . . ? C2 C1 C6 C5 1.5(6) . . . . ? N1 C1 C6 C5 -176.5(3) . . . . ? C2 C1 C6 C10 -176.1(4) . . . . ? N1 C1 C6 C10 5.9(5) . . . . ? C1 C2 C7 C8 -113.4(5) . . . . ? C3 C2 C7 C8 65.1(5) . . . . ? C1 C2 C7 C9 122.8(5) . . . . ? C3 C2 C7 C9 -58.7(6) . . . . ? C5 C6 C10 C12 71.4(5) . . . . ? C1 C6 C10 C12 -111.1(5) . . . . ? C5 C6 C10 C11 -52.4(6) . . . . ? C1 C6 C10 C11 125.1(5) . . . . ? N1 C14 C15 N2 -0.2(4) . . . . ? N2 C16 C17 N4 -111.8(4) . . . . ? N2 C16 C17 N3 67.1(4) . . . . ? C23 C18 C19 C20 2.9(7) . . . . ? N3 C18 C19 C20 -176.7(4) . . . . ? C23 C18 C19 C24 -179.9(4) . . . . ? N3 C18 C19 C24 0.6(6) . . . . ? C18 C19 C20 C21 -0.2(8) . . . . ? C24 C19 C20 C21 -177.5(5) . . . . ? C19 C20 C21 C22 -0.6(10) . . . . ? C20 C21 C22 C23 -1.2(11) . . . . ? C19 C18 C23 C22 -4.5(8) . . . . ? N3 C18 C23 C22 175.0(5) . . . . ? C19 C18 C23 C27 175.0(6) . . . . ? N3 C18 C23 C27 -5.5(8) . . . . ? C21 C22 C23 C18 3.6(10) . . . . ? C21 C22 C23 C27 -175.8(7) . . . . ? C20 C19 C24 C26 91.3(5) . . . . ? C18 C19 C24 C26 -85.9(5) . . . . ? C20 C19 C24 C25 -34.0(6) . . . . ? C18 C19 C24 C25 148.8(4) . . . . ? C18 C23 C27 C29 98.6(7) . . . . ? C22 C23 C27 C29 -82.0(9) . . . . ? C18 C23 C27 C28 -134.9(6) . . . . ? C22 C23 C27 C28 44.6(9) . . . . ? C35 C30 C31 C32 -0.7(5) . . . . ? N4 C30 C31 C32 172.0(3) . . . . ? C35 C30 C31 C36 -179.2(3) . . . . ? N4 C30 C31 C36 -6.5(5) . . . . ? C30 C31 C32 C33 0.6(6) . . . . ? C36 C31 C32 C33 179.1(4) . . . . ? C31 C32 C33 C34 -0.4(6) . . . . ? C32 C33 C34 C35 0.3(6) . . . . ? C33 C34 C35 C30 -0.4(6) . . . . ? C33 C34 C35 C39 -178.5(4) . . . . ? C31 C30 C35 C34 0.6(5) . . . . ? N4 C30 C35 C34 -171.9(3) . . . . ? C31 C30 C35 C39 178.6(3) . . . . ? N4 C30 C35 C39 6.1(5) . . . . ? C32 C31 C36 C38 -82.4(5) . . . . ? C30 C31 C36 C38 96.1(5) . . . . ? C32 C31 C36 C37 42.5(5) . . . . ? C30 C31 C36 C37 -139.0(4) . . . . ? C34 C35 C39 C41 66.4(5) . . . . ? C30 C35 C39 C41 -111.6(5) . . . . ? C34 C35 C39 C40 -56.9(5) . . . . ? C30 C35 C39 C40 125.1(4) . . . . ? N2 C13 N1 C14 -0.2(4) . . . . ? N2 C13 N1 C1 175.0(3) . . . . ? C15 C14 N1 C13 0.3(4) . . . . ? C15 C14 N1 C1 -175.0(3) . . . . ? C2 C1 N1 C13 86.1(5) . . . . ? C6 C1 N1 C13 -95.8(4) . . . . ? C2 C1 N1 C14 -99.4(4) . . . . ? C6 C1 N1 C14 78.7(5) . . . . ? N1 C13 N2 C15 0.0(4) . . . . ? N1 C13 N2 C16 -177.4(3) . . . . ? C14 C15 N2 C13 0.1(4) . . . . ? C14 C15 N2 C16 177.5(3) . . . . ? C17 C16 N2 C13 -120.3(4) . . . . ? C17 C16 N2 C15 62.7(4) . . . . ? N4 C17 N3 C18 1.0(5) . . . . ? C16 C17 N3 C18 -177.9(3) . . . . ? C19 C18 N3 C17 -86.7(4) . . . . ? C23 C18 N3 C17 93.8(5) . . . . ? N3 C17 N4 C30 177.1(3) . . . . ? C16 C17 N4 C30 -4.2(5) . . . . ? C35 C30 N4 C17 -70.1(5) . . . . ? C31 C30 N4 C17 117.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.098 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.057 data_complex6 _database_code_depnum_ccdc_archive 'CCDC 892659' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H59 K N4 O0.50' _chemical_formula_weight 679.04 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' K K 0.2009 0.2494 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.80520(10) _cell_length_b 14.34640(10) _cell_length_c 20.6098(2) _cell_angle_alpha 90.5980(10) _cell_angle_beta 94.8700(10) _cell_angle_gamma 95.8140(10) _cell_volume 4045.47(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 148119 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9676 _exptl_absorpt_correction_T_max 0.9804 _exptl_absorpt_process_details ? _exptl_special_details ; 'SADABS2007/2' ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; 'Bruker-Nonius FR591 rotating anode' ; _diffrn_radiation_monochromator ; '10cm confocal mirrors' ; _diffrn_measurement_device_type ; 'Bruker-Nonius 95mm CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83404 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.52 _reflns_number_total 18443 _reflns_number_gt 13353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) and COLLECT' ; _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+6.2852P] 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 18443 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 K1 K 0.19437(4) 0.83387(4) 0.22501(3) 0.03174(14) Uani 1 1 d . . . K2 K 0.5000 0.5000 0.5000 0.02707(17) Uani 1 2 d S . . K3 K 0.5000 1.0000 0.0000 0.03158(19) Uani 1 2 d S . . N1 N 0.22846(15) 0.49707(14) 0.39330(10) 0.0241(4) Uani 1 1 d . . . N3 N 0.10212(16) 0.62234(15) 0.34948(10) 0.0257(4) Uani 1 1 d . . . N4 N 0.02597(16) 0.62486(15) 0.25558(10) 0.0268(5) Uani 1 1 d . . . N2 N 0.33288(15) 0.61222(14) 0.45443(10) 0.0221(4) Uani 1 1 d . . . C30 C 0.29889(18) 0.43367(16) 0.40519(12) 0.0229(5) Uani 1 1 d . . . C19 C 0.40306(19) 0.77614(17) 0.45644(12) 0.0258(5) Uani 1 1 d . . . C35 C 0.37512(19) 0.42963(17) 0.36391(12) 0.0255(5) Uani 1 1 d . . . C3 C 0.10126(19) 0.67345(18) 0.29352(12) 0.0269(5) Uani 1 1 d . . . C34 C 0.43954(19) 0.36139(18) 0.37431(13) 0.0274(5) Uani 1 1 d . . . H34 H 0.4894 0.3570 0.3457 0.033 Uiso 1 1 calc R . . C32 C 0.35873(19) 0.30488(18) 0.46610(13) 0.0279(5) Uani 1 1 d . . . H32 H 0.3545 0.2628 0.5013 0.033 Uiso 1 1 calc R . . C1 C 0.25031(18) 0.58150(17) 0.41908(11) 0.0218(5) Uani 1 1 d . . . C18 C 0.34345(17) 0.70246(17) 0.48351(12) 0.0225(5) Uani 1 1 d . . . C27 C 0.23842(19) 0.64125(18) 0.57310(12) 0.0269(5) Uani 1 1 d . . . H27 H 0.2047 0.6005 0.5366 0.032 Uiso 1 1 calc R . . C31 C 0.29015(19) 0.36989(17) 0.45712(12) 0.0263(5) Uani 1 1 d . . . C23 C 0.30267(18) 0.71881(17) 0.54285(12) 0.0247(5) Uani 1 1 d . . . C21 C 0.3833(2) 0.87666(19) 0.54835(14) 0.0333(6) Uani 1 1 d . . . H21 H 0.3976 0.9353 0.5707 0.040 Uiso 1 1 calc R . . C33 C 0.43257(19) 0.29993(18) 0.42528(13) 0.0285(6) Uani 1 1 d . . . H33 H 0.4780 0.2548 0.4322 0.034 Uiso 1 1 calc R . . C36 C 0.2049(2) 0.37138(19) 0.49875(14) 0.0318(6) Uani 1 1 d . . . H36 H 0.1947 0.4385 0.5064 0.038 Uiso 1 1 calc R . . C6 C -0.0128(2) 0.65817(19) 0.19398(13) 0.0304(6) Uani 1 1 d . . . C22 C 0.3246(2) 0.80573(18) 0.57476(13) 0.0300(6) Uani 1 1 d . . . H22 H 0.2988 0.8162 0.6152 0.036 Uiso 1 1 calc R . . C5 C 0.0306(2) 0.5489(2) 0.34696(14) 0.0343(6) Uani 1 1 d . . . H5 H 0.0186 0.5053 0.3805 0.041 Uiso 1 1 calc R . . C2 C 0.17037(18) 0.64736(17) 0.40662(12) 0.0245(5) Uani 1 1 d . . . H2A H 0.1329 0.6482 0.4455 0.029 Uiso 1 1 calc R . . H2B H 0.2019 0.7116 0.4013 0.029 Uiso 1 1 calc R . . C20 C 0.4211(2) 0.86257(19) 0.48974(14) 0.0325(6) Uani 1 1 d . . . H20 H 0.4602 0.9124 0.4716 0.039 Uiso 1 1 calc R . . C7 C 0.0216(2) 0.6257(2) 0.13665(14) 0.0344(6) Uani 1 1 d . . . C4 C -0.0196(2) 0.5498(2) 0.28803(14) 0.0352(6) Uani 1 1 d . . . H4 H -0.0745 0.5082 0.2719 0.042 Uiso 1 1 calc R . . C8 C -0.0187(2) 0.6576(2) 0.07805(14) 0.0386(7) Uani 1 1 d . . . H8 H 0.0034 0.6371 0.0384 0.046 Uiso 1 1 calc R . . C10 C -0.1215(2) 0.7518(2) 0.13338(15) 0.0389(7) Uani 1 1 d . . . H10 H -0.1690 0.7954 0.1318 0.047 Uiso 1 1 calc R . . C25 C 0.5367(2) 0.8278(2) 0.38173(16) 0.0423(7) Uani 1 1 d . . . H25A H 0.5162 0.8902 0.3731 0.063 Uiso 1 1 calc R . . H25B H 0.5681 0.8060 0.3443 0.063 Uiso 1 1 calc R . . H25C H 0.5831 0.8309 0.4206 0.063 Uiso 1 1 calc R . . C11 C -0.0837(2) 0.7214(2) 0.19385(14) 0.0350(6) Uani 1 1 d . . . C12 C 0.1034(2) 0.5619(2) 0.13761(16) 0.0442(7) Uani 1 1 d . . . H12 H 0.1111 0.5346 0.1819 0.053 Uiso 1 1 calc R . . C9 C -0.0908(2) 0.7193(2) 0.07609(15) 0.0409(7) Uani 1 1 d . . . H9 H -0.1187 0.7389 0.0354 0.049 Uiso 1 1 calc R . . C15 C -0.1181(2) 0.7587(2) 0.25666(15) 0.0456(8) Uani 1 1 d . . . H15 H -0.0877 0.7239 0.2935 0.055 Uiso 1 1 calc R . . C14 C 0.0832(3) 0.4819(2) 0.08819(18) 0.0524(9) Uani 1 1 d . . . H14A H 0.0202 0.4468 0.0946 0.079 Uiso 1 1 calc R . . H14B H 0.1351 0.4402 0.0939 0.079 Uiso 1 1 calc R . . H14C H 0.0813 0.5071 0.0441 0.079 Uiso 1 1 calc R . . C13 C 0.1999(3) 0.6189(3) 0.1253(3) 0.0760(14) Uani 1 1 d . . . H13A H 0.1909 0.6541 0.0851 0.114 Uiso 1 1 calc R . . H13B H 0.2503 0.5764 0.1210 0.114 Uiso 1 1 calc R . . H13C H 0.2200 0.6627 0.1619 0.114 Uiso 1 1 calc R . . N5 N 0.34805(15) 0.90212(15) 0.15231(10) 0.0248(4) Uani 1 1 d . . . N6 N 0.44744(15) 1.04111(15) 0.13214(10) 0.0245(4) Uani 1 1 d . . . C40 C 0.40140(17) 0.98165(17) 0.17089(12) 0.0227(5) Uani 1 1 d . . . C44 C 0.63522(19) 1.0235(2) 0.20949(13) 0.0294(6) Uani 1 1 d . . . H44 H 0.5809 0.9724 0.1998 0.035 Uiso 1 1 calc R . . C41 C 0.40792(18) 0.99661(18) 0.24512(12) 0.0246(5) Uani 1 1 d . . . H41A H 0.3997 0.9345 0.2656 0.030 Uiso 1 1 calc R . . H41B H 0.4744 1.0259 0.2597 0.030 Uiso 1 1 calc R . . C42 C 0.50288(19) 1.12219(18) 0.16044(12) 0.0260(5) Uani 1 1 d . . . C45 C 0.6776(2) 1.0121(2) 0.27972(14) 0.0383(7) Uani 1 1 d . . . H45A H 0.7356 1.0570 0.2891 0.057 Uiso 1 1 calc R . . H45B H 0.6956 0.9482 0.2854 0.057 Uiso 1 1 calc R . . H45C H 0.6285 1.0239 0.3097 0.057 Uiso 1 1 calc R . . C43 C 0.59288(19) 1.11684(19) 0.19823(12) 0.0280(6) Uani 1 1 d . . . C47 C 0.5256(2) 1.2914(2) 0.17471(13) 0.0347(6) Uani 1 1 d . . . H47 H 0.5037 1.3512 0.1665 0.042 Uiso 1 1 calc R . . C50 C 0.3763(2) 1.2197(2) 0.10472(13) 0.0312(6) Uani 1 1 d . . . H50 H 0.3741 1.1734 0.0679 0.037 Uiso 1 1 calc R . . C51 C 0.2845(2) 1.1955(2) 0.14087(14) 0.0363(6) Uani 1 1 d . . . H51A H 0.2843 1.1316 0.1573 0.054 Uiso 1 1 calc R . . H51B H 0.2261 1.1997 0.1109 0.054 Uiso 1 1 calc R . . H51C H 0.2845 1.2396 0.1775 0.054 Uiso 1 1 calc R . . C46 C 0.6452(2) 1.1990(2) 0.22396(13) 0.0346(6) Uani 1 1 d . . . H46 H 0.7053 1.1956 0.2495 0.041 Uiso 1 1 calc R . . C48 C 0.4701(2) 1.21125(19) 0.14770(12) 0.0296(6) Uani 1 1 d . . . C49 C 0.7131(2) 1.0107(2) 0.16239(15) 0.0434(7) Uani 1 1 d . . . H49A H 0.6842 1.0134 0.1175 0.065 Uiso 1 1 calc R . . H49B H 0.7382 0.9498 0.1694 0.065 Uiso 1 1 calc R . . H49C H 0.7669 1.0607 0.1702 0.065 Uiso 1 1 calc R . . N7 N 0.33677(15) 1.05449(14) 0.26937(10) 0.0226(4) Uani 1 1 d . . . N8 N 0.20716(15) 1.09576(15) 0.30386(10) 0.0240(4) Uani 1 1 d . . . C53 C 0.24121(18) 1.02213(18) 0.27342(12) 0.0245(5) Uani 1 1 d . . . C54 C 0.36128(19) 1.14306(18) 0.29708(12) 0.0277(5) Uani 1 1 d . . . H54 H 0.4237 1.1782 0.2997 0.033 Uiso 1 1 calc R . . C52 C 0.6115(2) 1.2853(2) 0.21304(14) 0.0374(7) Uani 1 1 d . . . H52 H 0.6474 1.3404 0.2319 0.045 Uiso 1 1 calc R . . C55 C 0.27922(19) 1.16951(18) 0.31948(12) 0.0269(5) Uani 1 1 d . . . H55 H 0.2720 1.2266 0.3414 0.032 Uiso 1 1 calc R . . C60 C 0.03937(19) 1.13860(19) 0.29138(13) 0.0282(5) Uani 1 1 d . . . C57 C 0.09252(19) 1.04077(18) 0.38209(13) 0.0273(5) Uani 1 1 d . . . C59 C -0.0525(2) 1.1346(2) 0.31507(14) 0.0317(6) Uani 1 1 d . . . H59 H -0.1021 1.1664 0.2929 0.038 Uiso 1 1 calc R . . C56 C 0.11051(18) 1.09158(17) 0.32573(12) 0.0243(5) Uani 1 1 d . . . C62 C 0.0604(2) 1.1943(2) 0.23111(15) 0.0392(7) Uani 1 1 d . . . H62 H 0.1291 1.1864 0.2219 0.047 Uiso 1 1 calc R . . C58 C -0.0008(2) 1.0387(2) 0.40298(13) 0.0319(6) Uani 1 1 d . . . H58 H -0.0156 1.0045 0.4407 0.038 Uiso 1 1 calc R . . C70 C 0.3831(2) 0.4963(2) 0.30761(13) 0.0336(6) Uani 1 1 d . . . H70 H 0.3547 0.5547 0.3201 0.040 Uiso 1 1 calc R . . C65 C 0.2121(2) 1.0527(2) 0.48048(15) 0.0378(7) Uani 1 1 d . . . H65A H 0.2402 1.1139 0.4664 0.057 Uiso 1 1 calc R . . H65B H 0.2629 1.0213 0.5051 0.057 Uiso 1 1 calc R . . H65C H 0.1594 1.0615 0.5082 0.057 Uiso 1 1 calc R . . C61 C -0.07264(19) 1.0850(2) 0.37043(13) 0.0321(6) Uani 1 1 d . . . H61 H -0.1357 1.0828 0.3859 0.039 Uiso 1 1 calc R . . C67 C 0.2992(2) 0.5798(2) 0.61653(14) 0.0367(6) Uani 1 1 d . . . H67A H 0.3465 0.5527 0.5910 0.055 Uiso 1 1 calc R . . H67B H 0.2561 0.5294 0.6339 0.055 Uiso 1 1 calc R . . H67C H 0.3340 0.6179 0.6526 0.055 Uiso 1 1 calc R . . C64 C 0.1354(2) 0.8938(2) 0.44030(15) 0.0407(7) Uani 1 1 d . . . H64A H 0.0841 0.8966 0.4701 0.061 Uiso 1 1 calc R . . H64B H 0.1900 0.8641 0.4620 0.061 Uiso 1 1 calc R . . H64C H 0.1090 0.8570 0.4013 0.061 Uiso 1 1 calc R . . C63 C 0.1713(2) 0.9928(2) 0.42094(13) 0.0308(6) Uani 1 1 d . . . H63 H 0.2259 0.9878 0.3925 0.037 Uiso 1 1 calc R . . C66 C 0.3696(2) 1.3166(2) 0.07489(15) 0.0420(7) Uani 1 1 d . . . H66A H 0.3613 1.3622 0.1092 0.063 Uiso 1 1 calc R . . H66B H 0.3135 1.3137 0.0421 0.063 Uiso 1 1 calc R . . H66C H 0.4297 1.3358 0.0543 0.063 Uiso 1 1 calc R . . C71 C 0.1112(2) 0.3241(2) 0.46181(17) 0.0424(7) Uani 1 1 d . . . H71A H 0.1009 0.3533 0.4194 0.064 Uiso 1 1 calc R . . H71B H 0.0554 0.3314 0.4871 0.064 Uiso 1 1 calc R . . H71C H 0.1175 0.2572 0.4554 0.064 Uiso 1 1 calc R . . C68 C 0.1591(2) 0.6768(2) 0.61136(17) 0.0455(8) Uani 1 1 d . . . H68A H 0.1894 0.7099 0.6510 0.068 Uiso 1 1 calc R . . H68B H 0.1142 0.6237 0.6232 0.068 Uiso 1 1 calc R . . H68C H 0.1229 0.7198 0.5844 0.068 Uiso 1 1 calc R . . C80 C 0.26804(19) 0.89592(18) 0.04080(13) 0.0270(5) Uani 1 1 d . . . C79 C 0.34470(18) 0.87440(18) 0.08592(12) 0.0243(5) Uani 1 1 d . . . C72 C 0.2217(3) 0.3272(2) 0.56568(15) 0.0447(8) Uani 1 1 d . . . H72A H 0.2233 0.2595 0.5602 0.067 Uiso 1 1 calc R . . H72B H 0.1685 0.3392 0.5922 0.067 Uiso 1 1 calc R . . H72C H 0.2840 0.3548 0.5874 0.067 Uiso 1 1 calc R . . C73 C 0.4878(3) 0.5245(3) 0.29193(19) 0.0530(9) Uani 1 1 d . . . H73A H 0.5272 0.5479 0.3317 0.080 Uiso 1 1 calc R . . H73B H 0.4884 0.5738 0.2594 0.080 Uiso 1 1 calc R . . H73C H 0.5152 0.4699 0.2747 0.080 Uiso 1 1 calc R . . C74 C 0.3216(3) 0.4538(3) 0.24788(16) 0.0622(11) Uani 1 1 d . . . H74A H 0.3451 0.3942 0.2361 0.093 Uiso 1 1 calc R . . H74B H 0.3270 0.4970 0.2115 0.093 Uiso 1 1 calc R . . H74C H 0.2531 0.4428 0.2575 0.093 Uiso 1 1 calc R . . C75 C -0.2277(3) 0.7417(3) 0.25837(18) 0.0560(9) Uani 1 1 d . . . H75A H -0.2461 0.7632 0.3005 0.084 Uiso 1 1 calc R . . H75B H -0.2484 0.6745 0.2524 0.084 Uiso 1 1 calc R . . H75C H -0.2598 0.7763 0.2234 0.084 Uiso 1 1 calc R . . C76 C -0.0821(3) 0.8623(3) 0.2672(2) 0.0725(13) Uani 1 1 d . . . H76A H -0.1060 0.8978 0.2299 0.109 Uiso 1 1 calc R . . H76B H -0.0104 0.8700 0.2717 0.109 Uiso 1 1 calc R . . H76C H -0.1066 0.8855 0.3069 0.109 Uiso 1 1 calc R . . C77 C -0.0048(4) 1.1593(4) 0.17219(19) 0.0854(16) Uani 1 1 d . . . H77A H 0.0036 1.0935 0.1636 0.128 Uiso 1 1 calc R . . H77B H 0.0125 1.1967 0.1345 0.128 Uiso 1 1 calc R . . H77C H -0.0730 1.1651 0.1799 0.128 Uiso 1 1 calc R . . C78 C 0.0547(4) 1.2997(3) 0.2444(2) 0.0809(14) Uani 1 1 d . . . H78A H 0.0771 1.3357 0.2074 0.121 Uiso 1 1 calc R . . H78B H 0.0965 1.3197 0.2839 0.121 Uiso 1 1 calc R . . H78C H -0.0130 1.3105 0.2503 0.121 Uiso 1 1 calc R . . C84 C 0.41482(19) 0.81666(18) 0.06638(12) 0.0261(5) Uani 1 1 d . . . C83 C 0.4057(2) 0.78126(19) 0.00251(13) 0.0305(6) Uani 1 1 d . . . H83 H 0.4528 0.7429 -0.0109 0.037 Uiso 1 1 calc R . . C81 C 0.2612(2) 0.8567(2) -0.02213(13) 0.0317(6) Uani 1 1 d . . . H81 H 0.2081 0.8689 -0.0522 0.038 Uiso 1 1 calc R . . C82 C 0.3295(2) 0.8009(2) -0.04160(13) 0.0334(6) Uani 1 1 d . . . H82 H 0.3242 0.7762 -0.0848 0.040 Uiso 1 1 calc R . . C85 C 0.19178(19) 0.9575(2) 0.06003(14) 0.0325(6) Uani 1 1 d . . . H85 H 0.2147 0.9863 0.1037 0.039 Uiso 1 1 calc R . . C87 C 0.1775(2) 1.0373(2) 0.01225(16) 0.0429(7) Uani 1 1 d . . . H87A H 0.2403 1.0747 0.0089 0.064 Uiso 1 1 calc R . . H87B H 0.1306 1.0771 0.0281 0.064 Uiso 1 1 calc R . . H87C H 0.1526 1.0108 -0.0307 0.064 Uiso 1 1 calc R . . C86 C 0.0938(2) 0.8992(2) 0.06620(17) 0.0450(8) Uani 1 1 d . . . H86A H 0.0662 0.8756 0.0230 0.068 Uiso 1 1 calc R . . H86B H 0.0485 0.9385 0.0847 0.068 Uiso 1 1 calc R . . H86C H 0.1039 0.8463 0.0948 0.068 Uiso 1 1 calc R . . C88 C 0.4970(2) 0.7915(2) 0.11470(13) 0.0320(6) Uani 1 1 d . . . H88 H 0.5076 0.8423 0.1489 0.038 Uiso 1 1 calc R . . C90 C 0.5937(2) 0.7871(3) 0.08542(17) 0.0557(10) Uani 1 1 d . . . H90A H 0.6448 0.7781 0.1201 0.084 Uiso 1 1 calc R . . H90B H 0.6108 0.8458 0.0632 0.084 Uiso 1 1 calc R . . H90C H 0.5879 0.7346 0.0541 0.084 Uiso 1 1 calc R . . C89 C 0.4686(3) 0.7017(3) 0.1484(2) 0.0701(13) Uani 1 1 d . . . H89A H 0.4071 0.7064 0.1682 0.105 Uiso 1 1 calc R . . H89B H 0.5200 0.6906 0.1824 0.105 Uiso 1 1 calc R . . H89C H 0.4600 0.6496 0.1167 0.105 Uiso 1 1 calc R . . O1 O 0.7683(3) 0.4827(3) 0.1844(2) 0.1027(12) Uani 1 1 d . . . C91 C 0.8150(4) 0.4208(5) 0.1449(3) 0.114(2) Uani 1 1 d . . . H91A H 0.7930 0.3546 0.1534 0.137 Uiso 1 1 calc R . . H91B H 0.8869 0.4309 0.1540 0.137 Uiso 1 1 calc R . . C92 C 0.7858(4) 0.4442(4) 0.0768(3) 0.0981(19) Uani 1 1 d . . . H92A H 0.7837 0.3888 0.0475 0.118 Uiso 1 1 calc R . . H92B H 0.8312 0.4953 0.0612 0.118 Uiso 1 1 calc R . . C93 C 0.6828(5) 0.4758(4) 0.0810(3) 0.112(2) Uani 1 1 d . . . H93A H 0.6658 0.5181 0.0451 0.135 Uiso 1 1 calc R . . H93B H 0.6324 0.4214 0.0802 0.135 Uiso 1 1 calc R . . C94 C 0.6939(5) 0.5259(4) 0.1453(3) 0.1062(19) Uani 1 1 d . . . H94A H 0.7142 0.5934 0.1401 0.127 Uiso 1 1 calc R . . H94B H 0.6315 0.5193 0.1660 0.127 Uiso 1 1 calc R . . C99 C 0.4474(2) 0.75971(19) 0.39294(13) 0.0306(6) Uani 1 1 d . . . H99 H 0.4688 0.6951 0.3939 0.037 Uiso 1 1 calc R . . C69 C 0.3710(2) 0.7633(2) 0.33424(14) 0.0354(6) Uani 1 1 d . . . H69A H 0.3192 0.7118 0.3367 0.053 Uiso 1 1 calc R . . H69B H 0.4025 0.7571 0.2938 0.053 Uiso 1 1 calc R . . H69C H 0.3428 0.8233 0.3350 0.053 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 K1 0.0349(3) 0.0276(3) 0.0324(3) -0.0012(2) 0.0081(2) -0.0025(2) K2 0.0251(4) 0.0265(4) 0.0283(4) -0.0061(3) -0.0027(3) 0.0011(3) K3 0.0376(5) 0.0329(4) 0.0247(4) 0.0015(3) 0.0095(3) -0.0002(3) N1 0.0247(11) 0.0204(10) 0.0266(11) -0.0033(8) -0.0035(8) 0.0047(8) N3 0.0258(11) 0.0257(11) 0.0253(11) -0.0037(8) -0.0035(9) 0.0063(9) N4 0.0273(11) 0.0267(11) 0.0246(11) 0.0006(9) -0.0054(9) -0.0001(9) N2 0.0235(10) 0.0178(10) 0.0243(10) -0.0022(8) -0.0029(8) 0.0021(8) C30 0.0251(12) 0.0179(11) 0.0239(12) -0.0062(9) -0.0060(10) 0.0013(9) C19 0.0267(13) 0.0234(12) 0.0265(13) 0.0023(10) -0.0052(10) 0.0046(10) C35 0.0274(13) 0.0235(12) 0.0245(12) -0.0048(10) -0.0033(10) 0.0029(10) C3 0.0251(13) 0.0288(13) 0.0265(13) -0.0009(10) -0.0018(10) 0.0047(10) C34 0.0239(13) 0.0256(13) 0.0321(14) -0.0070(10) -0.0020(10) 0.0037(10) C32 0.0323(14) 0.0216(12) 0.0276(13) -0.0020(10) -0.0066(11) 0.0008(10) C1 0.0244(12) 0.0229(12) 0.0182(11) 0.0009(9) 0.0017(9) 0.0038(9) C18 0.0199(12) 0.0229(12) 0.0244(12) -0.0005(9) -0.0054(9) 0.0063(9) C27 0.0259(13) 0.0276(13) 0.0264(13) -0.0074(10) -0.0001(10) 0.0018(10) C31 0.0303(13) 0.0203(12) 0.0269(13) -0.0052(10) -0.0033(10) 0.0016(10) C23 0.0219(12) 0.0242(12) 0.0273(13) -0.0038(10) -0.0054(10) 0.0060(10) C21 0.0392(16) 0.0218(13) 0.0370(15) -0.0065(11) -0.0107(12) 0.0055(11) C33 0.0282(13) 0.0211(12) 0.0345(14) -0.0050(10) -0.0091(11) 0.0047(10) C36 0.0359(15) 0.0266(13) 0.0333(15) -0.0013(11) 0.0041(12) 0.0040(11) C6 0.0286(14) 0.0324(14) 0.0279(14) 0.0003(11) -0.0057(11) -0.0015(11) C22 0.0324(14) 0.0279(13) 0.0296(14) -0.0063(11) -0.0033(11) 0.0079(11) C5 0.0317(15) 0.0319(15) 0.0374(15) 0.0071(12) -0.0035(12) -0.0007(11) C2 0.0244(12) 0.0253(12) 0.0227(12) -0.0052(10) -0.0058(10) 0.0046(10) C20 0.0345(15) 0.0233(13) 0.0369(15) 0.0030(11) -0.0093(12) 0.0006(11) C7 0.0332(15) 0.0356(15) 0.0325(15) -0.0012(12) -0.0034(12) -0.0009(12) C4 0.0321(15) 0.0301(14) 0.0401(16) 0.0015(12) -0.0064(12) -0.0055(11) C8 0.0415(17) 0.0428(17) 0.0300(15) -0.0016(12) 0.0024(12) -0.0030(13) C10 0.0311(15) 0.0469(18) 0.0379(16) 0.0051(13) -0.0044(12) 0.0049(13) C25 0.0385(17) 0.0454(18) 0.0414(17) 0.0118(14) 0.0017(13) -0.0031(14) C11 0.0296(14) 0.0398(16) 0.0343(15) 0.0004(12) -0.0059(12) 0.0053(12) C12 0.0497(19) 0.0479(19) 0.0357(16) -0.0046(14) -0.0006(14) 0.0128(15) C9 0.0381(17) 0.0459(18) 0.0345(16) 0.0086(13) -0.0082(13) -0.0071(14) C15 0.0481(19) 0.056(2) 0.0346(16) -0.0032(14) -0.0080(14) 0.0249(16) C14 0.053(2) 0.048(2) 0.055(2) -0.0105(16) 0.0081(17) 0.0032(16) C13 0.040(2) 0.059(2) 0.126(4) -0.036(3) -0.010(2) 0.0090(18) N5 0.0237(11) 0.0299(11) 0.0210(10) -0.0005(8) 0.0053(8) 0.0009(9) N6 0.0234(11) 0.0296(11) 0.0202(10) -0.0024(8) 0.0046(8) -0.0005(8) C40 0.0198(12) 0.0289(13) 0.0208(12) -0.0021(10) 0.0048(9) 0.0061(10) C44 0.0227(13) 0.0390(15) 0.0257(13) -0.0008(11) 0.0023(10) -0.0004(11) C41 0.0215(12) 0.0333(14) 0.0200(12) -0.0015(10) 0.0051(9) 0.0042(10) C42 0.0274(13) 0.0332(14) 0.0174(12) -0.0013(10) 0.0064(10) -0.0005(10) C45 0.0332(15) 0.0485(18) 0.0313(15) 0.0041(13) -0.0026(12) -0.0009(13) C43 0.0298(14) 0.0338(14) 0.0199(12) -0.0029(10) 0.0054(10) -0.0024(11) C47 0.0457(17) 0.0318(15) 0.0273(14) -0.0023(11) 0.0094(12) 0.0021(12) C50 0.0347(15) 0.0342(14) 0.0262(13) 0.0002(11) 0.0072(11) 0.0067(11) C51 0.0325(15) 0.0456(17) 0.0321(15) 0.0012(12) 0.0080(12) 0.0063(13) C46 0.0332(15) 0.0443(17) 0.0237(13) -0.0051(12) 0.0010(11) -0.0062(12) C48 0.0342(14) 0.0331(14) 0.0219(12) -0.0038(10) 0.0091(11) 0.0005(11) C49 0.0410(17) 0.055(2) 0.0376(17) 0.0076(14) 0.0135(14) 0.0143(15) N7 0.0214(10) 0.0269(11) 0.0197(10) -0.0031(8) 0.0046(8) 0.0014(8) N8 0.0201(10) 0.0271(11) 0.0250(11) -0.0046(8) 0.0037(8) 0.0018(8) C53 0.0229(12) 0.0291(13) 0.0221(12) -0.0013(10) 0.0055(10) 0.0018(10) C54 0.0268(13) 0.0311(14) 0.0239(13) -0.0070(10) 0.0028(10) -0.0035(10) C52 0.0482(18) 0.0337(15) 0.0282(14) -0.0085(11) 0.0068(13) -0.0085(13) C55 0.0276(13) 0.0282(13) 0.0247(13) -0.0064(10) 0.0036(10) 0.0008(10) C60 0.0271(13) 0.0302(14) 0.0277(13) -0.0013(10) 0.0036(10) 0.0034(11) C57 0.0256(13) 0.0296(13) 0.0276(13) -0.0043(10) 0.0041(10) 0.0068(10) C59 0.0241(13) 0.0382(15) 0.0338(15) -0.0003(12) 0.0008(11) 0.0094(11) C56 0.0217(12) 0.0269(13) 0.0249(12) -0.0055(10) 0.0059(10) 0.0023(10) C62 0.0311(15) 0.0510(18) 0.0368(16) 0.0113(14) 0.0077(12) 0.0064(13) C58 0.0299(14) 0.0397(16) 0.0279(14) 0.0027(11) 0.0093(11) 0.0068(12) C70 0.0410(16) 0.0315(14) 0.0304(14) 0.0018(11) 0.0051(12) 0.0116(12) C65 0.0347(16) 0.0335(15) 0.0429(17) 0.0016(12) -0.0070(13) 0.0007(12) C61 0.0215(13) 0.0432(16) 0.0332(15) -0.0024(12) 0.0085(11) 0.0057(11) C67 0.0331(15) 0.0426(17) 0.0336(15) 0.0075(12) 0.0034(12) -0.0014(12) C64 0.0469(18) 0.0331(15) 0.0417(17) -0.0055(13) -0.0063(14) 0.0112(13) C63 0.0276(14) 0.0403(15) 0.0269(13) 0.0013(11) 0.0074(11) 0.0106(11) C66 0.0468(18) 0.0435(18) 0.0390(17) 0.0056(13) 0.0120(14) 0.0139(14) C71 0.0309(15) 0.0432(18) 0.0527(19) 0.0014(14) 0.0061(14) -0.0014(13) C68 0.0323(16) 0.0462(18) 0.059(2) -0.0112(15) 0.0146(14) 0.0005(13) C80 0.0240(13) 0.0277(13) 0.0284(13) -0.0001(10) 0.0031(10) -0.0021(10) C79 0.0234(12) 0.0268(13) 0.0217(12) -0.0013(10) 0.0061(10) -0.0051(10) C72 0.056(2) 0.0421(18) 0.0371(17) 0.0030(13) 0.0106(15) 0.0073(15) C73 0.051(2) 0.053(2) 0.060(2) 0.0236(17) 0.0172(17) 0.0139(16) C74 0.085(3) 0.068(3) 0.0304(17) 0.0045(16) -0.0113(18) 0.006(2) C75 0.056(2) 0.072(3) 0.0429(19) 0.0073(17) 0.0102(16) 0.0175(19) C76 0.053(2) 0.079(3) 0.084(3) -0.043(2) -0.010(2) 0.018(2) C77 0.087(3) 0.124(4) 0.035(2) 0.012(2) -0.003(2) -0.031(3) C78 0.111(4) 0.053(2) 0.082(3) 0.025(2) 0.027(3) 0.007(2) C84 0.0284(13) 0.0271(13) 0.0225(12) -0.0002(10) 0.0051(10) -0.0013(10) C83 0.0355(15) 0.0296(14) 0.0267(13) -0.0027(11) 0.0066(11) 0.0024(11) C81 0.0309(14) 0.0359(15) 0.0264(13) -0.0001(11) -0.0023(11) -0.0025(11) C82 0.0401(16) 0.0364(15) 0.0222(13) -0.0051(11) 0.0027(11) -0.0032(12) C85 0.0245(13) 0.0389(15) 0.0336(15) -0.0002(12) 0.0009(11) 0.0025(11) C87 0.0401(17) 0.0425(17) 0.0465(18) 0.0040(14) -0.0018(14) 0.0112(14) C86 0.0265(15) 0.056(2) 0.053(2) 0.0000(16) 0.0069(14) 0.0001(14) C88 0.0312(14) 0.0406(16) 0.0257(13) -0.0017(11) 0.0051(11) 0.0089(12) C90 0.0344(17) 0.096(3) 0.0366(18) 0.0110(18) 0.0024(14) 0.0065(18) C89 0.047(2) 0.081(3) 0.081(3) 0.048(2) -0.004(2) 0.005(2) O1 0.099(3) 0.099(3) 0.105(3) -0.022(2) 0.015(2) -0.016(2) C91 0.089(4) 0.162(6) 0.081(4) -0.050(4) 0.037(3) -0.057(4) C92 0.101(4) 0.095(4) 0.091(4) -0.023(3) 0.035(3) -0.045(3) C93 0.127(5) 0.100(4) 0.098(4) -0.002(3) 0.012(4) -0.049(4) C94 0.116(5) 0.076(4) 0.122(5) 0.000(3) 0.013(4) -0.014(3) C99 0.0321(14) 0.0277(13) 0.0318(14) 0.0052(11) 0.0007(11) 0.0026(11) C69 0.0411(16) 0.0357(15) 0.0281(14) 0.0031(11) 0.0003(12) -0.0010(12) _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 K1 N5 2.803(2) . ? K1 C53 2.862(3) . ? K1 C3 2.953(3) . ? K2 N2 3.035(2) . ? K2 N2 3.035(2) 2_666 ? K2 C34 3.248(2) 2_666 ? K2 C34 3.248(2) . ? K2 C33 3.256(2) 2_666 ? K2 C33 3.256(2) . ? K2 C35 3.260(2) 2_666 ? K2 C35 3.260(2) . ? K2 C32 3.279(2) 2_666 ? K2 C32 3.279(2) . ? K2 C30 3.307(2) 2_666 ? K2 C30 3.307(2) . ? K3 N6 2.946(2) . ? K3 N6 2.946(2) 2_675 ? K3 C84 3.146(2) . ? K3 C84 3.146(2) 2_675 ? K3 C83 3.276(3) 2_675 ? K3 C83 3.276(3) . ? K3 C79 3.303(2) . ? K3 C79 3.303(2) 2_675 ? N1 C1 1.314(3) . ? N1 C30 1.406(3) . ? N3 C5 1.366(3) . ? N3 C3 1.373(3) . ? N3 C2 1.462(3) . ? N4 C3 1.372(3) . ? N4 C4 1.397(4) . ? N4 C6 1.441(3) . ? N2 C1 1.332(3) . ? N2 C18 1.410(3) . ? C30 C35 1.414(4) . ? C30 C31 1.420(4) . ? C19 C20 1.400(4) . ? C19 C18 1.421(4) . ? C19 C99 1.517(4) . ? C35 C34 1.394(4) . ? C35 C70 1.515(4) . ? C34 C33 1.382(4) . ? C34 H34 0.9500 . ? C32 C33 1.382(4) . ? C32 C31 1.398(4) . ? C32 H32 0.9500 . ? C1 C2 1.531(3) . ? C18 C23 1.416(4) . ? C27 C67 1.523(4) . ? C27 C23 1.524(4) . ? C27 C68 1.527(4) . ? C27 H27 1.0000 . ? C31 C36 1.516(4) . ? C23 C22 1.397(3) . ? C21 C20 1.377(4) . ? C21 C22 1.381(4) . ? C21 H21 0.9500 . ? C33 H33 0.9500 . ? C36 C72 1.533(4) . ? C36 C71 1.535(4) . ? C36 H36 1.0000 . ? C6 C11 1.400(4) . ? C6 C7 1.403(4) . ? C22 H22 0.9500 . ? C5 C4 1.347(4) . ? C5 H5 0.9500 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C20 H20 0.9500 . ? C7 C8 1.388(4) . ? C7 C12 1.522(4) . ? C4 H4 0.9500 . ? C8 C9 1.396(5) . ? C8 H8 0.9500 . ? C10 C9 1.380(4) . ? C10 C11 1.401(4) . ? C10 H10 0.9500 . ? C25 C99 1.529(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C11 C15 1.526(4) . ? C12 C14 1.515(4) . ? C12 C13 1.533(5) . ? C12 H12 1.0000 . ? C9 H9 0.9500 . ? C15 C75 1.513(5) . ? C15 C76 1.525(5) . ? C15 H15 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? N5 C40 1.328(3) . ? N5 C79 1.417(3) . ? N6 C40 1.327(3) . ? N6 C42 1.417(3) . ? C40 C41 1.536(3) . ? C44 C43 1.526(4) . ? C44 C45 1.531(4) . ? C44 C49 1.532(4) . ? C44 H44 1.0000 . ? C41 N7 1.464(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C48 1.418(4) . ? C42 C43 1.419(4) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C43 C46 1.394(4) . ? C47 C52 1.379(4) . ? C47 C48 1.398(4) . ? C47 H47 0.9500 . ? C50 C48 1.522(4) . ? C50 C66 1.534(4) . ? C50 C51 1.536(4) . ? C50 H50 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C46 C52 1.380(4) . ? C46 H46 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? N7 C53 1.363(3) . ? N7 C54 1.386(3) . ? N8 C53 1.366(3) . ? N8 C55 1.392(3) . ? N8 C56 1.440(3) . ? C54 C55 1.346(4) . ? C54 H54 0.9500 . ? C52 H52 0.9500 . ? C55 H55 0.9500 . ? C60 C59 1.393(4) . ? C60 C56 1.395(4) . ? C60 C62 1.516(4) . ? C57 C58 1.391(4) . ? C57 C56 1.404(4) . ? C57 C63 1.522(4) . ? C59 C61 1.384(4) . ? C59 H59 0.9500 . ? C62 C77 1.498(5) . ? C62 C78 1.545(5) . ? C62 H62 1.0000 . ? C58 C61 1.379(4) . ? C58 H58 0.9500 . ? C70 C74 1.520(4) . ? C70 C73 1.524(4) . ? C70 H70 1.0000 . ? C65 C63 1.525(4) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C61 H61 0.9500 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C64 C63 1.525(4) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C63 H63 1.0000 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C80 C81 1.400(4) . ? C80 C79 1.409(4) . ? C80 C85 1.516(4) . ? C79 C84 1.417(4) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C84 C83 1.397(4) . ? C84 C88 1.519(4) . ? C83 C82 1.385(4) . ? C83 H83 0.9500 . ? C81 C82 1.378(4) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C85 C86 1.532(4) . ? C85 C87 1.534(4) . ? C85 H85 1.0000 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C88 C89 1.503(5) . ? C88 C90 1.517(4) . ? C88 H88 1.0000 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? O1 C91 1.435(7) . ? O1 C94 1.445(7) . ? C91 C92 1.478(8) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C93 1.545(9) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.491(8) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C99 C69 1.541(4) . ? C99 H99 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 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 N5 K1 C53 76.94(7) . . ? N5 K1 C3 147.02(7) . . ? C53 K1 C3 127.30(7) . . ? N2 K2 N2 180.000(1) . 2_666 ? N2 K2 C34 91.62(6) . 2_666 ? N2 K2 C34 88.38(6) 2_666 2_666 ? N2 K2 C34 88.38(6) . . ? N2 K2 C34 91.62(6) 2_666 . ? C34 K2 C34 180.0 2_666 . ? N2 K2 C33 78.77(6) . 2_666 ? N2 K2 C33 101.23(6) 2_666 2_666 ? C34 K2 C33 24.53(7) 2_666 2_666 ? C34 K2 C33 155.47(7) . 2_666 ? N2 K2 C33 101.23(6) . . ? N2 K2 C33 78.77(6) 2_666 . ? C34 K2 C33 155.47(7) 2_666 . ? C34 K2 C33 24.53(7) . . ? C33 K2 C33 180.0 2_666 . ? N2 K2 C35 116.29(6) . 2_666 ? N2 K2 C35 63.71(6) 2_666 2_666 ? C34 K2 C35 24.74(6) 2_666 2_666 ? C34 K2 C35 155.26(6) . 2_666 ? C33 K2 C35 43.66(6) 2_666 2_666 ? C33 K2 C35 136.34(6) . 2_666 ? N2 K2 C35 63.71(6) . . ? N2 K2 C35 116.29(6) 2_666 . ? C34 K2 C35 155.26(6) 2_666 . ? C34 K2 C35 24.74(6) . . ? C33 K2 C35 136.34(6) 2_666 . ? C33 K2 C35 43.66(6) . . ? C35 K2 C35 180.0 2_666 . ? N2 K2 C32 90.03(6) . 2_666 ? N2 K2 C32 89.97(6) 2_666 2_666 ? C34 K2 C32 42.86(7) 2_666 2_666 ? C34 K2 C32 137.14(7) . 2_666 ? C33 K2 C32 24.42(7) 2_666 2_666 ? C33 K2 C32 155.58(7) . 2_666 ? C35 K2 C32 50.46(6) 2_666 2_666 ? C35 K2 C32 129.54(6) . 2_666 ? N2 K2 C32 89.97(6) . . ? N2 K2 C32 90.03(6) 2_666 . ? C34 K2 C32 137.14(7) 2_666 . ? C34 K2 C32 42.86(7) . . ? C33 K2 C32 155.58(7) 2_666 . ? C33 K2 C32 24.42(7) . . ? C35 K2 C32 129.54(6) 2_666 . ? C35 K2 C32 50.46(6) . . ? C32 K2 C32 180.0 2_666 . ? N2 K2 C30 129.30(6) . 2_666 ? N2 K2 C30 50.70(5) 2_666 2_666 ? C34 K2 C30 43.31(6) 2_666 2_666 ? C34 K2 C30 136.69(6) . 2_666 ? C33 K2 C30 50.58(6) 2_666 2_666 ? C33 K2 C30 129.42(6) . 2_666 ? C35 K2 C30 24.85(6) 2_666 2_666 ? C35 K2 C30 155.15(6) . 2_666 ? C32 K2 C30 43.11(6) 2_666 2_666 ? C32 K2 C30 136.89(6) . 2_666 ? N2 K2 C30 50.70(5) . . ? N2 K2 C30 129.30(6) 2_666 . ? C34 K2 C30 136.69(6) 2_666 . ? C34 K2 C30 43.31(6) . . ? C33 K2 C30 129.42(6) 2_666 . ? C33 K2 C30 50.58(6) . . ? C35 K2 C30 155.15(6) 2_666 . ? C35 K2 C30 24.85(6) . . ? C32 K2 C30 136.89(6) 2_666 . ? C32 K2 C30 43.11(6) . . ? C30 K2 C30 180.0 2_666 . ? N6 K3 N6 180.0 . 2_675 ? N6 K3 C84 68.96(6) . . ? N6 K3 C84 111.04(6) 2_675 . ? N6 K3 C84 111.04(6) . 2_675 ? N6 K3 C84 68.96(6) 2_675 2_675 ? C84 K3 C84 180.00(8) . 2_675 ? N6 K3 C83 86.88(6) . 2_675 ? N6 K3 C83 93.12(6) 2_675 2_675 ? C84 K3 C83 154.98(6) . 2_675 ? C84 K3 C83 25.02(6) 2_675 2_675 ? N6 K3 C83 93.12(6) . . ? N6 K3 C83 86.88(6) 2_675 . ? C84 K3 C83 25.02(6) . . ? C84 K3 C83 154.98(6) 2_675 . ? C83 K3 C83 180.0 2_675 . ? N6 K3 C79 52.26(6) . . ? N6 K3 C79 127.74(6) 2_675 . ? C84 K3 C79 25.23(6) . . ? C84 K3 C79 154.77(6) 2_675 . ? C83 K3 C79 136.76(6) 2_675 . ? C83 K3 C79 43.24(6) . . ? N6 K3 C79 127.74(6) . 2_675 ? N6 K3 C79 52.26(6) 2_675 2_675 ? C84 K3 C79 154.77(7) . 2_675 ? C84 K3 C79 25.23(6) 2_675 2_675 ? C83 K3 C79 43.24(6) 2_675 2_675 ? C83 K3 C79 136.76(6) . 2_675 ? C79 K3 C79 180.0 . 2_675 ? C1 N1 C30 116.3(2) . . ? C5 N3 C3 113.2(2) . . ? C5 N3 C2 124.0(2) . . ? C3 N3 C2 122.8(2) . . ? C3 N4 C4 112.6(2) . . ? C3 N4 C6 123.0(2) . . ? C4 N4 C6 123.5(2) . . ? C1 N2 C18 120.0(2) . . ? C1 N2 K2 127.50(15) . . ? C18 N2 K2 111.89(14) . . ? N1 C30 C35 120.6(2) . . ? N1 C30 C31 119.5(2) . . ? C35 C30 C31 119.9(2) . . ? N1 C30 K2 119.25(14) . . ? C35 C30 K2 75.70(14) . . ? C31 C30 K2 78.57(14) . . ? C20 C19 C18 119.0(2) . . ? C20 C19 C99 121.1(2) . . ? C18 C19 C99 119.8(2) . . ? C34 C35 C30 119.0(2) . . ? C34 C35 C70 121.1(2) . . ? C30 C35 C70 119.8(2) . . ? C34 C35 K2 77.17(14) . . ? C30 C35 K2 79.46(14) . . ? C70 C35 K2 115.79(16) . . ? N4 C3 N3 101.5(2) . . ? N4 C3 K1 112.25(16) . . ? N3 C3 K1 146.26(17) . . ? C33 C34 C35 121.5(3) . . ? C33 C34 K2 78.04(15) . . ? C35 C34 K2 78.09(14) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? K2 C34 H34 115.1 . . ? C33 C32 C31 121.9(2) . . ? C33 C32 K2 76.86(15) . . ? C31 C32 K2 79.89(14) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? K2 C32 H32 114.5 . . ? N1 C1 N2 126.0(2) . . ? N1 C1 C2 114.6(2) . . ? N2 C1 C2 119.4(2) . . ? N2 C18 C23 120.7(2) . . ? N2 C18 C19 119.8(2) . . ? C23 C18 C19 119.2(2) . . ? C67 C27 C23 111.5(2) . . ? C67 C27 C68 109.4(2) . . ? C23 C27 C68 113.8(2) . . ? C67 C27 H27 107.3 . . ? C23 C27 H27 107.3 . . ? C68 C27 H27 107.3 . . ? C32 C31 C30 118.3(2) . . ? C32 C31 C36 122.3(2) . . ? C30 C31 C36 119.4(2) . . ? C32 C31 K2 75.72(15) . . ? C30 C31 K2 76.72(14) . . ? C36 C31 K2 120.14(16) . . ? C22 C23 C18 119.4(2) . . ? C22 C23 C27 120.1(2) . . ? C18 C23 C27 120.4(2) . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C34 C33 C32 119.3(2) . . ? C34 C33 K2 77.43(14) . . ? C32 C33 K2 78.72(14) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? K2 C33 H33 114.1 . . ? C31 C36 C72 114.1(2) . . ? C31 C36 C71 110.1(2) . . ? C72 C36 C71 110.3(3) . . ? C31 C36 H36 107.4 . . ? C72 C36 H36 107.4 . . ? C71 C36 H36 107.4 . . ? C11 C6 C7 122.7(3) . . ? C11 C6 N4 118.5(2) . . ? C7 C6 N4 118.8(2) . . ? C21 C22 C23 120.9(3) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C4 C5 N3 107.1(2) . . ? C4 C5 H5 126.4 . . ? N3 C5 H5 126.4 . . ? N3 C2 C1 114.6(2) . . ? N3 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? N3 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C8 C7 C6 117.3(3) . . ? C8 C7 C12 120.4(3) . . ? C6 C7 C12 122.2(3) . . ? C5 C4 N4 105.6(2) . . ? C5 C4 H4 127.2 . . ? N4 C4 H4 127.2 . . ? C7 C8 C9 121.5(3) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C9 C10 C11 121.0(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C99 C25 H25A 109.5 . . ? C99 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C99 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C6 C11 C10 117.6(3) . . ? C6 C11 C15 122.2(3) . . ? C10 C11 C15 120.2(3) . . ? C14 C12 C7 113.2(3) . . ? C14 C12 C13 109.0(3) . . ? C7 C12 C13 110.0(3) . . ? C14 C12 H12 108.1 . . ? C7 C12 H12 108.1 . . ? C13 C12 H12 108.1 . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C75 C15 C76 111.4(3) . . ? C75 C15 C11 112.3(3) . . ? C76 C15 C11 110.6(3) . . ? C75 C15 H15 107.4 . . ? C76 C15 H15 107.4 . . ? C11 C15 H15 107.4 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C40 N5 C79 117.6(2) . . ? C40 N5 K1 119.39(15) . . ? C79 N5 K1 118.61(15) . . ? C40 N6 C42 118.5(2) . . ? C40 N6 K3 126.47(16) . . ? C42 N6 K3 112.25(14) . . ? N6 C40 N5 125.9(2) . . ? N6 C40 C41 122.4(2) . . ? N5 C40 C41 111.7(2) . . ? C43 C44 C45 113.3(2) . . ? C43 C44 C49 110.5(2) . . ? C45 C44 C49 110.0(2) . . ? C43 C44 H44 107.6 . . ? C45 C44 H44 107.6 . . ? C49 C44 H44 107.6 . . ? N7 C41 C40 115.8(2) . . ? N7 C41 H41A 108.3 . . ? C40 C41 H41A 108.3 . . ? N7 C41 H41B 108.3 . . ? C40 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? N6 C42 C48 119.1(2) . . ? N6 C42 C43 121.6(2) . . ? C48 C42 C43 119.2(2) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 C43 C42 119.2(3) . . ? C46 C43 C44 119.3(2) . . ? C42 C43 C44 121.5(2) . . ? C52 C47 C48 121.3(3) . . ? C52 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C48 C50 C66 114.2(2) . . ? C48 C50 C51 112.4(2) . . ? C66 C50 C51 107.9(2) . . ? C48 C50 H50 107.3 . . ? C66 C50 H50 107.3 . . ? C51 C50 H50 107.3 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C52 C46 C43 121.3(3) . . ? C52 C46 H46 119.4 . . ? C43 C46 H46 119.4 . . ? C47 C48 C42 119.1(3) . . ? C47 C48 C50 120.3(3) . . ? C42 C48 C50 120.5(2) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C53 N7 C54 113.1(2) . . ? C53 N7 C41 122.8(2) . . ? C54 N7 C41 123.8(2) . . ? C53 N8 C55 113.1(2) . . ? C53 N8 C56 123.0(2) . . ? C55 N8 C56 123.4(2) . . ? N7 C53 N8 101.7(2) . . ? N7 C53 K1 112.97(16) . . ? N8 C53 K1 145.21(17) . . ? C55 C54 N7 106.5(2) . . ? C55 C54 H54 126.8 . . ? N7 C54 H54 126.8 . . ? C47 C52 C46 119.9(3) . . ? C47 C52 H52 120.1 . . ? C46 C52 H52 120.1 . . ? C54 C55 N8 105.7(2) . . ? C54 C55 H55 127.1 . . ? N8 C55 H55 127.1 . . ? C59 C60 C56 117.7(2) . . ? C59 C60 C62 120.3(2) . . ? C56 C60 C62 122.0(2) . . ? C58 C57 C56 117.0(2) . . ? C58 C57 C63 120.5(2) . . ? C56 C57 C63 122.5(2) . . ? C61 C59 C60 121.1(3) . . ? C61 C59 H59 119.4 . . ? C60 C59 H59 119.4 . . ? C60 C56 C57 122.7(2) . . ? C60 C56 N8 119.5(2) . . ? C57 C56 N8 117.8(2) . . ? C77 C62 C60 112.6(3) . . ? C77 C62 C78 111.6(4) . . ? C60 C62 C78 110.2(3) . . ? C77 C62 H62 107.4 . . ? C60 C62 H62 107.4 . . ? C78 C62 H62 107.4 . . ? C61 C58 C57 121.9(3) . . ? C61 C58 H58 119.1 . . ? C57 C58 H58 119.1 . . ? C35 C70 C74 109.6(3) . . ? C35 C70 C73 113.7(2) . . ? C74 C70 C73 110.8(3) . . ? C35 C70 H70 107.5 . . ? C74 C70 H70 107.5 . . ? C73 C70 H70 107.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C58 C61 C59 119.7(2) . . ? C58 C61 H61 120.1 . . ? C59 C61 H61 120.1 . . ? C27 C67 H67A 109.5 . . ? C27 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C27 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C57 C63 C64 112.6(2) . . ? C57 C63 C65 110.1(2) . . ? C64 C63 C65 111.2(2) . . ? C57 C63 H63 107.6 . . ? C64 C63 H63 107.6 . . ? C65 C63 H63 107.6 . . ? C50 C66 H66A 109.5 . . ? C50 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C50 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C36 C71 H71A 109.5 . . ? C36 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C36 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C27 C68 H68A 109.5 . . ? C27 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C27 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C81 C80 C79 118.8(2) . . ? C81 C80 C85 120.0(2) . . ? C79 C80 C85 121.2(2) . . ? C80 C79 C84 119.8(2) . . ? C80 C79 N5 121.1(2) . . ? C84 C79 N5 118.8(2) . . ? C80 C79 K3 88.85(15) . . ? C84 C79 K3 71.18(14) . . ? N5 C79 K3 114.80(15) . . ? C36 C72 H72A 109.5 . . ? C36 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C36 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C70 C74 H74A 109.5 . . ? C70 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C70 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C15 C75 H75A 109.5 . . ? C15 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C15 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C15 C76 H76A 109.5 . . ? C15 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C15 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C62 C77 H77A 109.5 . . ? C62 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C62 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C62 C78 H78A 109.5 . . ? C62 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C62 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C83 C84 C79 119.0(2) . . ? C83 C84 C88 120.5(2) . . ? C79 C84 C88 120.5(2) . . ? C83 C84 K3 82.72(15) . . ? C79 C84 K3 83.59(15) . . ? C88 C84 K3 104.99(16) . . ? C82 C83 C84 121.4(3) . . ? C82 C83 K3 90.19(17) . . ? C84 C83 K3 72.26(15) . . ? C82 C83 H83 119.3 . . ? C84 C83 H83 119.3 . . ? K3 C83 H83 107.9 . . ? C82 C81 C80 121.7(3) . . ? C82 C81 H81 119.1 . . ? C80 C81 H81 119.1 . . ? C81 C82 C83 119.3(2) . . ? C81 C82 H82 120.3 . . ? C83 C82 H82 120.3 . . ? C80 C85 C86 110.9(2) . . ? C80 C85 C87 112.5(2) . . ? C86 C85 C87 109.8(2) . . ? C80 C85 H85 107.8 . . ? C86 C85 H85 107.8 . . ? C87 C85 H85 107.8 . . ? 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 . . ? 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 . . ? C89 C88 C90 110.5(3) . . ? C89 C88 C84 111.2(3) . . ? C90 C88 C84 114.0(2) . . ? C89 C88 H88 106.9 . . ? C90 C88 H88 106.9 . . ? C84 C88 H88 106.9 . . ? C88 C90 H90A 109.5 . . ? C88 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C88 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C88 C89 H89A 109.5 . . ? C88 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C88 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C91 O1 C94 110.3(5) . . ? O1 C91 C92 105.5(6) . . ? O1 C91 H91A 110.6 . . ? C92 C91 H91A 110.6 . . ? O1 C91 H91B 110.6 . . ? C92 C91 H91B 110.6 . . ? H91A C91 H91B 108.8 . . ? C91 C92 C93 102.9(5) . . ? C91 C92 H92A 111.2 . . ? C93 C92 H92A 111.2 . . ? C91 C92 H92B 111.2 . . ? C93 C92 H92B 111.2 . . ? H92A C92 H92B 109.1 . . ? C94 C93 C92 101.8(5) . . ? C94 C93 H93A 111.4 . . ? C92 C93 H93A 111.4 . . ? C94 C93 H93B 111.4 . . ? C92 C93 H93B 111.4 . . ? H93A C93 H93B 109.3 . . ? O1 C94 C93 105.9(5) . . ? O1 C94 H94A 110.6 . . ? C93 C94 H94A 110.6 . . ? O1 C94 H94B 110.6 . . ? C93 C94 H94B 110.6 . . ? H94A C94 H94B 108.7 . . ? C19 C99 C25 114.4(2) . . ? C19 C99 C69 111.1(2) . . ? C25 C99 C69 108.7(2) . . ? C19 C99 H99 107.5 . . ? C25 C99 H99 107.5 . . ? C69 C99 H99 107.5 . . ? C99 C69 H69A 109.5 . . ? C99 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C99 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.638 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.065 data_complex7 _database_code_depnum_ccdc_archive 'CCDC 892660' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H56 Ag Cl N4' _chemical_formula_weight 748.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2894(7) _cell_length_b 12.4817(13) _cell_length_c 16.3801(17) _cell_angle_alpha 80.103(4) _cell_angle_beta 86.108(5) _cell_angle_gamma 74.035(5) _cell_volume 1992.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7655 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8586 _exptl_absorpt_correction_T_max 0.9646 _exptl_absorpt_process_details ? _exptl_special_details ; 'SADABS2007/2' ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; 'Bruker-Nonius 95mm CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39376 _diffrn_reflns_av_R_equivalents 0.2321 _diffrn_reflns_av_sigmaI/netI 0.3277 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.80 _reflns_number_total 8364 _reflns_number_gt 3367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) and COLLECT' ; _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8364 _refine_ls_number_parameters 441 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2433 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 Ag1 Ag 0.35757(5) 0.10224(5) 0.74820(3) 0.0381(2) Uani 1 1 d . . . Cl1 Cl 0.57875(15) 0.08291(17) 0.78215(11) 0.0521(6) Uani 1 1 d . . . N1 N 0.1226(4) 0.1027(4) 0.6424(3) 0.0290(13) Uani 1 1 d . . . N2 N 0.0453(4) 0.1369(4) 0.7624(3) 0.0261(13) Uani 1 1 d . . . N3 N -0.0624(5) 0.3212(5) 0.9211(3) 0.0277(13) Uani 1 1 d D . . N4 N -0.0780(4) 0.3517(5) 0.7750(3) 0.0269(13) Uani 1 1 d . . . C1 C 0.2095(5) 0.0742(6) 0.5711(4) 0.0284(16) Uani 1 1 d . . . C2 C 0.2513(6) 0.1586(6) 0.5187(4) 0.0343(17) Uani 1 1 d . . . C3 C 0.3226(6) 0.1294(6) 0.4472(4) 0.0384(18) Uani 1 1 d . . . H3 H 0.3536 0.1847 0.4098 0.046 Uiso 1 1 calc R . . C4 C 0.3492(6) 0.0206(7) 0.4295(4) 0.0439(19) Uani 1 1 d . . . H4 H 0.3958 0.0028 0.3794 0.053 Uiso 1 1 calc R . . C5 C 0.3086(6) -0.0619(6) 0.4841(4) 0.0416(19) Uani 1 1 d . . . H5 H 0.3290 -0.1366 0.4719 0.050 Uiso 1 1 calc R . . C6 C 0.2379(6) -0.0367(6) 0.5569(4) 0.0306(16) Uani 1 1 d . . . C7 C 0.2245(6) 0.2781(6) 0.5363(4) 0.0372(18) Uani 1 1 d . . . H7 H 0.1735 0.2825 0.5903 0.045 Uiso 1 1 calc R . . C8 C 0.3555(6) 0.3097(6) 0.5443(4) 0.052(2) Uani 1 1 d . . . H8A H 0.4120 0.2535 0.5859 0.078 Uiso 1 1 calc R . . H8B H 0.3345 0.3842 0.5614 0.078 Uiso 1 1 calc R . . H8C H 0.4041 0.3116 0.4907 0.078 Uiso 1 1 calc R . . C9 C 0.1375(7) 0.3626(6) 0.4698(5) 0.059(2) Uani 1 1 d . . . H9A H 0.1830 0.3567 0.4155 0.089 Uiso 1 1 calc R . . H9B H 0.1238 0.4392 0.4819 0.089 Uiso 1 1 calc R . . H9C H 0.0498 0.3462 0.4691 0.089 Uiso 1 1 calc R . . C10 C 0.1996(6) -0.1297(5) 0.6190(4) 0.0344(17) Uani 1 1 d . . . H10 H 0.1563 -0.0955 0.6684 0.041 Uiso 1 1 calc R . . C11 C 0.0955(7) -0.1770(6) 0.5834(4) 0.055(2) Uani 1 1 d . . . H11A H 0.1380 -0.2178 0.5382 0.082 Uiso 1 1 calc R . . H11B H 0.0185 -0.1146 0.5622 0.082 Uiso 1 1 calc R . . H11C H 0.0640 -0.2287 0.6272 0.082 Uiso 1 1 calc R . . C12 C 0.3236(7) -0.2231(7) 0.6483(5) 0.062(2) Uani 1 1 d . . . H12A H 0.3677 -0.2592 0.6013 0.093 Uiso 1 1 calc R . . H12B H 0.2967 -0.2794 0.6905 0.093 Uiso 1 1 calc R . . H12C H 0.3868 -0.1914 0.6722 0.093 Uiso 1 1 calc R . . C13 C 0.1612(6) 0.1160(5) 0.7161(4) 0.0244(15) Uani 1 1 d . . . C14 C -0.0161(6) 0.1143(5) 0.6430(4) 0.0322(17) Uani 1 1 d . . . H14 H -0.0666 0.1074 0.5987 0.039 Uiso 1 1 calc R . . C15 C -0.0643(6) 0.1371(5) 0.7174(4) 0.0295(16) Uani 1 1 d . . . H15 H -0.1559 0.1508 0.7361 0.035 Uiso 1 1 calc R . . C16 C 0.0337(6) 0.1654(5) 0.8448(4) 0.0310(17) Uani 1 1 d . . . H16A H 0.1251 0.1498 0.8673 0.037 Uiso 1 1 calc R . . H16B H -0.0160 0.1176 0.8814 0.037 Uiso 1 1 calc R . . C17 C -0.0406(5) 0.2895(5) 0.8441(4) 0.0252(16) Uani 1 1 d . . . C18 C -0.0178(6) 0.2464(5) 0.9969(4) 0.0267(16) Uani 1 1 d . . . C19 C -0.1109(6) 0.1957(5) 1.0443(4) 0.0293(16) Uani 1 1 d . . . C20 C -0.0691(6) 0.1291(6) 1.1205(4) 0.0366(18) Uani 1 1 d . . . H20 H -0.1313 0.0966 1.1546 0.044 Uiso 1 1 calc R . . C21 C 0.0616(6) 0.1096(5) 1.1470(4) 0.0335(17) Uani 1 1 d . . . H21 H 0.0890 0.0642 1.1989 0.040 Uiso 1 1 calc R . . C22 C 0.1520(6) 0.1572(5) 1.0971(4) 0.0304(16) Uani 1 1 d . . . H22 H 0.2425 0.1409 1.1146 0.036 Uiso 1 1 calc R . . C23 C 0.1154(5) 0.2270(5) 1.0231(4) 0.0288(16) Uani 1 1 d . . . C24 C -0.2531(5) 0.2112(6) 1.0155(4) 0.0356(18) Uani 1 1 d . . . H24 H -0.2585 0.2480 0.9561 0.043 Uiso 1 1 calc R . . C25 C -0.3583(6) 0.2887(7) 1.0656(5) 0.063(3) Uani 1 1 d . . . H25A H -0.3605 0.2514 1.1232 0.095 Uiso 1 1 calc R . . H25B H -0.4477 0.3046 1.0416 0.095 Uiso 1 1 calc R . . H25C H -0.3340 0.3597 1.0638 0.095 Uiso 1 1 calc R . . C26 C -0.2833(6) 0.0968(6) 1.0206(5) 0.055(2) Uani 1 1 d . . . H26A H -0.2046 0.0432 1.0001 0.082 Uiso 1 1 calc R . . H26B H -0.3616 0.1056 0.9868 0.082 Uiso 1 1 calc R . . H26C H -0.3031 0.0685 1.0784 0.082 Uiso 1 1 calc R . . C27 C 0.2152(6) 0.2821(5) 0.9716(4) 0.0333(17) Uani 1 1 d . . . H27 H 0.1849 0.3012 0.9129 0.040 Uiso 1 1 calc R . . C28 C 0.2145(6) 0.3928(6) 1.0010(4) 0.0405(19) Uani 1 1 d . . . H28A H 0.1230 0.4439 0.9967 0.061 Uiso 1 1 calc R . . H28B H 0.2773 0.4284 0.9663 0.061 Uiso 1 1 calc R . . H28C H 0.2426 0.3766 1.0588 0.061 Uiso 1 1 calc R . . C29 C 0.3568(6) 0.2027(6) 0.9731(4) 0.046(2) Uani 1 1 d . . . H29A H 0.3898 0.1839 1.0299 0.069 Uiso 1 1 calc R . . H29B H 0.4173 0.2395 0.9371 0.069 Uiso 1 1 calc R . . H29C H 0.3547 0.1334 0.9533 0.069 Uiso 1 1 calc R . . C30 C -0.1531(6) 0.4663(6) 0.7750(4) 0.0285(16) Uani 1 1 d . . . C31 C -0.2956(6) 0.4921(6) 0.7688(4) 0.0321(17) Uani 1 1 d . . . C32 C -0.3685(6) 0.6061(6) 0.7627(4) 0.0371(18) Uani 1 1 d . . . H32 H -0.4642 0.6257 0.7599 0.045 Uiso 1 1 calc R . . C33 C -0.3046(6) 0.6907(6) 0.7608(4) 0.0354(18) Uani 1 1 d . . . H33 H -0.3559 0.7673 0.7564 0.042 Uiso 1 1 calc R . . C34 C -0.1653(6) 0.6626(6) 0.7652(4) 0.0326(17) Uani 1 1 d . . . H34 H -0.1216 0.7210 0.7628 0.039 Uiso 1 1 calc R . . C35 C -0.0883(6) 0.5522(6) 0.7729(4) 0.0265(15) Uani 1 1 d . . . C36 C -0.3631(6) 0.3996(6) 0.7632(4) 0.0403(19) Uani 1 1 d . . . H36 H -0.3079 0.3283 0.7959 0.048 Uiso 1 1 calc R . . C37 C -0.5069(6) 0.4216(6) 0.7997(5) 0.069(3) Uani 1 1 d . . . H37A H -0.5059 0.4311 0.8577 0.104 Uiso 1 1 calc R . . H37B H -0.5428 0.3574 0.7964 0.104 Uiso 1 1 calc R . . H37C H -0.5643 0.4903 0.7682 0.104 Uiso 1 1 calc R . . C38 C -0.3597(7) 0.3804(7) 0.6727(5) 0.063(2) Uani 1 1 d . . . H38A H -0.4140 0.4485 0.6389 0.094 Uiso 1 1 calc R . . H38B H -0.3969 0.3167 0.6700 0.094 Uiso 1 1 calc R . . H38C H -0.2661 0.3636 0.6515 0.094 Uiso 1 1 calc R . . C39 C 0.0666(5) 0.5182(5) 0.7770(4) 0.0320(17) Uani 1 1 d . . . H39 H 0.0936 0.4465 0.8173 0.038 Uiso 1 1 calc R . . C40 C 0.1321(6) 0.4937(6) 0.6931(4) 0.0425(19) Uani 1 1 d . . . H40A H 0.1113 0.5633 0.6526 0.064 Uiso 1 1 calc R . . H40B H 0.0968 0.4370 0.6742 0.064 Uiso 1 1 calc R . . H40C H 0.2303 0.4649 0.6989 0.064 Uiso 1 1 calc R . . C41 C 0.1188(6) 0.6061(6) 0.8095(4) 0.0395(18) Uani 1 1 d . . . H41A H 0.1018 0.6755 0.7687 0.059 Uiso 1 1 calc R . . H41B H 0.2162 0.5767 0.8186 0.059 Uiso 1 1 calc R . . H41C H 0.0719 0.6225 0.8618 0.059 Uiso 1 1 calc R . . H1 H -0.112(5) 0.3998(18) 0.924(4) 0.07(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0289(3) 0.0477(4) 0.0368(4) -0.0101(3) -0.0019(2) -0.0067(2) Cl1 0.0295(9) 0.0757(16) 0.0523(13) -0.0197(11) -0.0032(8) -0.0100(10) N1 0.026(3) 0.039(4) 0.024(3) -0.010(3) 0.001(2) -0.008(3) N2 0.025(3) 0.031(4) 0.021(3) -0.006(3) 0.002(2) -0.005(2) N3 0.028(3) 0.027(4) 0.028(4) -0.009(3) -0.002(2) -0.005(3) N4 0.023(3) 0.030(4) 0.027(4) -0.001(3) -0.007(2) -0.007(3) C1 0.024(3) 0.029(5) 0.030(4) -0.007(4) -0.003(3) -0.002(3) C2 0.032(4) 0.044(5) 0.030(4) -0.008(4) 0.001(3) -0.014(4) C3 0.041(4) 0.035(5) 0.037(5) 0.002(4) -0.001(3) -0.010(4) C4 0.047(4) 0.052(6) 0.028(5) -0.006(4) 0.008(3) -0.006(4) C5 0.038(4) 0.043(5) 0.039(5) -0.014(4) -0.004(3) 0.000(4) C6 0.033(4) 0.037(5) 0.020(4) 0.001(4) 0.000(3) -0.011(3) C7 0.043(4) 0.037(5) 0.033(4) -0.010(4) 0.005(3) -0.012(4) C8 0.042(4) 0.055(6) 0.064(6) -0.017(5) 0.003(4) -0.019(4) C9 0.065(5) 0.052(6) 0.060(6) -0.013(5) -0.013(4) -0.011(4) C10 0.026(3) 0.038(5) 0.035(4) -0.007(4) -0.008(3) 0.002(3) C11 0.063(5) 0.061(6) 0.046(5) -0.001(4) -0.011(4) -0.029(4) C12 0.051(5) 0.062(6) 0.057(6) 0.018(5) 0.004(4) -0.006(4) C13 0.032(4) 0.027(4) 0.016(4) -0.008(3) 0.000(3) -0.007(3) C14 0.032(4) 0.034(5) 0.030(4) -0.007(4) -0.006(3) -0.006(3) C15 0.028(3) 0.027(4) 0.032(4) -0.006(3) -0.003(3) -0.003(3) C16 0.030(3) 0.039(5) 0.026(4) -0.002(4) -0.003(3) -0.014(3) C17 0.013(3) 0.026(5) 0.037(5) -0.004(4) 0.000(3) -0.009(3) C18 0.032(4) 0.022(4) 0.021(4) -0.003(3) -0.001(3) -0.001(3) C19 0.037(4) 0.019(4) 0.031(4) -0.007(3) 0.005(3) -0.006(3) C20 0.037(4) 0.038(5) 0.037(5) -0.008(4) 0.009(3) -0.013(4) C21 0.042(4) 0.028(5) 0.027(4) -0.004(3) -0.001(3) -0.006(3) C22 0.025(3) 0.029(5) 0.032(4) -0.003(4) -0.008(3) 0.001(3) C23 0.024(3) 0.027(4) 0.036(5) -0.013(4) 0.001(3) -0.005(3) C24 0.030(4) 0.044(5) 0.037(4) -0.007(4) -0.001(3) -0.016(3) C25 0.028(4) 0.063(6) 0.102(7) -0.037(5) -0.005(4) 0.001(4) C26 0.043(4) 0.050(6) 0.077(6) -0.025(5) -0.009(4) -0.011(4) C27 0.031(4) 0.038(5) 0.034(4) -0.012(4) -0.005(3) -0.009(3) C28 0.042(4) 0.040(5) 0.044(5) -0.002(4) 0.004(3) -0.022(4) C29 0.030(4) 0.058(6) 0.049(5) -0.007(4) 0.006(3) -0.015(4) C30 0.029(4) 0.023(5) 0.025(4) 0.000(3) -0.006(3) 0.005(3) C31 0.030(4) 0.042(5) 0.023(4) -0.007(4) 0.002(3) -0.008(4) C32 0.021(3) 0.041(5) 0.039(5) -0.002(4) -0.005(3) 0.006(4) C33 0.027(4) 0.032(5) 0.042(5) -0.008(4) -0.003(3) 0.003(3) C34 0.040(4) 0.030(5) 0.025(4) -0.007(4) 0.000(3) -0.003(3) C35 0.029(3) 0.026(5) 0.023(4) -0.006(3) 0.003(3) -0.005(3) C36 0.023(3) 0.038(5) 0.056(6) 0.003(4) -0.006(3) -0.006(3) C37 0.037(4) 0.052(6) 0.118(8) -0.005(5) 0.006(4) -0.017(4) C38 0.075(5) 0.066(7) 0.053(6) -0.002(5) -0.022(4) -0.031(5) C39 0.032(4) 0.027(4) 0.036(4) -0.002(4) -0.001(3) -0.006(3) C40 0.032(4) 0.049(5) 0.047(5) -0.019(4) 0.008(3) -0.007(3) C41 0.039(4) 0.040(5) 0.040(5) -0.010(4) 0.000(3) -0.009(4) _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 Ag1 C13 2.076(5) . ? Ag1 Cl1 2.3174(16) . ? N1 C13 1.346(7) . ? N1 C14 1.393(7) . ? N1 C1 1.454(7) . ? N2 C13 1.356(7) . ? N2 C15 1.387(7) . ? N2 C16 1.443(7) . ? N3 C17 1.371(7) . ? N3 C18 1.438(8) . ? N3 H1 0.9800(11) . ? N4 C17 1.275(7) . ? N4 C30 1.427(7) . ? C1 C2 1.387(8) . ? C1 C6 1.390(8) . ? C2 C3 1.388(8) . ? C2 C7 1.514(9) . ? C3 C4 1.386(9) . ? C3 H3 0.9500 . ? C4 C5 1.381(9) . ? C4 H4 0.9500 . ? C5 C6 1.391(8) . ? C5 H5 0.9500 . ? C6 C10 1.526(9) . ? C7 C9 1.523(9) . ? C7 C8 1.524(8) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.514(8) . ? C10 C11 1.545(8) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.332(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.526(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 C23 1.408(8) . ? C18 C19 1.408(8) . ? C19 C20 1.398(8) . ? C19 C24 1.519(8) . ? C20 C21 1.386(8) . ? C20 H20 0.9500 . ? C21 C22 1.385(8) . ? C21 H21 0.9500 . ? C22 C23 1.375(8) . ? C22 H22 0.9500 . ? C23 C27 1.520(8) . ? C24 C26 1.530(9) . ? C24 C25 1.535(8) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.519(8) . ? C27 C28 1.537(8) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.405(8) . ? C30 C31 1.419(8) . ? C31 C32 1.404(9) . ? C31 C36 1.519(8) . ? C32 C33 1.384(8) . ? C32 H32 0.9500 . ? C33 C34 1.382(8) . ? C33 H33 0.9500 . ? C34 C35 1.377(8) . ? C34 H34 0.9500 . ? C35 C39 1.536(8) . ? C36 C37 1.528(8) . ? C36 C38 1.539(9) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.529(8) . ? C39 C40 1.531(8) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 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 C13 Ag1 Cl1 178.49(18) . . ? C13 N1 C14 110.8(5) . . ? C13 N1 C1 126.9(5) . . ? C14 N1 C1 122.2(5) . . ? C13 N2 C15 111.0(5) . . ? C13 N2 C16 125.1(5) . . ? C15 N2 C16 123.7(5) . . ? C17 N3 C18 124.1(5) . . ? C17 N3 H1 117(4) . . ? C18 N3 H1 119(4) . . ? C17 N4 C30 118.7(5) . . ? C2 C1 C6 123.8(6) . . ? C2 C1 N1 119.2(6) . . ? C6 C1 N1 116.8(6) . . ? C1 C2 C3 116.9(6) . . ? C1 C2 C7 123.5(6) . . ? C3 C2 C7 119.6(6) . . ? C4 C3 C2 121.0(6) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 120.5(6) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.5(7) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 117.3(6) . . ? C1 C6 C10 122.5(6) . . ? C5 C6 C10 120.2(6) . . ? C2 C7 C9 111.2(5) . . ? C2 C7 C8 111.7(5) . . ? C9 C7 C8 110.1(6) . . ? C2 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C6 111.2(5) . . ? C12 C10 C11 111.0(6) . . ? C6 C10 C11 111.8(5) . . ? C12 C10 H10 107.5 . . ? C6 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 104.5(5) . . ? N1 C13 Ag1 125.9(4) . . ? N2 C13 Ag1 129.5(4) . . ? C15 C14 N1 107.0(5) . . ? C15 C14 H14 126.5 . . ? N1 C14 H14 126.5 . . ? C14 C15 N2 106.7(5) . . ? C14 C15 H15 126.7 . . ? N2 C15 H15 126.7 . . ? N2 C16 C17 111.1(5) . . ? N2 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? N2 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C17 N3 126.8(6) . . ? N4 C17 C16 118.8(6) . . ? N3 C17 C16 114.3(6) . . ? C23 C18 C19 121.5(6) . . ? C23 C18 N3 120.0(5) . . ? C19 C18 N3 118.5(5) . . ? C20 C19 C18 117.9(5) . . ? C20 C19 C24 119.6(5) . . ? C18 C19 C24 122.4(6) . . ? C21 C20 C19 121.0(6) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.3(6) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 122.3(5) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C18 117.8(5) . . ? C22 C23 C27 121.0(5) . . ? C18 C23 C27 121.2(6) . . ? C19 C24 C26 110.6(5) . . ? C19 C24 C25 111.1(5) . . ? C26 C24 C25 111.1(5) . . ? C19 C24 H24 108.0 . . ? C26 C24 H24 108.0 . . ? C25 C24 H24 108.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 111.7(5) . . ? C29 C27 C28 111.1(5) . . ? C23 C27 C28 110.4(5) . . ? C29 C27 H27 107.8 . . ? C23 C27 H27 107.8 . . ? C28 C27 H27 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 120.9(6) . . ? C35 C30 N4 121.5(5) . . ? C31 C30 N4 117.3(5) . . ? C32 C31 C30 117.2(6) . . ? C32 C31 C36 122.3(5) . . ? C30 C31 C36 120.3(6) . . ? C33 C32 C31 121.8(5) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C34 C33 C32 119.3(6) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 121.7(6) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C34 C35 C30 119.0(5) . . ? C34 C35 C39 123.0(6) . . ? C30 C35 C39 118.0(6) . . ? C31 C36 C37 113.7(6) . . ? C31 C36 C38 109.8(5) . . ? C37 C36 C38 111.1(6) . . ? C31 C36 H36 107.3 . . ? C37 C36 H36 107.3 . . ? C38 C36 H36 107.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C40 111.6(5) . . ? C41 C39 C35 112.0(5) . . ? C40 C39 C35 111.2(5) . . ? C41 C39 H39 107.3 . . ? C40 C39 H39 107.3 . . ? C35 C39 H39 107.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 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 C13 N1 C1 C2 -81.3(8) . . . . ? C14 N1 C1 C2 102.0(7) . . . . ? C13 N1 C1 C6 103.1(7) . . . . ? C14 N1 C1 C6 -73.5(7) . . . . ? C6 C1 C2 C3 1.6(9) . . . . ? N1 C1 C2 C3 -173.7(5) . . . . ? C6 C1 C2 C7 -177.6(6) . . . . ? N1 C1 C2 C7 7.1(9) . . . . ? C1 C2 C3 C4 0.5(9) . . . . ? C7 C2 C3 C4 179.7(6) . . . . ? C2 C3 C4 C5 -1.9(10) . . . . ? C3 C4 C5 C6 1.3(10) . . . . ? C2 C1 C6 C5 -2.1(9) . . . . ? N1 C1 C6 C5 173.2(5) . . . . ? C2 C1 C6 C10 175.3(5) . . . . ? N1 C1 C6 C10 -9.3(8) . . . . ? C4 C5 C6 C1 0.6(9) . . . . ? C4 C5 C6 C10 -176.9(5) . . . . ? C1 C2 C7 C9 -118.2(7) . . . . ? C3 C2 C7 C9 62.7(8) . . . . ? C1 C2 C7 C8 118.4(6) . . . . ? C3 C2 C7 C8 -60.8(8) . . . . ? C1 C6 C10 C12 -119.2(7) . . . . ? C5 C6 C10 C12 58.2(8) . . . . ? C1 C6 C10 C11 116.1(6) . . . . ? C5 C6 C10 C11 -66.5(7) . . . . ? C14 N1 C13 N2 -0.5(7) . . . . ? C1 N1 C13 N2 -177.4(6) . . . . ? C14 N1 C13 Ag1 178.2(4) . . . . ? C1 N1 C13 Ag1 1.2(9) . . . . ? C15 N2 C13 N1 -0.3(7) . . . . ? C16 N2 C13 N1 -175.1(5) . . . . ? C15 N2 C13 Ag1 -178.9(4) . . . . ? C16 N2 C13 Ag1 6.3(9) . . . . ? Cl1 Ag1 C13 N1 -39(8) . . . . ? Cl1 Ag1 C13 N2 139(7) . . . . ? C13 N1 C14 C15 1.1(7) . . . . ? C1 N1 C14 C15 178.2(6) . . . . ? N1 C14 C15 N2 -1.2(7) . . . . ? C13 N2 C15 C14 0.9(7) . . . . ? C16 N2 C15 C14 175.9(5) . . . . ? C13 N2 C16 C17 107.7(6) . . . . ? C15 N2 C16 C17 -66.5(7) . . . . ? C30 N4 C17 N3 -1.3(8) . . . . ? C30 N4 C17 C16 177.0(4) . . . . ? C18 N3 C17 N4 179.7(5) . . . . ? C18 N3 C17 C16 1.3(7) . . . . ? N2 C16 C17 N4 -2.1(7) . . . . ? N2 C16 C17 N3 176.4(4) . . . . ? C17 N3 C18 C23 83.7(7) . . . . ? C17 N3 C18 C19 -97.5(7) . . . . ? C23 C18 C19 C20 2.9(9) . . . . ? N3 C18 C19 C20 -175.9(5) . . . . ? C23 C18 C19 C24 -177.2(5) . . . . ? N3 C18 C19 C24 3.9(9) . . . . ? C18 C19 C20 C21 -2.7(9) . . . . ? C24 C19 C20 C21 177.4(5) . . . . ? C19 C20 C21 C22 0.1(9) . . . . ? C20 C21 C22 C23 2.6(9) . . . . ? C21 C22 C23 C18 -2.4(9) . . . . ? C21 C22 C23 C27 177.2(6) . . . . ? C19 C18 C23 C22 -0.4(9) . . . . ? N3 C18 C23 C22 178.4(5) . . . . ? C19 C18 C23 C27 180.0(5) . . . . ? N3 C18 C23 C27 -1.2(9) . . . . ? C20 C19 C24 C26 -51.2(8) . . . . ? C18 C19 C24 C26 128.9(6) . . . . ? C20 C19 C24 C25 72.6(8) . . . . ? C18 C19 C24 C25 -107.3(7) . . . . ? C22 C23 C27 C29 38.6(8) . . . . ? C18 C23 C27 C29 -141.9(6) . . . . ? C22 C23 C27 C28 -85.7(7) . . . . ? C18 C23 C27 C28 93.9(7) . . . . ? C17 N4 C30 C35 87.0(7) . . . . ? C17 N4 C30 C31 -99.2(6) . . . . ? C35 C30 C31 C32 -1.6(9) . . . . ? N4 C30 C31 C32 -175.5(5) . . . . ? C35 C30 C31 C36 174.4(6) . . . . ? N4 C30 C31 C36 0.5(8) . . . . ? C30 C31 C32 C33 1.6(9) . . . . ? C36 C31 C32 C33 -174.4(6) . . . . ? C31 C32 C33 C34 -0.2(10) . . . . ? C32 C33 C34 C35 -1.1(9) . . . . ? C33 C34 C35 C30 1.0(9) . . . . ? C33 C34 C35 C39 179.3(5) . . . . ? C31 C30 C35 C34 0.4(9) . . . . ? N4 C30 C35 C34 174.0(5) . . . . ? C31 C30 C35 C39 -178.0(5) . . . . ? N4 C30 C35 C39 -4.4(8) . . . . ? C32 C31 C36 C37 -33.5(9) . . . . ? C30 C31 C36 C37 150.7(6) . . . . ? C32 C31 C36 C38 91.6(7) . . . . ? C30 C31 C36 C38 -84.2(7) . . . . ? C34 C35 C39 C41 25.2(8) . . . . ? C30 C35 C39 C41 -156.5(5) . . . . ? C34 C35 C39 C40 -100.3(7) . . . . ? C30 C35 C39 C40 77.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.545 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.113 data_complex8 _database_code_depnum_ccdc_archive 'CCDC 892661' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C46H66N4Cl1Cr1O1 _chemical_formula_sum 'C46 H66 Cl Cr N4 O' _chemical_formula_weight 778.48 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.4973(4) _cell_length_b 16.0212(4) _cell_length_c 18.7006(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4343.48(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 78790 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'light purple' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 0.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9476 _exptl_absorpt_correction_T_max 0.9928 _exptl_absorpt_process_details ; 'SADABS 2007/2 (Sheldrick, G.M., 2007)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; 'Bruker-Nonius APEX II CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30195 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.64 _reflns_number_total 9596 _reflns_number_gt 7847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_data_reduction ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 Farrugia 1997' _computing_publication_material 'WinGX Farrugia 1997' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+4.4226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(2) _refine_ls_number_reflns 9596 _refine_ls_number_parameters 487 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.003 _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 Cr1 Cr 0.31801(3) 0.35981(3) 0.82288(2) 0.02105(11) Uani 1 1 d . . . Cl2 Cl 0.45526(5) 0.28856(5) 0.81010(5) 0.03200(18) Uani 1 1 d . A . N1 N 0.45345(17) 0.50493(15) 0.76239(12) 0.0213(5) Uani 1 1 d . . . N2 N 0.31371(19) 0.54055(14) 0.77892(12) 0.0223(5) Uani 1 1 d . . . C1 C 0.3719(2) 0.47474(18) 0.78750(15) 0.0201(6) Uani 1 1 d . A . C3 C 0.3569(2) 0.60908(19) 0.74912(16) 0.0267(7) Uani 1 1 d . A . H3 H 0.3296 0.6615 0.7384 0.032 Uiso 1 1 calc R . . C2 C 0.4448(2) 0.58680(18) 0.73836(16) 0.0257(7) Uani 1 1 d . A . H2 H 0.4921 0.6204 0.7182 0.031 Uiso 1 1 calc R . . C8 C 0.6858(2) 0.41675(19) 0.79346(17) 0.0322(7) Uani 1 1 d . A . H8 H 0.7318 0.4144 0.8296 0.039 Uiso 1 1 calc R . . C9 C 0.6043(2) 0.45965(19) 0.80689(17) 0.0264(7) Uani 1 1 d . . . C6 C 0.6358(2) 0.38011(18) 0.67596(18) 0.0307(7) Uani 1 1 d . A . H6 H 0.6484 0.3541 0.6314 0.037 Uiso 1 1 calc R . . C7 C 0.7014(2) 0.37785(19) 0.72942(18) 0.0314(8) Uani 1 1 d . . . H7 H 0.7578 0.3491 0.7217 0.038 Uiso 1 1 calc R A . C5 C 0.5521(2) 0.41967(17) 0.68626(17) 0.0250(6) Uani 1 1 d . . . C4 C 0.5390(2) 0.45959(18) 0.75210(16) 0.0232(6) Uani 1 1 d . A . C11 C 0.4790(2) 0.4193(2) 0.62837(17) 0.0308(7) Uani 1 1 d . A . H11 H 0.4195 0.4367 0.6509 0.037 Uiso 1 1 calc R . . C12 C 0.5864(2) 0.5033(2) 0.87783(18) 0.0331(8) Uani 1 1 d . A . H12 H 0.5193 0.4968 0.8892 0.040 Uiso 1 1 calc R . . C17 C 0.1916(2) 0.38661(17) 0.94682(15) 0.0240(6) Uani 1 1 d . . . N3 N 0.22331(17) 0.42398(15) 0.88097(13) 0.0218(5) Uani 1 1 d . A . C18 C 0.2467(2) 0.39076(19) 1.00860(16) 0.0253(7) Uani 1 1 d . A . C22 C 0.1070(2) 0.3443(2) 0.94817(17) 0.0283(7) Uani 1 1 d . A . C19 C 0.2203(2) 0.3444(2) 1.06844(17) 0.0307(7) Uani 1 1 d . . . H19 H 0.2581 0.3451 1.1099 0.037 Uiso 1 1 calc R A . C20 C 0.1407(3) 0.2979(2) 1.06867(18) 0.0363(8) Uani 1 1 d . A . H20 H 0.1249 0.2653 1.1093 0.044 Uiso 1 1 calc R . . C25 C 0.3336(2) 0.44388(19) 1.01178(16) 0.0287(7) Uani 1 1 d . . . H25 H 0.3317 0.4836 0.9705 0.034 Uiso 1 1 calc R A . C24 C -0.0570(2) 0.3709(2) 0.9106(2) 0.0414(9) Uani 1 1 d . A . H24A H -0.0845 0.3243 0.9371 0.062 Uiso 1 1 calc R . . H24B H -0.0952 0.3836 0.8687 0.062 Uiso 1 1 calc R . . H24C H -0.0537 0.4201 0.9416 0.062 Uiso 1 1 calc R . . C26 C 0.4198(3) 0.3910(2) 1.0039(2) 0.0431(9) Uani 1 1 d . A . H26A H 0.4198 0.3470 1.0402 0.065 Uiso 1 1 calc R . . H26B H 0.4745 0.4263 1.0100 0.065 Uiso 1 1 calc R . . H26C H 0.4209 0.3657 0.9562 0.065 Uiso 1 1 calc R . . C21 C 0.0842(3) 0.2989(2) 1.00971(18) 0.0335(8) Uani 1 1 d . . . H21 H 0.0283 0.2681 1.0107 0.040 Uiso 1 1 calc R A . C23 C 0.0365(3) 0.2645(2) 0.84561(19) 0.0385(8) Uani 1 1 d . A . H23A H 0.0969 0.2531 0.8241 0.058 Uiso 1 1 calc R . . H23B H -0.0103 0.2681 0.8079 0.058 Uiso 1 1 calc R . . H23C H 0.0205 0.2194 0.8787 0.058 Uiso 1 1 calc R . . N4 N 0.15033(18) 0.54739(15) 0.91689(13) 0.0231(6) Uani 1 1 d . A . C32 C 0.1759(2) 0.69745(18) 0.93071(16) 0.0271(7) Uani 1 1 d . A . C30 C 0.1948(2) 0.50449(18) 0.86980(15) 0.0227(6) Uani 1 1 d . . . C36 C 0.0409(2) 0.6476(2) 0.86488(16) 0.0282(7) Uani 1 1 d . A . C28 C 0.0403(2) 0.3468(2) 0.88612(17) 0.0320(7) Uani 1 1 d . . . H28 H 0.0622 0.3907 0.8521 0.038 Uiso 1 1 calc R A . C31 C 0.1228(2) 0.63072(19) 0.90239(15) 0.0247(7) Uani 1 1 d . . . C27 C 0.3375(3) 0.4959(2) 1.08050(18) 0.0427(10) Uani 1 1 d . A . H27A H 0.2770 0.5211 1.0894 0.064 Uiso 1 1 calc R . . H27B H 0.3838 0.5400 1.0753 0.064 Uiso 1 1 calc R . . H27C H 0.3541 0.4598 1.1208 0.064 Uiso 1 1 calc R . . C29 C 0.2157(2) 0.5377(2) 0.79597(16) 0.0252(7) Uani 1 1 d . A . H29A H 0.1841 0.5021 0.7603 0.030 Uiso 1 1 calc R . . H29B H 0.1899 0.5947 0.7918 0.030 Uiso 1 1 calc R . . C33 C 0.1479(2) 0.7792(2) 0.91831(18) 0.0331(8) Uani 1 1 d . . . H33 H 0.1836 0.8241 0.9366 0.040 Uiso 1 1 calc R A . C42 C 0.3452(2) 0.6595(2) 0.93113(18) 0.0333(8) Uani 1 1 d . A . H42A H 0.3356 0.6081 0.9038 0.050 Uiso 1 1 calc R . . H42B H 0.3987 0.6527 0.9627 0.050 Uiso 1 1 calc R . . H42C H 0.3563 0.7060 0.8982 0.050 Uiso 1 1 calc R . . C37 C -0.0210(2) 0.5768(2) 0.83896(18) 0.0338(8) Uani 1 1 d . . . H37 H 0.0050 0.5235 0.8582 0.041 Uiso 1 1 calc R A . C34 C 0.0678(3) 0.7959(2) 0.87929(19) 0.0368(8) Uani 1 1 d . A . H34 H 0.0498 0.8520 0.8702 0.044 Uiso 1 1 calc R . . C40 C 0.2596(2) 0.6779(2) 0.97607(18) 0.0316(8) Uani 1 1 d . . . H40 H 0.2452 0.6261 1.0037 0.038 Uiso 1 1 calc R A . C39 C -0.0237(3) 0.5691(3) 0.7580(2) 0.0456(10) Uani 1 1 d . A . H39A H -0.0480 0.6208 0.7374 0.068 Uiso 1 1 calc R . . H39B H -0.0637 0.5223 0.7446 0.068 Uiso 1 1 calc R . . H39C H 0.0388 0.5591 0.7399 0.068 Uiso 1 1 calc R . . C45 C 0.5010(3) 0.4820(2) 0.5698(2) 0.0476(10) Uani 1 1 d . . . H45A H 0.5032 0.5383 0.5903 0.071 Uiso 1 1 calc R A . H45B H 0.4530 0.4797 0.5329 0.071 Uiso 1 1 calc R . . H45C H 0.5608 0.4685 0.5484 0.071 Uiso 1 1 calc R . . C38 C -0.1184(2) 0.5856(2) 0.8682(2) 0.0400(9) Uani 1 1 d . A . H38A H -0.1165 0.5863 0.9206 0.060 Uiso 1 1 calc R . . H38B H -0.1560 0.5384 0.8520 0.060 Uiso 1 1 calc R . . H38C H -0.1456 0.6378 0.8509 0.060 Uiso 1 1 calc R . . C46 C 0.4651(3) 0.3318(2) 0.5973(2) 0.0417(9) Uani 1 1 d . . . H46A H 0.5199 0.3157 0.5699 0.063 Uiso 1 1 calc R A . H46B H 0.4111 0.3318 0.5658 0.063 Uiso 1 1 calc R . . H46C H 0.4554 0.2919 0.6363 0.063 Uiso 1 1 calc R . . C44 C 0.6069(3) 0.5981(2) 0.8727(2) 0.0426(9) Uani 1 1 d . . . H44A H 0.6727 0.6065 0.8631 0.064 Uiso 1 1 calc R A . H44B H 0.5905 0.6251 0.9180 0.064 Uiso 1 1 calc R . . H44C H 0.5706 0.6225 0.8338 0.064 Uiso 1 1 calc R . . C35 C 0.0153(2) 0.7308(2) 0.85411(18) 0.0349(8) Uani 1 1 d . . . H35 H -0.0399 0.7427 0.8287 0.042 Uiso 1 1 calc R A . C43 C 0.6408(3) 0.4662(3) 0.9396(2) 0.0442(9) Uani 1 1 d . . . H43A H 0.6313 0.4057 0.9409 0.066 Uiso 1 1 calc R A . H43B H 0.6196 0.4909 0.9846 0.066 Uiso 1 1 calc R . . H43C H 0.7065 0.4782 0.9330 0.066 Uiso 1 1 calc R . . C41 C 0.2832(3) 0.7458(2) 1.0304(2) 0.0422(9) Uani 1 1 d . A . H41A H 0.3057 0.7954 1.0052 0.063 Uiso 1 1 calc R . . H41B H 0.3311 0.7253 1.0629 0.063 Uiso 1 1 calc R . . H41C H 0.2279 0.7601 1.0579 0.063 Uiso 1 1 calc R . . C51 C 0.2521(2) 0.3465(2) 0.72628(16) 0.0291(7) Uani 1 1 d . A . H51A H 0.1872 0.3323 0.7345 0.044 Uiso 1 1 calc R . . H51B H 0.2817 0.3020 0.6987 0.044 Uiso 1 1 calc R . . H51C H 0.2558 0.3991 0.6996 0.044 Uiso 1 1 calc R . . O1A O 0.26519(16) 0.24149(13) 0.85504(11) 0.0272(5) Uani 0.485(6) 1 d P A 1 C47A C 0.2614(14) 0.1695(8) 0.8070(8) 0.0335(7) Uani 0.485(6) 1 d PD A 1 H47A H 0.3202 0.1634 0.7806 0.040 Uiso 0.485(6) 1 calc PR A 1 H47B H 0.2106 0.1758 0.7721 0.040 Uiso 0.485(6) 1 calc PR A 1 C48A C 0.2446(6) 0.0932(5) 0.8555(4) 0.0335(7) Uani 0.485(6) 1 d PD A 1 H48A H 0.1801 0.0900 0.8726 0.040 Uiso 0.485(6) 1 calc PR A 1 H48B H 0.2620 0.0401 0.8320 0.040 Uiso 0.485(6) 1 calc PR A 1 C49A C 0.3112(6) 0.1173(4) 0.9145(4) 0.0335(7) Uani 0.485(6) 1 d PD A 1 H49A H 0.3762 0.1115 0.8990 0.040 Uiso 0.485(6) 1 calc PR A 1 H49B H 0.3011 0.0838 0.9582 0.040 Uiso 0.485(6) 1 calc PR A 1 C50A C 0.2847(9) 0.2084(5) 0.9257(9) 0.0335(7) Uani 0.485(6) 1 d PD A 1 H50A H 0.2297 0.2127 0.9568 0.040 Uiso 0.485(6) 1 calc PR A 1 H50B H 0.3361 0.2395 0.9483 0.040 Uiso 0.485(6) 1 calc PR A 1 O1B O 0.26519(16) 0.24149(13) 0.85504(11) 0.0272(5) Uani 0.515(6) 1 d P A 2 C47B C 0.2646(13) 0.1771(7) 0.7983(8) 0.0335(7) Uani 0.515(6) 1 d PD A 2 H47C H 0.3191 0.1832 0.7669 0.040 Uiso 0.515(6) 1 calc PR A 2 H47D H 0.2081 0.1817 0.7688 0.040 Uiso 0.515(6) 1 calc PR A 2 C48B C 0.2672(6) 0.0938(4) 0.8378(3) 0.0335(7) Uani 0.515(6) 1 d PD A 2 H48C H 0.3272 0.0655 0.8304 0.040 Uiso 0.515(6) 1 calc PR A 2 H48D H 0.2172 0.0566 0.8207 0.040 Uiso 0.515(6) 1 calc PR A 2 C49B C 0.2534(6) 0.1157(4) 0.9167(3) 0.0335(7) Uani 0.515(6) 1 d PD A 2 H49C H 0.2848 0.0751 0.9484 0.040 Uiso 0.515(6) 1 calc PR A 2 H49D H 0.1872 0.1182 0.9294 0.040 Uiso 0.515(6) 1 calc PR A 2 C50B C 0.2986(8) 0.2022(5) 0.9212(8) 0.0335(7) Uani 0.515(6) 1 d PD A 2 H50C H 0.2777 0.2332 0.9640 0.040 Uiso 0.515(6) 1 calc PR A 2 H50D H 0.3667 0.1981 0.9217 0.040 Uiso 0.515(6) 1 calc PR A 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 Cr1 0.0216(2) 0.0204(2) 0.0212(2) 0.00059(19) 0.0007(2) 0.0011(2) Cl2 0.0248(4) 0.0255(4) 0.0457(5) 0.0034(3) 0.0024(4) 0.0038(3) N1 0.0193(13) 0.0217(12) 0.0230(13) 0.0008(10) 0.0022(11) -0.0010(11) N2 0.0236(13) 0.0240(12) 0.0192(12) 0.0040(9) 0.0015(11) 0.0005(12) C1 0.0189(16) 0.0230(15) 0.0185(14) -0.0003(11) 0.0001(12) 0.0025(12) C3 0.0315(18) 0.0238(15) 0.0247(15) 0.0030(12) 0.0038(14) 0.0011(13) C2 0.0259(17) 0.0211(15) 0.0303(17) 0.0034(12) 0.0041(14) -0.0026(13) C8 0.0265(17) 0.0316(16) 0.0384(18) 0.0013(13) -0.0081(15) -0.0010(15) C9 0.0219(16) 0.0247(15) 0.0324(18) -0.0003(13) 0.0002(14) -0.0047(12) C6 0.0320(18) 0.0275(16) 0.0327(17) -0.0036(14) 0.0055(16) 0.0019(13) C7 0.0253(19) 0.0279(17) 0.0411(19) -0.0018(13) 0.0034(14) 0.0026(13) C5 0.0253(16) 0.0233(14) 0.0265(16) 0.0009(12) 0.0020(14) -0.0024(12) C4 0.0212(16) 0.0230(15) 0.0256(15) 0.0007(12) 0.0065(13) -0.0012(13) C11 0.0244(18) 0.0414(19) 0.0268(17) -0.0050(14) 0.0007(14) 0.0036(15) C12 0.0292(19) 0.0384(19) 0.0315(18) -0.0026(15) -0.0027(15) -0.0030(16) C17 0.0259(17) 0.0210(14) 0.0251(15) 0.0000(11) 0.0057(14) 0.0031(13) N3 0.0245(14) 0.0214(12) 0.0194(13) 0.0007(10) 0.0031(11) 0.0010(11) C18 0.0306(18) 0.0212(15) 0.0241(16) -0.0005(12) 0.0029(13) 0.0046(13) C22 0.0293(18) 0.0275(17) 0.0281(16) -0.0009(13) 0.0060(13) -0.0009(14) C19 0.0348(19) 0.0320(18) 0.0252(16) -0.0017(13) 0.0031(14) 0.0018(15) C20 0.049(2) 0.0346(18) 0.0259(17) 0.0047(14) 0.0097(16) -0.0041(17) C25 0.035(2) 0.0301(16) 0.0212(15) 0.0018(12) 0.0005(14) -0.0021(15) C24 0.031(2) 0.047(2) 0.046(2) 0.0004(17) 0.0041(16) -0.0021(17) C26 0.033(2) 0.045(2) 0.051(2) 0.0036(18) -0.0042(17) 0.0031(17) C21 0.037(2) 0.0301(17) 0.0337(18) 0.0020(14) 0.0088(15) -0.0075(15) C23 0.030(2) 0.046(2) 0.040(2) -0.0070(16) 0.0034(16) -0.0075(16) N4 0.0214(14) 0.0238(13) 0.0240(13) 0.0001(10) 0.0011(11) 0.0001(11) C32 0.0267(17) 0.0254(15) 0.0293(16) -0.0010(12) 0.0064(14) 0.0010(14) C30 0.0214(16) 0.0250(14) 0.0216(14) 0.0016(12) -0.0021(13) 0.0009(13) C36 0.0266(17) 0.0310(16) 0.0271(16) 0.0013(13) 0.0034(13) 0.0040(15) C28 0.0291(18) 0.0393(19) 0.0278(16) -0.0009(14) 0.0050(14) -0.0070(16) C31 0.0271(17) 0.0228(15) 0.0243(15) 0.0026(12) 0.0077(13) 0.0012(13) C27 0.059(3) 0.038(2) 0.0306(18) -0.0022(15) -0.0076(18) -0.0102(19) C29 0.0207(16) 0.0308(16) 0.0243(16) 0.0026(12) 0.0018(12) 0.0040(13) C33 0.035(2) 0.0268(17) 0.0375(19) -0.0002(14) 0.0068(15) -0.0017(15) C42 0.0304(19) 0.0308(18) 0.0386(19) -0.0045(14) 0.0008(15) -0.0028(14) C37 0.0266(19) 0.0333(18) 0.041(2) 0.0011(15) -0.0051(15) 0.0064(14) C34 0.040(2) 0.0274(17) 0.043(2) 0.0073(15) 0.0063(17) 0.0094(16) C40 0.033(2) 0.0290(17) 0.0330(19) -0.0040(14) 0.0004(15) 0.0008(14) C39 0.032(2) 0.056(2) 0.049(2) -0.0121(19) -0.0062(18) 0.0058(18) C45 0.062(3) 0.046(2) 0.034(2) 0.0033(17) -0.0072(19) 0.001(2) C38 0.0262(19) 0.043(2) 0.051(2) -0.0033(17) 0.0046(17) 0.0005(16) C46 0.036(2) 0.049(2) 0.040(2) -0.0114(16) -0.0088(17) -0.0037(18) C44 0.047(2) 0.041(2) 0.040(2) -0.0144(17) -0.0034(18) -0.0070(18) C35 0.032(2) 0.039(2) 0.0341(18) 0.0047(15) 0.0022(15) 0.0136(16) C43 0.034(2) 0.063(3) 0.036(2) -0.0006(18) -0.0076(17) -0.0063(19) C41 0.044(2) 0.044(2) 0.039(2) -0.0117(16) -0.0015(17) 0.0016(18) C51 0.0297(18) 0.0327(18) 0.0251(16) -0.0014(13) -0.0026(13) -0.0033(14) O1A 0.0340(13) 0.0214(11) 0.0262(11) -0.0001(9) 0.0014(10) -0.0014(9) C47A 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) C48A 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) C49A 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) C50A 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) O1B 0.0340(13) 0.0214(11) 0.0262(11) -0.0001(9) 0.0014(10) -0.0014(9) C47B 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) C48B 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) C49B 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) C50B 0.0366(16) 0.0262(11) 0.0377(15) 0.0023(9) 0.0042(15) -0.0006(11) _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 Cr1 N3 2.030(2) . ? Cr1 C51 2.055(3) . ? Cr1 C1 2.107(3) . ? Cr1 O1A 2.131(2) . ? Cr1 Cl2 2.3064(9) . ? N1 C1 1.361(4) . ? N1 C2 1.392(4) . ? N1 C4 1.451(4) . ? N2 C1 1.360(4) . ? N2 C3 1.381(4) . ? N2 C29 1.457(4) . ? C3 C2 1.339(4) . ? C3 H3 0.9500 . ? C2 H2 0.9500 . ? C8 C7 1.369(4) . ? C8 C9 1.391(5) . ? C8 H8 0.9500 . ? C9 C4 1.394(4) . ? C9 C12 1.522(5) . ? C6 C7 1.380(5) . ? C6 C5 1.383(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C5 C4 1.400(4) . ? C5 C11 1.514(4) . ? C11 C45 1.519(5) . ? C11 C46 1.531(5) . ? C11 H11 1.0000 . ? C12 C43 1.519(5) . ? C12 C44 1.551(5) . ? C12 H12 1.0000 . ? C17 C22 1.401(4) . ? C17 C18 1.406(4) . ? C17 N3 1.444(4) . ? N3 C30 1.370(4) . ? C18 C19 1.397(4) . ? C18 C25 1.522(5) . ? C22 C21 1.401(4) . ? C22 C28 1.511(5) . ? C19 C20 1.373(5) . ? C19 H19 0.9500 . ? C20 C21 1.374(5) . ? C20 H20 0.9500 . ? C25 C26 1.516(5) . ? C25 C27 1.533(4) . ? C25 H25 1.0000 . ? C24 C28 1.533(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C21 H21 0.9500 . ? C23 C28 1.521(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N4 C30 1.290(4) . ? N4 C31 1.419(4) . ? C32 C33 1.390(4) . ? C32 C31 1.420(4) . ? C32 C40 1.513(5) . ? C30 C29 1.510(4) . ? C36 C35 1.399(5) . ? C36 C31 1.406(4) . ? C36 C37 1.525(5) . ? C28 H28 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C33 C34 1.398(5) . ? C33 H33 0.9500 . ? C42 C40 1.528(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C37 C39 1.519(5) . ? C37 C38 1.522(5) . ? C37 H37 1.0000 . ? C34 C35 1.375(5) . ? C34 H34 0.9500 . ? C40 C41 1.526(5) . ? C40 H40 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C35 H35 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? O1A C50A 1.452(17) . ? O1A C47A 1.463(17) . ? C47A C48A 1.541(7) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C48A C49A 1.516(8) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C49A C50A 1.523(8) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C47B C48B 1.527(7) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C48B C49B 1.531(7) . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? C49B C50B 1.534(8) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50B H50C 0.9900 . ? C50B H50D 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 N3 Cr1 C51 102.01(12) . . ? N3 Cr1 C1 88.64(10) . . ? C51 Cr1 C1 89.25(12) . . ? N3 Cr1 O1A 93.24(9) . . ? C51 Cr1 O1A 89.36(11) . . ? C1 Cr1 O1A 177.86(10) . . ? N3 Cr1 Cl2 152.81(8) . . ? C51 Cr1 Cl2 105.02(10) . . ? C1 Cr1 Cl2 94.59(8) . . ? O1A Cr1 Cl2 84.21(6) . . ? C1 N1 C2 111.6(3) . . ? C1 N1 C4 127.6(2) . . ? C2 N1 C4 120.4(2) . . ? C1 N2 C3 112.5(3) . . ? C1 N2 C29 123.7(2) . . ? C3 N2 C29 123.7(3) . . ? N2 C1 N1 102.9(2) . . ? N2 C1 Cr1 119.0(2) . . ? N1 C1 Cr1 137.8(2) . . ? C2 C3 N2 106.3(3) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? C3 C2 N1 106.8(3) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C7 C8 C9 121.6(3) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C4 116.3(3) . . ? C8 C9 C12 122.0(3) . . ? C4 C9 C12 121.7(3) . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C6 C5 C4 116.7(3) . . ? C6 C5 C11 120.8(3) . . ? C4 C5 C11 122.4(3) . . ? C9 C4 C5 123.7(3) . . ? C9 C4 N1 118.8(3) . . ? C5 C4 N1 117.4(3) . . ? C5 C11 C45 111.5(3) . . ? C5 C11 C46 111.5(3) . . ? C45 C11 C46 111.0(3) . . ? C5 C11 H11 107.5 . . ? C45 C11 H11 107.5 . . ? C46 C11 H11 107.5 . . ? C43 C12 C9 113.2(3) . . ? C43 C12 C44 109.3(3) . . ? C9 C12 C44 111.3(3) . . ? C43 C12 H12 107.6 . . ? C9 C12 H12 107.6 . . ? C44 C12 H12 107.6 . . ? C22 C17 C18 120.3(3) . . ? C22 C17 N3 119.6(3) . . ? C18 C17 N3 120.0(3) . . ? C30 N3 C17 115.1(2) . . ? C30 N3 Cr1 126.81(19) . . ? C17 N3 Cr1 117.47(18) . . ? C19 C18 C17 118.5(3) . . ? C19 C18 C25 119.6(3) . . ? C17 C18 C25 121.9(3) . . ? C21 C22 C17 118.2(3) . . ? C21 C22 C28 119.6(3) . . ? C17 C22 C28 122.3(3) . . ? C20 C19 C18 121.5(3) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.4(3) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C26 C25 C18 111.5(3) . . ? C26 C25 C27 110.8(3) . . ? C18 C25 C27 111.5(3) . . ? C26 C25 H25 107.6 . . ? C18 C25 H25 107.6 . . ? C27 C25 H25 107.6 . . ? C28 C24 H24A 109.5 . . ? C28 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C28 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C21 C22 121.7(3) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C28 C23 H23A 109.5 . . ? C28 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C28 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C30 N4 C31 120.7(3) . . ? C33 C32 C31 119.3(3) . . ? C33 C32 C40 121.5(3) . . ? C31 C32 C40 119.2(3) . . ? N4 C30 N3 123.3(3) . . ? N4 C30 C29 122.5(3) . . ? N3 C30 C29 114.2(3) . . ? C35 C36 C31 118.6(3) . . ? C35 C36 C37 120.5(3) . . ? C31 C36 C37 120.8(3) . . ? C22 C28 C23 112.5(3) . . ? C22 C28 C24 111.5(3) . . ? C23 C28 C24 109.5(3) . . ? C22 C28 H28 107.7 . . ? C23 C28 H28 107.7 . . ? C24 C28 H28 107.7 . . ? C36 C31 N4 120.9(3) . . ? C36 C31 C32 120.0(3) . . ? N4 C31 C32 119.0(3) . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C29 C30 114.0(2) . . ? N2 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? N2 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C32 C33 C34 120.7(3) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C39 C37 C38 110.0(3) . . ? C39 C37 C36 113.1(3) . . ? C38 C37 C36 111.3(3) . . ? C39 C37 H37 107.4 . . ? C38 C37 H37 107.4 . . ? C36 C37 H37 107.4 . . ? C35 C34 C33 119.6(3) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C32 C40 C41 113.9(3) . . ? C32 C40 C42 112.5(3) . . ? C41 C40 C42 108.7(3) . . ? C32 C40 H40 107.1 . . ? C41 C40 H40 107.1 . . ? C42 C40 H40 107.1 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C11 C45 H45A 109.5 . . ? C11 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C11 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C11 C46 H46A 109.5 . . ? C11 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C11 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C12 C44 H44A 109.5 . . ? C12 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C12 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C34 C35 C36 121.8(3) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C12 C43 H43A 109.5 . . ? C12 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C12 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Cr1 C51 H51A 109.5 . . ? Cr1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Cr1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50A O1A C47A 106.1(5) . . ? C50A O1A Cr1 120.8(5) . . ? C47A O1A Cr1 122.8(5) . . ? O1A C47A C48A 105.7(9) . . ? O1A C47A H47A 110.6 . . ? C48A C47A H47A 110.6 . . ? O1A C47A H47B 110.6 . . ? C48A C47A H47B 110.6 . . ? H47A C47A H47B 108.7 . . ? C49A C48A C47A 97.2(8) . . ? C49A C48A H48A 112.3 . . ? C47A C48A H48A 112.3 . . ? C49A C48A H48B 112.3 . . ? C47A C48A H48B 112.3 . . ? H48A C48A H48B 109.9 . . ? C48A C49A C50A 100.6(8) . . ? C48A C49A H49A 111.6 . . ? C50A C49A H49A 111.6 . . ? C48A C49A H49B 111.6 . . ? C50A C49A H49B 111.6 . . ? H49A C49A H49B 109.4 . . ? O1A C50A C49A 105.9(9) . . ? O1A C50A H50A 110.6 . . ? C49A C50A H50A 110.6 . . ? O1A C50A H50B 110.6 . . ? C49A C50A H50B 110.6 . . ? H50A C50A H50B 108.7 . . ? C48B C47B H47C 110.7 . . ? C48B C47B H47D 110.7 . . ? H47C C47B H47D 108.8 . . ? C47B C48B C49B 105.2(7) . . ? C47B C48B H48C 110.7 . . ? C49B C48B H48C 110.7 . . ? C47B C48B H48D 110.7 . . ? C49B C48B H48D 110.7 . . ? H48C C48B H48D 108.8 . . ? C48B C49B C50B 101.8(7) . . ? C48B C49B H49C 111.4 . . ? C50B C49B H49C 111.4 . . ? C48B C49B H49D 111.4 . . ? C50B C49B H49D 111.4 . . ? H49C C49B H49D 109.3 . . ? C49B C50B H50C 111.5 . . ? C49B C50B H50D 111.5 . . ? H50C C50B H50D 109.3 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.301 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.065 data_complex9 _database_code_depnum_ccdc_archive 'CCDC 892662' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H110 Cl2 Cr2 N8' _chemical_formula_sum 'C82 H110 Cl2 Cr2 N8' _chemical_formula_weight 1382.68 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2847(9) _cell_length_b 15.9373(11) _cell_length_c 22.3137(13) _cell_angle_alpha 90.00 _cell_angle_beta 119.069(3) _cell_angle_gamma 90.00 _cell_volume 3818.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6042 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.89 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9167 _exptl_absorpt_correction_T_max 0.9421 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42589 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 30.11 _reflns_number_total 11240 _reflns_number_gt 5891 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+1.3540P] 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 11240 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1653 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.002 _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 0.8829(2) 0.85497(15) 1.08297(11) 0.0274(5) Uani 1 1 d . . . C2 C 0.9031(2) 0.77380(17) 1.17140(13) 0.0337(6) Uani 1 1 d . . . H2 H 0.9401 0.7417 1.2124 0.040 Uiso 1 1 calc R . . C3 C 0.7807(2) 0.78746(16) 1.13035(12) 0.0328(6) Uani 1 1 d . . . H3 H 0.7143 0.7672 1.1367 0.039 Uiso 1 1 calc R . . C4 C 1.1001(2) 0.81695(17) 1.17850(12) 0.0321(6) Uani 1 1 d . . . C5 C 1.1629(2) 0.75528(19) 1.16337(13) 0.0385(6) Uani 1 1 d . . . C6 C 1.2923(3) 0.7510(2) 1.20626(15) 0.0453(7) Uani 1 1 d . . . H6 H 1.3393 0.7098 1.1980 0.054 Uiso 1 1 calc R . . C7 C 1.3519(3) 0.8062(2) 1.26047(15) 0.0472(8) Uani 1 1 d . . . H7 H 1.4394 0.8020 1.2894 0.057 Uiso 1 1 calc R . . C8 C 1.2865(3) 0.8670(2) 1.27318(15) 0.0461(7) Uani 1 1 d . . . H8 H 1.3297 0.9046 1.3104 0.055 Uiso 1 1 calc R . . C9 C 1.1582(2) 0.87445(17) 1.23249(13) 0.0346(6) Uani 1 1 d . . . C10 C 1.0974(3) 0.6928(2) 1.10516(15) 0.0481(8) Uani 1 1 d . . . H10 H 1.0065 0.7064 1.0808 0.058 Uiso 1 1 calc R . . C11 C 1.1124(5) 0.6043(3) 1.1293(2) 0.1112(19) Uani 1 1 d . . . H11A H 1.2011 0.5898 1.1538 0.167 Uiso 1 1 calc R . . H11B H 1.0686 0.5669 1.0899 0.167 Uiso 1 1 calc R . . H11C H 1.0773 0.5980 1.1603 0.167 Uiso 1 1 calc R . . C12 C 1.1448(7) 0.7020(5) 1.0549(3) 0.167(3) Uani 1 1 d . . . H12A H 1.1344 0.7603 1.0391 0.251 Uiso 1 1 calc R . . H12B H 1.0976 0.6649 1.0157 0.251 Uiso 1 1 calc R . . H12C H 1.2332 0.6869 1.0772 0.251 Uiso 1 1 calc R . . C13 C 1.0861(3) 0.93927(18) 1.24827(15) 0.0432(7) Uani 1 1 d . . . H13 H 1.0001 0.9421 1.2081 0.052 Uiso 1 1 calc R . . C14 C 1.0744(4) 0.9144(2) 1.31145(18) 0.0588(9) Uani 1 1 d . . . H14A H 1.0335 0.8596 1.3035 0.088 Uiso 1 1 calc R . . H14B H 1.0248 0.9565 1.3195 0.088 Uiso 1 1 calc R . . H14C H 1.1576 0.9111 1.3517 0.088 Uiso 1 1 calc R . . C15 C 1.1437(3) 1.0267(2) 1.25885(17) 0.0586(9) Uani 1 1 d . . . H15A H 1.2273 1.0261 1.2988 0.088 Uiso 1 1 calc R . . H15B H 1.0915 1.0672 1.2664 0.088 Uiso 1 1 calc R . . H15C H 1.1493 1.0430 1.2181 0.088 Uiso 1 1 calc R . . C16 C 0.6535(2) 0.86622(16) 1.02112(12) 0.0289(5) Uani 1 1 d . . . H16A H 0.6494 0.9280 1.0240 0.035 Uiso 1 1 calc R . . H16B H 0.5838 0.8420 1.0258 0.035 Uiso 1 1 calc R . . C17 C 0.6382(2) 0.84268(15) 0.95160(12) 0.0263(5) Uani 1 1 d . . . C18 C 0.6677(3) 0.8854(2) 0.86061(13) 0.0417(7) Uani 1 1 d . . . C19 C 0.5716(3) 0.9432(2) 0.81889(15) 0.0597(11) Uani 1 1 d . . . C20 C 0.5280(4) 0.9414(3) 0.74871(18) 0.0819(15) Uani 1 1 d . . . H20 H 0.4657 0.9804 0.7202 0.098 Uiso 1 1 calc R . . C21 C 0.5718(4) 0.8857(4) 0.71983(18) 0.0909(17) Uani 1 1 d . . . H21 H 0.5390 0.8857 0.6715 0.109 Uiso 1 1 calc R . . C22 C 0.6633(4) 0.8291(3) 0.75950(19) 0.0786(14) Uani 1 1 d . . . H22 H 0.6928 0.7902 0.7384 0.094 Uiso 1 1 calc R . . C23 C 0.7139(3) 0.8285(2) 0.83183(16) 0.0533(9) Uani 1 1 d . . . C24 C 0.5158(3) 1.0041(2) 0.84864(19) 0.0637(10) Uani 1 1 d . . . H24 H 0.5240 0.9776 0.8912 0.076 Uiso 1 1 calc R . . C25 C 0.5879(6) 1.0867(3) 0.8704(3) 0.1125(19) Uani 1 1 d . . . H25A H 0.6756 1.0753 0.9028 0.169 Uiso 1 1 calc R . . H25B H 0.5527 1.1226 0.8924 0.169 Uiso 1 1 calc R . . H25C H 0.5815 1.1153 0.8299 0.169 Uiso 1 1 calc R . . C26 C 0.3770(4) 1.0207(4) 0.8016(3) 0.118(2) Uani 1 1 d . . . H26A H 0.3661 1.0569 0.7636 0.176 Uiso 1 1 calc R . . H26B H 0.3422 1.0485 0.8277 0.176 Uiso 1 1 calc R . . H26C H 0.3338 0.9673 0.7834 0.176 Uiso 1 1 calc R . . C27 C 0.8147(3) 0.7669(2) 0.8743(2) 0.0615(10) Uani 1 1 d . . . H27 H 0.8246 0.7674 0.9215 0.074 Uiso 1 1 calc R . . C28 C 0.7861(5) 0.6764(3) 0.8479(3) 0.1057(18) Uani 1 1 d . . . H28A H 0.7038 0.6604 0.8410 0.159 Uiso 1 1 calc R . . H28B H 0.8493 0.6388 0.8816 0.159 Uiso 1 1 calc R . . H28C H 0.7870 0.6723 0.8043 0.159 Uiso 1 1 calc R . . C29 C 0.9401(4) 0.7923(3) 0.8806(3) 0.0880(14) Uani 1 1 d . . . H29A H 0.9337 0.7921 0.8350 0.132 Uiso 1 1 calc R . . H29B H 1.0044 0.7524 0.9103 0.132 Uiso 1 1 calc R . . H29C H 0.9625 0.8487 0.9003 0.132 Uiso 1 1 calc R . . C30 C 0.4912(2) 0.74161(15) 0.93956(12) 0.0282(5) Uani 1 1 d . . . C31 C 0.5428(2) 0.66619(17) 0.97477(14) 0.0356(6) Uani 1 1 d . . . C32 C 0.4793(3) 0.6229(2) 1.00247(16) 0.0498(8) Uani 1 1 d . . . H32 H 0.5143 0.5728 1.0276 0.060 Uiso 1 1 calc R . . C33 C 0.3672(3) 0.6511(2) 0.99426(18) 0.0558(9) Uani 1 1 d . . . H33 H 0.3259 0.6210 1.0141 0.067 Uiso 1 1 calc R . . C34 C 0.3149(3) 0.7230(2) 0.95718(17) 0.0489(8) Uani 1 1 d . . . H34 H 0.2364 0.7414 0.9508 0.059 Uiso 1 1 calc R . . C35 C 0.3749(2) 0.76910(17) 0.92890(14) 0.0372(6) Uani 1 1 d . . . C36 C 0.6604(3) 0.62905(18) 0.97930(16) 0.0455(7) Uani 1 1 d . . . H36 H 0.7098 0.6759 0.9745 0.055 Uiso 1 1 calc R . . C37 C 0.6243(3) 0.5691(2) 0.91956(17) 0.0561(9) Uani 1 1 d . . . H37A H 0.5737 0.5234 0.9224 0.084 Uiso 1 1 calc R . . H37B H 0.6998 0.5459 0.9214 0.084 Uiso 1 1 calc R . . H37C H 0.5762 0.5995 0.8763 0.084 Uiso 1 1 calc R . . C38 C 0.7436(3) 0.5835(2) 1.04658(18) 0.0642(10) Uani 1 1 d . . . H38A H 0.7667 0.6221 1.0851 0.096 Uiso 1 1 calc R . . H38B H 0.8191 0.5637 1.0465 0.096 Uiso 1 1 calc R . . H38C H 0.6985 0.5355 1.0513 0.096 Uiso 1 1 calc R . . C39 C 0.3154(3) 0.84755(19) 0.88794(18) 0.0533(9) Uani 1 1 d . . . H39 H 0.3707 0.8692 0.8701 0.064 Uiso 1 1 calc R . . C40 C 0.3047(5) 0.9153(3) 0.9320(3) 0.138(3) Uani 1 1 d . . . H40A H 0.2462 0.8974 0.9475 0.207 Uiso 1 1 calc R . . H40B H 0.2744 0.9671 0.9052 0.207 Uiso 1 1 calc R . . H40C H 0.3866 0.9254 0.9719 0.207 Uiso 1 1 calc R . . C41 C 0.1883(3) 0.8317(2) 0.82701(15) 0.0483(8) Uani 1 1 d . . . H41A H 0.1308 0.8134 0.8432 0.072 Uiso 1 1 calc R . . H41B H 0.1946 0.7879 0.7981 0.072 Uiso 1 1 calc R . . H41C H 0.1570 0.8835 0.8004 0.072 Uiso 1 1 calc R . . N1 N 0.96475(18) 0.81564(13) 1.14222(10) 0.0284(4) Uani 1 1 d . . . N2 N 0.77090(18) 0.83653(12) 1.07740(10) 0.0266(4) Uani 1 1 d . . . N3 N 0.71155(19) 0.88745(14) 0.93335(10) 0.0328(5) Uani 1 1 d . . . N4 N 0.55717(18) 0.78740(13) 0.91282(10) 0.0289(5) Uani 1 1 d . . . Cl1 Cl 1.09295(7) 0.97996(6) 1.07770(3) 0.0594(3) Uani 1 1 d . . . Cr1 Cr 0.88766(4) 0.92924(3) 1.00311(2) 0.03245(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0286(12) 0.0265(13) 0.0183(11) -0.0007(9) 0.0045(9) -0.0052(9) C2 0.0365(14) 0.0383(15) 0.0245(12) 0.0080(11) 0.0133(11) -0.0041(11) C3 0.0369(14) 0.0369(15) 0.0258(12) 0.0040(11) 0.0163(11) -0.0066(11) C4 0.0264(12) 0.0410(15) 0.0224(12) 0.0104(11) 0.0067(10) -0.0033(10) C5 0.0340(14) 0.0517(17) 0.0289(13) 0.0082(12) 0.0147(11) -0.0010(12) C6 0.0347(15) 0.061(2) 0.0408(16) 0.0124(15) 0.0186(13) 0.0076(14) C7 0.0299(14) 0.063(2) 0.0387(16) 0.0144(15) 0.0089(12) -0.0031(14) C8 0.0353(15) 0.0527(19) 0.0334(15) 0.0064(13) 0.0034(12) -0.0087(13) C9 0.0306(13) 0.0392(15) 0.0259(13) 0.0074(11) 0.0075(10) -0.0066(11) C10 0.0442(16) 0.064(2) 0.0366(16) -0.0037(14) 0.0203(13) 0.0075(15) C11 0.139(5) 0.066(3) 0.074(3) -0.008(2) 0.009(3) -0.016(3) C12 0.230(8) 0.227(8) 0.115(5) -0.100(5) 0.139(5) -0.115(6) C13 0.0398(15) 0.0401(17) 0.0347(15) -0.0015(12) 0.0063(12) -0.0040(12) C14 0.073(2) 0.047(2) 0.065(2) -0.0013(16) 0.041(2) -0.0032(17) C15 0.073(2) 0.0431(19) 0.0476(19) 0.0005(15) 0.0201(17) -0.0102(16) C16 0.0264(11) 0.0298(13) 0.0232(11) -0.0019(10) 0.0063(9) -0.0045(10) C17 0.0241(11) 0.0245(12) 0.0227(11) 0.0040(9) 0.0054(9) -0.0017(9) C18 0.0374(15) 0.0587(19) 0.0236(13) 0.0004(13) 0.0105(11) -0.0250(13) C19 0.0421(17) 0.088(3) 0.0290(15) 0.0214(16) 0.0017(13) -0.0272(17) C20 0.058(2) 0.139(4) 0.0293(17) 0.026(2) 0.0060(17) -0.028(2) C21 0.064(3) 0.168(5) 0.0228(17) 0.004(2) 0.0075(18) -0.053(3) C22 0.077(3) 0.127(4) 0.048(2) -0.032(2) 0.042(2) -0.057(3) C23 0.0474(18) 0.077(2) 0.0375(16) -0.0101(16) 0.0222(15) -0.0329(17) C24 0.055(2) 0.068(2) 0.060(2) 0.0338(19) 0.0220(18) 0.0068(18) C25 0.155(5) 0.087(4) 0.147(5) -0.006(3) 0.113(4) -0.034(3) C26 0.078(3) 0.143(5) 0.097(4) 0.058(4) 0.015(3) 0.048(3) C27 0.070(2) 0.068(2) 0.070(2) -0.0217(19) 0.052(2) -0.0236(19) C28 0.140(5) 0.082(3) 0.147(5) -0.044(3) 0.111(4) -0.045(3) C29 0.062(2) 0.078(3) 0.133(4) -0.003(3) 0.055(3) -0.010(2) C30 0.0279(12) 0.0276(13) 0.0243(11) -0.0053(10) 0.0091(10) -0.0093(10) C31 0.0355(14) 0.0321(14) 0.0357(14) 0.0002(11) 0.0146(12) -0.0065(11) C32 0.0503(18) 0.0444(18) 0.0543(19) 0.0119(15) 0.0252(16) -0.0068(14) C33 0.063(2) 0.056(2) 0.064(2) -0.0003(17) 0.0431(19) -0.0173(17) C34 0.0404(16) 0.051(2) 0.062(2) -0.0128(16) 0.0309(15) -0.0121(14) C35 0.0314(13) 0.0303(14) 0.0443(16) -0.0088(12) 0.0141(12) -0.0075(11) C36 0.0387(15) 0.0314(15) 0.0611(19) 0.0096(14) 0.0201(14) 0.0000(12) C37 0.0529(19) 0.070(2) 0.0491(19) 0.0099(17) 0.0276(16) 0.0154(17) C38 0.056(2) 0.055(2) 0.053(2) -0.0031(16) 0.0041(16) 0.0114(16) C39 0.0278(14) 0.0379(17) 0.076(2) -0.0019(16) 0.0104(14) -0.0026(12) C40 0.127(4) 0.060(3) 0.098(4) -0.046(3) -0.048(3) 0.046(3) C41 0.0424(16) 0.056(2) 0.0439(17) -0.0067(14) 0.0187(14) -0.0010(14) N1 0.0268(10) 0.0326(11) 0.0217(10) 0.0047(8) 0.0087(8) -0.0047(8) N2 0.0265(10) 0.0269(11) 0.0207(10) -0.0010(8) 0.0071(8) -0.0068(8) N3 0.0328(11) 0.0364(12) 0.0191(10) 0.0019(9) 0.0048(8) -0.0134(9) N4 0.0295(10) 0.0284(11) 0.0230(10) 0.0000(8) 0.0081(8) -0.0058(8) Cl1 0.0477(4) 0.0797(6) 0.0254(3) 0.0177(3) -0.0022(3) -0.0390(4) Cr1 0.0318(2) 0.0357(2) 0.01985(19) 0.00346(17) 0.00465(15) -0.01474(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.353(3) . ? C1 N1 1.364(3) . ? C1 Cr1 2.163(2) . ? C2 C3 1.344(4) . ? C2 N1 1.386(3) . ? C2 H2 0.9500 . ? C3 N2 1.372(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 C9 1.402(4) . ? C4 N1 1.454(3) . ? C5 C6 1.403(4) . ? C5 C10 1.520(4) . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.373(4) . ? C7 H7 0.9500 . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 C13 1.510(4) . ? C10 C11 1.488(5) . ? C10 C12 1.500(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.529(4) . ? C13 C14 1.537(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N2 1.457(3) . ? C16 C17 1.516(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N4 1.296(3) . ? C17 N3 1.358(3) . ? C18 C23 1.382(5) . ? C18 C19 1.428(5) . ? C18 N3 1.441(3) . ? C19 C20 1.387(5) . ? C19 C24 1.515(6) . ? C20 C21 1.353(7) . ? C20 H20 0.9500 . ? C21 C22 1.377(7) . ? C21 H21 0.9500 . ? C22 C23 1.420(5) . ? C22 H22 0.9500 . ? C23 C27 1.502(5) . ? C24 C25 1.528(6) . ? C24 C26 1.530(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.531(5) . ? C27 C28 1.532(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.400(4) . ? C30 C31 1.407(4) . ? C30 N4 1.419(3) . ? C31 C32 1.391(4) . ? C31 C36 1.518(4) . ? C32 C33 1.374(5) . ? C32 H32 0.9500 . ? C33 C34 1.376(5) . ? C33 H33 0.9500 . ? C34 C35 1.391(4) . ? C34 H34 0.9500 . ? C35 C39 1.511(4) . ? C36 C37 1.520(5) . ? C36 C38 1.528(4) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.508(6) . ? C39 C41 1.513(4) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N3 Cr1 2.0675(19) . ? Cl1 Cr1 2.3884(8) . ? Cl1 Cr1 2.4124(8) 3_777 ? Cr1 Cl1 2.4124(8) 3_777 ? 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 N2 C1 N1 103.1(2) . . ? N2 C1 Cr1 118.46(16) . . ? N1 C1 Cr1 138.41(18) . . ? C3 C2 N1 106.7(2) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C2 C3 N2 106.3(2) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? C5 C4 C9 124.1(2) . . ? C5 C4 N1 118.3(2) . . ? C9 C4 N1 117.0(2) . . ? C4 C5 C6 116.6(3) . . ? C4 C5 C10 123.1(2) . . ? C6 C5 C10 120.3(3) . . ? C7 C6 C5 120.6(3) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 121.0(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 121.1(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 116.6(3) . . ? C8 C9 C13 120.9(3) . . ? C4 C9 C13 122.5(2) . . ? C11 C10 C12 109.8(5) . . ? C11 C10 C5 113.0(3) . . ? C12 C10 C5 109.7(3) . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C5 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 112.3(3) . . ? C9 C13 C14 111.3(2) . . ? C15 C13 C14 109.7(3) . . ? C9 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 112.3(2) . . ? N2 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N2 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? N4 C17 N3 124.3(2) . . ? N4 C17 C16 121.6(2) . . ? N3 C17 C16 114.0(2) . . ? C23 C18 C19 121.1(3) . . ? C23 C18 N3 121.7(3) . . ? C19 C18 N3 117.2(3) . . ? C20 C19 C18 117.8(4) . . ? C20 C19 C24 119.9(4) . . ? C18 C19 C24 122.3(3) . . ? C21 C20 C19 121.7(4) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 120.9(4) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C23 120.3(4) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 118.2(4) . . ? C18 C23 C27 122.3(3) . . ? C22 C23 C27 119.5(4) . . ? C19 C24 C25 112.1(3) . . ? C19 C24 C26 113.6(4) . . ? C25 C24 C26 110.5(4) . . ? C19 C24 H24 106.7 . . ? C25 C24 H24 106.7 . . ? C26 C24 H24 106.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.7(3) . . ? C23 C27 C28 114.1(4) . . ? C29 C27 C28 108.5(3) . . ? C23 C27 H27 107.4 . . ? C29 C27 H27 107.4 . . ? C28 C27 H27 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 120.5(2) . . ? C35 C30 N4 120.8(2) . . ? C31 C30 N4 118.7(2) . . ? C32 C31 C30 118.3(3) . . ? C32 C31 C36 119.9(3) . . ? C30 C31 C36 121.7(2) . . ? C33 C32 C31 121.4(3) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 119.8(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 121.2(3) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C30 118.7(3) . . ? C34 C35 C39 120.3(3) . . ? C30 C35 C39 121.0(3) . . ? C31 C36 C37 108.9(2) . . ? C31 C36 C38 114.3(3) . . ? C37 C36 C38 109.5(3) . . ? C31 C36 H36 108.0 . . ? C37 C36 H36 108.0 . . ? C38 C36 H36 108.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C35 111.6(3) . . ? C40 C39 C41 109.0(3) . . ? C35 C39 C41 113.0(3) . . ? C40 C39 H39 107.7 . . ? C35 C39 H39 107.7 . . ? C41 C39 H39 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C1 N1 C2 111.3(2) . . ? C1 N1 C4 129.6(2) . . ? C2 N1 C4 118.9(2) . . ? C1 N2 C3 112.6(2) . . ? C1 N2 C16 123.1(2) . . ? C3 N2 C16 124.3(2) . . ? C17 N3 C18 112.74(19) . . ? C17 N3 Cr1 123.20(15) . . ? C18 N3 Cr1 122.49(16) . . ? C17 N4 C30 118.6(2) . . ? Cr1 Cl1 Cr1 97.84(3) . 3_777 ? N3 Cr1 C1 90.39(8) . . ? N3 Cr1 Cl1 176.37(6) . . ? C1 Cr1 Cl1 93.04(6) . . ? N3 Cr1 Cl1 94.46(6) . 3_777 ? C1 Cr1 Cl1 174.73(7) . 3_777 ? Cl1 Cr1 Cl1 82.16(3) . 3_777 ? 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 N1 C2 C3 N2 0.3(3) . . . . ? C9 C4 C5 C6 0.9(4) . . . . ? N1 C4 C5 C6 -170.8(2) . . . . ? C9 C4 C5 C10 179.0(3) . . . . ? N1 C4 C5 C10 7.3(4) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C10 C5 C6 C7 -178.2(3) . . . . ? C5 C6 C7 C8 -0.8(5) . . . . ? C6 C7 C8 C9 0.7(5) . . . . ? C7 C8 C9 C4 0.1(4) . . . . ? C7 C8 C9 C13 177.7(3) . . . . ? C5 C4 C9 C8 -1.0(4) . . . . ? N1 C4 C9 C8 170.9(2) . . . . ? C5 C4 C9 C13 -178.5(3) . . . . ? N1 C4 C9 C13 -6.7(4) . . . . ? C4 C5 C10 C11 -117.4(4) . . . . ? C6 C5 C10 C11 60.6(5) . . . . ? C4 C5 C10 C12 119.7(5) . . . . ? C6 C5 C10 C12 -62.3(5) . . . . ? C8 C9 C13 C15 49.9(4) . . . . ? C4 C9 C13 C15 -132.7(3) . . . . ? C8 C9 C13 C14 -73.5(3) . . . . ? C4 C9 C13 C14 103.9(3) . . . . ? N2 C16 C17 N4 110.3(2) . . . . ? N2 C16 C17 N3 -72.9(3) . . . . ? C23 C18 C19 C20 -1.3(4) . . . . ? N3 C18 C19 C20 -179.6(3) . . . . ? C23 C18 C19 C24 177.8(3) . . . . ? N3 C18 C19 C24 -0.5(4) . . . . ? C18 C19 C20 C21 1.7(5) . . . . ? C24 C19 C20 C21 -177.3(4) . . . . ? C19 C20 C21 C22 -0.9(6) . . . . ? C20 C21 C22 C23 -0.4(6) . . . . ? C19 C18 C23 C22 0.1(4) . . . . ? N3 C18 C23 C22 178.3(3) . . . . ? C19 C18 C23 C27 -179.9(3) . . . . ? N3 C18 C23 C27 -1.6(4) . . . . ? C21 C22 C23 C18 0.8(5) . . . . ? C21 C22 C23 C27 -179.3(3) . . . . ? C20 C19 C24 C25 -92.4(4) . . . . ? C18 C19 C24 C25 88.5(4) . . . . ? C20 C19 C24 C26 33.7(5) . . . . ? C18 C19 C24 C26 -145.3(3) . . . . ? C18 C23 C27 C29 -105.4(4) . . . . ? C22 C23 C27 C29 74.7(4) . . . . ? C18 C23 C27 C28 131.2(3) . . . . ? C22 C23 C27 C28 -48.8(4) . . . . ? C35 C30 C31 C32 -4.2(4) . . . . ? N4 C30 C31 C32 178.2(2) . . . . ? C35 C30 C31 C36 172.1(3) . . . . ? N4 C30 C31 C36 -5.5(4) . . . . ? C30 C31 C32 C33 2.0(5) . . . . ? C36 C31 C32 C33 -174.4(3) . . . . ? C31 C32 C33 C34 0.8(5) . . . . ? C32 C33 C34 C35 -1.4(5) . . . . ? C33 C34 C35 C30 -0.8(4) . . . . ? C33 C34 C35 C39 179.6(3) . . . . ? C31 C30 C35 C34 3.7(4) . . . . ? N4 C30 C35 C34 -178.8(2) . . . . ? C31 C30 C35 C39 -176.7(3) . . . . ? N4 C30 C35 C39 0.8(4) . . . . ? C32 C31 C36 C37 85.1(3) . . . . ? C30 C31 C36 C37 -91.2(3) . . . . ? C32 C31 C36 C38 -37.7(4) . . . . ? C30 C31 C36 C38 146.0(3) . . . . ? C34 C35 C39 C40 65.2(4) . . . . ? C30 C35 C39 C40 -114.4(4) . . . . ? C34 C35 C39 C41 -58.0(4) . . . . ? C30 C35 C39 C41 122.4(3) . . . . ? N2 C1 N1 C2 0.5(3) . . . . ? Cr1 C1 N1 C2 -177.9(2) . . . . ? N2 C1 N1 C4 -175.1(2) . . . . ? Cr1 C1 N1 C4 6.6(4) . . . . ? C3 C2 N1 C1 -0.5(3) . . . . ? C3 C2 N1 C4 175.6(2) . . . . ? C5 C4 N1 C1 -91.8(3) . . . . ? C9 C4 N1 C1 95.9(3) . . . . ? C5 C4 N1 C2 92.9(3) . . . . ? C9 C4 N1 C2 -79.4(3) . . . . ? N1 C1 N2 C3 -0.3(3) . . . . ? Cr1 C1 N2 C3 178.46(17) . . . . ? N1 C1 N2 C16 179.5(2) . . . . ? Cr1 C1 N2 C16 -1.7(3) . . . . ? C2 C3 N2 C1 0.0(3) . . . . ? C2 C3 N2 C16 -179.8(2) . . . . ? C17 C16 N2 C1 54.9(3) . . . . ? C17 C16 N2 C3 -125.2(2) . . . . ? N4 C17 N3 C18 16.4(4) . . . . ? C16 C17 N3 C18 -160.4(2) . . . . ? N4 C17 N3 Cr1 -149.7(2) . . . . ? C16 C17 N3 Cr1 33.6(3) . . . . ? C23 C18 N3 C17 -95.4(3) . . . . ? C19 C18 N3 C17 82.9(3) . . . . ? C23 C18 N3 Cr1 70.7(3) . . . . ? C19 C18 N3 Cr1 -111.0(2) . . . . ? N3 C17 N4 C30 176.6(2) . . . . ? C16 C17 N4 C30 -7.0(3) . . . . ? C35 C30 N4 C17 93.4(3) . . . . ? C31 C30 N4 C17 -89.0(3) . . . . ? C17 N3 Cr1 C1 9.3(2) . . . . ? C18 N3 Cr1 C1 -155.4(2) . . . . ? C17 N3 Cr1 Cl1 -168.6(2) . . . 3_777 ? C18 N3 Cr1 Cl1 26.7(2) . . . 3_777 ? N2 C1 Cr1 N3 -26.30(19) . . . . ? N1 C1 Cr1 N3 151.9(3) . . . . ? N2 C1 Cr1 Cl1 154.89(18) . . . . ? N1 C1 Cr1 Cl1 -26.9(3) . . . . ? Cr1 Cl1 Cr1 C1 -177.84(8) 3_777 . . . ? Cr1 Cl1 Cr1 Cl1 0.0 3_777 . . 3_777 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.475 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.064 data_complex10 _database_code_depnum_ccdc_archive 'CCDC 892663' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C82 H112 Cl4 Cr2 N8, C4 H10 O, 2(C H2 Cl2) ; _chemical_formula_sum 'C88 H126 Cl8 Cr2 N8 O' _chemical_formula_weight 1699.57 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.433(10) _cell_length_b 21.648(15) _cell_length_c 29.447(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.642(7) _cell_angle_gamma 90.00 _cell_volume 9119(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 20.56 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3608 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9498 _exptl_absorpt_correction_T_max 0.9596 _exptl_absorpt_process_details 'Bruker SADABS' # absolute Tmin and Tmax unknown, but SADABS gives ratio as 0.904 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Rigaku Saturn 724+ detector on Crystal Logics diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71778 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 24.21 _reflns_number_total 15908 _reflns_number_gt 9457 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'Bruker Apex2' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+5.5165P] 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 15908 _refine_ls_number_parameters 970 _refine_ls_number_restraints 1206 _refine_ls_R_factor_all 0.1224 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.2097 _refine_ls_wR_factor_gt 0.1778 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.019 _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 Cr1 Cr 0.82589(4) 0.15921(3) 0.61443(2) 0.03299(15) Uani 1 1 d U . . Cr2 Cr 0.85121(4) 0.30124(3) 0.60657(2) 0.03668(15) Uani 1 1 d U . . Cl1 Cl 0.96665(6) 0.20779(4) 0.60316(3) 0.0443(2) Uani 1 1 d U . . Cl2 Cl 0.80738(7) 0.23925(4) 0.66888(3) 0.0445(2) Uani 1 1 d U . . Cl3 Cl 0.74818(7) 0.23293(4) 0.56089(3) 0.0444(3) Uani 1 1 d U . . Cl4 Cl 0.83064(7) 0.09305(4) 0.55522(3) 0.0417(2) Uani 1 1 d U . . N1 N 0.9747(2) 0.06514(13) 0.66810(10) 0.0370(7) Uani 1 1 d U . . N2 N 0.8533(2) 0.08316(13) 0.70067(10) 0.0348(7) Uani 1 1 d U . . N3 N 0.6030(2) 0.10486(14) 0.68836(10) 0.0380(8) Uani 1 1 d U . . H903 H 0.5575 0.1042 0.6653 0.046 Uiso 1 1 calc R . . N4 N 0.7022(2) 0.11915(13) 0.63338(10) 0.0336(7) Uani 1 1 d U . . N5 N 0.8613(2) 0.36651(14) 0.50632(11) 0.0440(8) Uani 1 1 d U C . N6 N 0.9734(2) 0.38510(14) 0.55976(10) 0.0423(8) Uani 1 1 d U . . N7 N 1.0285(2) 0.44145(14) 0.67185(11) 0.0423(8) Uani 1 1 d U . . H907 H 1.0093 0.4456 0.6988 0.051 Uiso 1 1 calc R . . N8 N 0.9185(2) 0.36359(14) 0.65189(10) 0.0394(8) Uani 1 1 d U . . C1 C 0.8946(3) 0.09942(16) 0.66369(12) 0.0344(8) Uani 1 1 d U . . C2 C 0.9814(3) 0.02877(18) 0.70747(13) 0.0420(10) Uani 1 1 d U . . H2 H 1.0304 0.0009 0.7179 0.050 Uiso 1 1 calc R . . C3 C 0.9062(3) 0.04044(17) 0.72758(13) 0.0404(10) Uani 1 1 d U . . H3 H 0.8916 0.0227 0.7553 0.049 Uiso 1 1 calc R . . C4 C 1.0499(3) 0.06611(17) 0.63962(13) 0.0383(9) Uani 1 1 d U . . C5 C 1.0473(3) 0.02178(17) 0.60418(13) 0.0388(9) Uani 1 1 d U . . C6 C 1.1237(3) 0.0220(2) 0.57962(14) 0.0480(11) Uani 1 1 d U . . H6 H 1.1248 -0.0066 0.5553 0.058 Uiso 1 1 calc R . . C7 C 1.1971(3) 0.0620(2) 0.58937(15) 0.0547(12) Uani 1 1 d U . . H7 H 1.2476 0.0612 0.5717 0.066 Uiso 1 1 calc R . . C8 C 1.1973(3) 0.1031(2) 0.62475(15) 0.0520(11) Uani 1 1 d U . . H8 H 1.2491 0.1301 0.6317 0.062 Uiso 1 1 calc R . . C10 C 0.9712(3) -0.02561(18) 0.59435(13) 0.0431(10) Uani 1 1 d U . . H10 H 0.9128 -0.0082 0.6040 0.052 Uiso 1 1 calc R . . C11 C 0.9506(3) -0.04301(19) 0.54347(13) 0.0479(11) Uani 1 1 d U . . H11A H 0.9002 -0.0736 0.5393 0.072 Uiso 1 1 calc R . . H11B H 1.0070 -0.0605 0.5333 0.072 Uiso 1 1 calc R . . H11C H 0.9316 -0.0060 0.5254 0.072 Uiso 1 1 calc R . . C12 C 0.9965(4) -0.08455(19) 0.62235(16) 0.0623(13) Uani 1 1 d U . . H12A H 0.9461 -0.1149 0.6158 0.093 Uiso 1 1 calc R . . H12B H 1.0049 -0.0745 0.6551 0.093 Uiso 1 1 calc R . . H12C H 1.0547 -0.1019 0.6140 0.093 Uiso 1 1 calc R . . C9 C 1.1233(2) 0.10645(6) 0.65084(4) 0.0433(10) Uani 1 1 d DU . . C13 C 1.13067(10) 0.14890(4) 0.69260(4) 0.0504(11) Uani 1 1 d DU . . H13 H 1.0662 0.1567 0.7002 0.060 Uiso 1 1 calc R . . C14 C 1.1877(2) 0.11846(9) 0.73389(6) 0.0623(13) Uani 1 1 d DU . . H14A H 1.1917 0.1464 0.7602 0.093 Uiso 1 1 calc R . . H14B H 1.2507 0.1095 0.7268 0.093 Uiso 1 1 calc R . . H14C H 1.1573 0.0799 0.7412 0.093 Uiso 1 1 calc R . . C15 C 1.17512(19) 0.21140(7) 0.68333(9) 0.0588(12) Uani 1 1 d DU . . H15A H 1.1787 0.2373 0.7108 0.088 Uiso 1 1 calc R . . H15B H 1.1368 0.2321 0.6578 0.088 Uiso 1 1 calc R . . H15C H 1.2382 0.2046 0.6754 0.088 Uiso 1 1 calc R . . C16 C 0.7704(2) 0.11152(17) 0.71390(12) 0.0348(9) Uani 1 1 d U . . H16A H 0.7855 0.1544 0.7240 0.042 Uiso 1 1 calc R . . H16B H 0.7518 0.0887 0.7404 0.042 Uiso 1 1 calc R . . C17 C 0.6884(2) 0.11288(15) 0.67615(12) 0.0335(8) Uani 1 1 d U . . C18 C 0.5727(2) 0.09713(18) 0.73254(13) 0.0382(9) Uani 1 1 d U . . C19 C 0.5196(3) 0.04443(18) 0.73893(14) 0.0428(10) Uani 1 1 d U . . C20 C 0.4906(3) 0.0360(2) 0.78148(15) 0.0529(11) Uani 1 1 d U . . H20 H 0.4564 -0.0001 0.7872 0.064 Uiso 1 1 calc R . . C21 C 0.5111(3) 0.0798(2) 0.81605(15) 0.0550(12) Uani 1 1 d U . . H21 H 0.4930 0.0726 0.8454 0.066 Uiso 1 1 calc R . . C22 C 0.5571(3) 0.1328(2) 0.80796(14) 0.0512(11) Uani 1 1 d U . . H22 H 0.5671 0.1633 0.8313 0.061 Uiso 1 1 calc R . . C23 C 0.5899(3) 0.14351(18) 0.76583(13) 0.0422(10) Uani 1 1 d U . . C24 C 0.4873(3) 0.00159(18) 0.69924(14) 0.0472(10) Uani 1 1 d U . . H24 H 0.5359 0.0024 0.6780 0.057 Uiso 1 1 calc R . . C25 C 0.4722(3) -0.0657(2) 0.71154(17) 0.0613(13) Uani 1 1 d U . . H25A H 0.4519 -0.0893 0.6835 0.092 Uiso 1 1 calc R . . H25B H 0.4241 -0.0682 0.7320 0.092 Uiso 1 1 calc R . . H25C H 0.5308 -0.0830 0.7269 0.092 Uiso 1 1 calc R . . C26 C 0.3971(3) 0.0268(2) 0.67301(16) 0.0587(12) Uani 1 1 d U . . H26A H 0.3760 -0.0006 0.6472 0.088 Uiso 1 1 calc R . . H26B H 0.4084 0.0682 0.6615 0.088 Uiso 1 1 calc R . . H26C H 0.3489 0.0289 0.6935 0.088 Uiso 1 1 calc R . . C27 C 0.6316(3) 0.20654(18) 0.75768(14) 0.0472(10) Uani 1 1 d U . . H27 H 0.6512 0.2063 0.7264 0.057 Uiso 1 1 calc R . . C28 C 0.7181(3) 0.2219(2) 0.79219(15) 0.0546(12) Uani 1 1 d U . . H28A H 0.7425 0.2624 0.7850 0.082 Uiso 1 1 calc R . . H28B H 0.7662 0.1904 0.7904 0.082 Uiso 1 1 calc R . . H28C H 0.7006 0.2225 0.8232 0.082 Uiso 1 1 calc R . . C29 C 0.5588(4) 0.2579(2) 0.75902(17) 0.0669(14) Uani 1 1 d U . . H29A H 0.5872 0.2979 0.7536 0.100 Uiso 1 1 calc R . . H29B H 0.5369 0.2582 0.7891 0.100 Uiso 1 1 calc R . . H29C H 0.5058 0.2504 0.7352 0.100 Uiso 1 1 calc R . . C30 C 0.6213(3) 0.10104(17) 0.60084(12) 0.0358(9) Uani 1 1 d U . . C31 C 0.6179(3) 0.03817(17) 0.58800(12) 0.0363(9) Uani 1 1 d U . . C32 C 0.5356(3) 0.01794(19) 0.56161(13) 0.0431(10) Uani 1 1 d U . . H32 H 0.5305 -0.0242 0.5526 0.052 Uiso 1 1 calc R . . C33 C 0.4621(3) 0.05714(19) 0.54826(14) 0.0457(10) Uani 1 1 d U . . H33 H 0.4071 0.0419 0.5305 0.055 Uiso 1 1 calc R . . C34 C 0.4682(3) 0.11826(19) 0.56057(14) 0.0466(10) Uani 1 1 d U . . H34 H 0.4174 0.1451 0.5506 0.056 Uiso 1 1 calc R . . C35 C 0.5470(3) 0.14194(17) 0.58736(13) 0.0403(9) Uani 1 1 d U . . C36 C 0.5445(3) 0.20987(19) 0.60228(15) 0.0499(11) Uani 1 1 d U . . H36 H 0.6075 0.2214 0.6184 0.060 Uiso 1 1 calc R . . C37 C 0.4715(3) 0.2193(2) 0.63573(17) 0.0653(13) Uani 1 1 d U . . H37A H 0.4712 0.2627 0.6451 0.098 Uiso 1 1 calc R . . H37B H 0.4877 0.1932 0.6628 0.098 Uiso 1 1 calc R . . H37C H 0.4094 0.2079 0.6205 0.098 Uiso 1 1 calc R . . C38 C 0.5209(3) 0.2525(2) 0.56109(17) 0.0630(13) Uani 1 1 d U . . H38A H 0.5199 0.2954 0.5716 0.095 Uiso 1 1 calc R . . H38B H 0.4594 0.2415 0.5448 0.095 Uiso 1 1 calc R . . H38C H 0.5683 0.2480 0.5404 0.095 Uiso 1 1 calc R . . C39 C 0.6968(3) -0.00652(17) 0.60250(13) 0.0398(9) Uani 1 1 d U . . H39 H 0.7552 0.0185 0.6097 0.048 Uiso 1 1 calc R . . C40 C 0.7128(3) -0.05144(18) 0.56430(14) 0.0492(11) Uani 1 1 d U . . H40A H 0.7645 -0.0793 0.5752 0.074 Uiso 1 1 calc R . . H40B H 0.7281 -0.0282 0.5377 0.074 Uiso 1 1 calc R . . H40C H 0.6559 -0.0757 0.5555 0.074 Uiso 1 1 calc R . . C41 C 0.6846(3) -0.04347(19) 0.64549(15) 0.0522(11) Uani 1 1 d U . . H41A H 0.7383 -0.0710 0.6531 0.078 Uiso 1 1 calc R . . H41B H 0.6272 -0.0681 0.6399 0.078 Uiso 1 1 calc R . . H41C H 0.6804 -0.0150 0.6710 0.078 Uiso 1 1 calc R . . C51 C 0.8917(3) 0.35302(16) 0.55136(13) 0.0380(9) Uani 1 1 d U . . C52 C 0.9224(3) 0.40558(18) 0.48832(15) 0.0545(11) Uani 1 1 d U . . H52 H 0.9157 0.4215 0.4580 0.065 Uiso 1 1 calc R . . C53 C 0.9929(3) 0.41683(18) 0.52147(14) 0.0526(11) Uani 1 1 d U . . H53 H 1.0462 0.4418 0.5192 0.063 Uiso 1 1 calc R . . C54 C 0.7811(3) 0.34072(17) 0.47829(13) 0.0460(10) Uani 1 1 d DU . . C56 C 0.7168(4) 0.2639(2) 0.42550(15) 0.0652(13) Uani 1 1 d DU . . H56 H 0.7226 0.2275 0.4081 0.078 Uiso 1 1 calc R A 1 C57 C 0.6321(4) 0.2919(2) 0.42365(16) 0.0705(14) Uani 1 1 d U C . H57 H 0.5799 0.2746 0.4048 0.085 Uiso 1 1 calc R . . C58 C 0.6201(4) 0.3437(2) 0.44787(17) 0.0733(14) Uani 1 1 d DU . . H58 H 0.5601 0.3622 0.4456 0.088 Uiso 1 1 calc R B 3 C55A C 0.79600(6) 0.28772(8) 0.45269(6) 0.0537(10) Uani 0.469(5) 1 d PDU C 1 C60A C 0.89198(6) 0.25715(4) 0.46230(5) 0.0598(14) Uani 0.469(5) 1 d PDU C 1 H60A H 0.9247 0.2741 0.4918 0.072 Uiso 0.469(5) 1 calc PR C 1 C61A C 0.88252(18) 0.18748(5) 0.46752(14) 0.0621(18) Uani 0.469(5) 1 d PDU C 1 H61A H 0.9448 0.1689 0.4742 0.093 Uiso 0.469(5) 1 calc PR C 1 H61B H 0.8502 0.1701 0.4390 0.093 Uiso 0.469(5) 1 calc PR C 1 H61C H 0.8465 0.1786 0.4927 0.093 Uiso 0.469(5) 1 calc PR C 1 C62A C 0.95259(12) 0.27063(16) 0.42429(9) 0.0639(17) Uani 0.469(5) 1 d PDU C 1 H62A H 1.0137 0.2507 0.4318 0.096 Uiso 0.469(5) 1 calc PR C 1 H62B H 0.9611 0.3153 0.4217 0.096 Uiso 0.469(5) 1 calc PR C 1 H62C H 0.9216 0.2544 0.3951 0.096 Uiso 0.469(5) 1 calc PR C 1 C55B C 0.79600(6) 0.28772(8) 0.45269(6) 0.0537(10) Uani 0.531(5) 1 d PDU C 2 C60B C 0.88993(8) 0.25896(6) 0.44612(3) 0.0598(14) Uani 0.531(5) 1 d PDU C 2 H60B H 0.9400 0.2904 0.4547 0.072 Uiso 0.531(5) 1 calc PR C 2 C61B C 0.9105(2) 0.20278(9) 0.47700(7) 0.0621(18) Uani 0.531(5) 1 d PDU C 2 H61D H 0.9716 0.1856 0.4727 0.093 Uiso 0.531(5) 1 calc PR C 2 H61E H 0.8621 0.1714 0.4691 0.093 Uiso 0.531(5) 1 calc PR C 2 H61F H 0.9112 0.2151 0.5091 0.093 Uiso 0.531(5) 1 calc PR C 2 C62B C 0.8931(2) 0.23983(17) 0.39607(5) 0.0639(17) Uani 0.531(5) 1 d PDU C 2 H62D H 0.9544 0.2219 0.3931 0.096 Uiso 0.531(5) 1 calc PR C 2 H62E H 0.8828 0.2762 0.3762 0.096 Uiso 0.531(5) 1 calc PR C 2 H62F H 0.8443 0.2092 0.3869 0.096 Uiso 0.531(5) 1 calc PR C 2 C59A C 0.69490(17) 0.37030(6) 0.47618(8) 0.0598(11) Uani 0.735(11) 1 d PDU C 3 C63A C 0.68839(7) 0.43050(5) 0.50262(5) 0.0781(15) Uani 0.735(11) 1 d PDU C 3 H63A H 0.7298 0.4269 0.5326 0.094 Uiso 0.735(11) 1 calc PR C 3 C64A C 0.58874(9) 0.44179(12) 0.51244(11) 0.105(2) Uani 0.735(11) 1 d PDU C 3 H64A H 0.5865 0.4801 0.5300 0.158 Uiso 0.735(11) 1 calc PR C 3 H64B H 0.5686 0.4072 0.5302 0.158 Uiso 0.735(11) 1 calc PR C 3 H64C H 0.5470 0.4454 0.4834 0.158 Uiso 0.735(11) 1 calc PR C 3 C65A C 0.7211(2) 0.48622(8) 0.47654(12) 0.110(3) Uani 0.735(11) 1 d PDU C 3 H65A H 0.7177 0.5237 0.4949 0.165 Uiso 0.735(11) 1 calc PR C 3 H65B H 0.6806 0.4909 0.4473 0.165 Uiso 0.735(11) 1 calc PR C 3 H65C H 0.7857 0.4796 0.4708 0.165 Uiso 0.735(11) 1 calc PR C 3 C59B C 0.69490(17) 0.37030(6) 0.47618(8) 0.0598(11) Uani 0.265(11) 1 d PDU C 4 C63B C 0.67595(11) 0.43148(6) 0.49908(7) 0.0781(15) Uani 0.265(11) 1 d PDU C 4 H63B H 0.7254 0.4377 0.5258 0.094 Uiso 0.265(11) 1 calc PR C 4 C64B C 0.58127(16) 0.43031(16) 0.51662(14) 0.105(2) Uani 0.265(11) 1 d PDU C 4 H64D H 0.5708 0.4699 0.5313 0.158 Uiso 0.265(11) 1 calc PR C 4 H64E H 0.5803 0.3968 0.5390 0.158 Uiso 0.265(11) 1 calc PR C 4 H64F H 0.5319 0.4235 0.4909 0.158 Uiso 0.265(11) 1 calc PR C 4 C65B C 0.6791(4) 0.48644(9) 0.46625(14) 0.110(3) Uani 0.265(11) 1 d PDU C 4 H65D H 0.6664 0.5247 0.4820 0.165 Uiso 0.265(11) 1 calc PR C 4 H65E H 0.6317 0.4808 0.4395 0.165 Uiso 0.265(11) 1 calc PR C 4 H65F H 0.7411 0.4888 0.4563 0.165 Uiso 0.265(11) 1 calc PR C 4 C66 C 1.0358(3) 0.38037(17) 0.60200(13) 0.0416(9) Uani 1 1 d U . . H66A H 1.0905 0.4073 0.6000 0.050 Uiso 1 1 calc R . . H66B H 1.0589 0.3373 0.6054 0.050 Uiso 1 1 calc R . . C67 C 0.9925(3) 0.39803(16) 0.64499(13) 0.0385(9) Uani 1 1 d U . . C68 C 1.0968(3) 0.48228(18) 0.65998(13) 0.0439(10) Uani 1 1 d U . . C69 C 1.0657(3) 0.54310(18) 0.64735(13) 0.0475(10) Uani 1 1 d U . . C70 C 1.1322(3) 0.5867(2) 0.63821(15) 0.0588(12) Uani 1 1 d U . . H70 H 1.1124 0.6274 0.6296 0.071 Uiso 1 1 calc R . . C71 C 1.2255(4) 0.5720(2) 0.64142(16) 0.0660(14) Uani 1 1 d U . . H71 H 1.2695 0.6020 0.6345 0.079 Uiso 1 1 calc R . . C72 C 1.2546(3) 0.5138(2) 0.65468(15) 0.0621(13) Uani 1 1 d U . . H72 H 1.3195 0.5045 0.6580 0.074 Uiso 1 1 calc R . . C73 C 1.1917(3) 0.4675(2) 0.66357(14) 0.0509(11) Uani 1 1 d U . . C74 C 1.2294(3) 0.4048(2) 0.67872(18) 0.0697(14) Uani 1 1 d U . . H74 H 1.1749 0.3772 0.6815 0.084 Uiso 1 1 calc R . . C75 C 1.2860(4) 0.3754(3) 0.6431(2) 0.105(2) Uani 1 1 d U . . H75A H 1.3088 0.3347 0.6540 0.157 Uiso 1 1 calc R . . H75B H 1.3393 0.4020 0.6391 0.157 Uiso 1 1 calc R . . H75C H 1.2458 0.3710 0.6138 0.157 Uiso 1 1 calc R . . C76 C 1.2873(4) 0.4092(3) 0.7258(2) 0.107(2) Uani 1 1 d U . . H76A H 1.3107 0.3681 0.7355 0.160 Uiso 1 1 calc R . . H76B H 1.2482 0.4251 0.7480 0.160 Uiso 1 1 calc R . . H76C H 1.3402 0.4372 0.7243 0.160 Uiso 1 1 calc R . . C77 C 0.9629(3) 0.55881(19) 0.64345(15) 0.0546(11) Uani 1 1 d U . . H77 H 0.9341 0.5290 0.6634 0.066 Uiso 1 1 calc R . . C78 C 0.9454(4) 0.6236(2) 0.66129(19) 0.0787(16) Uani 1 1 d U . . H78A H 0.8779 0.6313 0.6585 0.118 Uiso 1 1 calc R . . H78B H 0.9744 0.6544 0.6432 0.118 Uiso 1 1 calc R . . H78C H 0.9725 0.6268 0.6935 0.118 Uiso 1 1 calc R . . C79 C 0.9141(3) 0.5497(2) 0.59494(15) 0.0597(13) Uani 1 1 d U . . H79A H 0.8476 0.5598 0.5938 0.090 Uiso 1 1 calc R . . H79B H 0.9207 0.5066 0.5858 0.090 Uiso 1 1 calc R . . H79C H 0.9424 0.5768 0.5740 0.090 Uiso 1 1 calc R . . C80 C 0.8793(3) 0.37774(17) 0.69342(13) 0.0399(9) Uani 1 1 d U . . C81 C 0.9196(3) 0.35200(16) 0.73548(13) 0.0404(9) Uani 1 1 d U . . C82 C 0.8785(3) 0.36476(17) 0.77465(14) 0.0439(10) Uani 1 1 d U . . H82 H 0.9041 0.3468 0.8030 0.053 Uiso 1 1 calc R . . C83 C 0.8023(3) 0.4025(2) 0.77324(15) 0.0542(11) Uani 1 1 d U . . H83 H 0.7766 0.4115 0.8006 0.065 Uiso 1 1 calc R . . C84 C 0.7632(3) 0.4272(2) 0.73250(15) 0.0555(12) Uani 1 1 d U . . H84 H 0.7105 0.4537 0.7319 0.067 Uiso 1 1 calc R . . C85 C 0.7988(3) 0.41454(19) 0.69167(14) 0.0464(10) Uani 1 1 d U . . C86 C 1.0071(3) 0.31233(17) 0.73984(14) 0.0432(10) Uani 1 1 d U . . H86 H 1.0221 0.3036 0.7083 0.052 Uiso 1 1 calc R . . C87 C 0.9944(3) 0.25067(18) 0.76327(15) 0.0536(12) Uani 1 1 d U . . H87A H 1.0523 0.2267 0.7649 0.080 Uiso 1 1 calc R . . H87B H 0.9433 0.2276 0.7456 0.080 Uiso 1 1 calc R . . H87C H 0.9794 0.2581 0.7943 0.080 Uiso 1 1 calc R . . C88 C 1.0888(3) 0.34744(19) 0.76556(15) 0.0520(11) Uani 1 1 d U . . H88A H 1.1451 0.3217 0.7681 0.078 Uiso 1 1 calc R . . H88B H 1.0747 0.3579 0.7963 0.078 Uiso 1 1 calc R . . H88C H 1.0994 0.3855 0.7489 0.078 Uiso 1 1 calc R . . C89 C 0.7467(3) 0.4372(2) 0.64703(17) 0.0667(13) Uani 1 1 d U . . H89 H 0.7887 0.4332 0.6228 0.080 Uiso 1 1 calc R . . C90 C 0.7155(4) 0.5049(2) 0.64869(18) 0.0819(16) Uani 1 1 d U . . H90A H 0.6823 0.5168 0.6188 0.123 Uiso 1 1 calc R . . H90B H 0.7705 0.5314 0.6562 0.123 Uiso 1 1 calc R . . H90C H 0.6739 0.5097 0.6722 0.123 Uiso 1 1 calc R . . C91 C 0.6625(4) 0.3956(3) 0.6343(2) 0.096(2) Uani 1 1 d U . . H91A H 0.6279 0.4094 0.6052 0.144 Uiso 1 1 calc R . . H91B H 0.6218 0.3976 0.6584 0.144 Uiso 1 1 calc R . . H91C H 0.6836 0.3530 0.6312 0.144 Uiso 1 1 calc R . . C100 C 0.6296(3) 0.1264(2) 0.47268(14) 0.0550(12) Uani 1 1 d DU . . H10A H 0.6691 0.1617 0.4846 0.066 Uiso 1 1 calc R . . H10B H 0.6186 0.1002 0.4990 0.066 Uiso 1 1 calc R . . Cl5 Cl 0.52157(9) 0.15414(6) 0.44509(5) 0.0684(4) Uani 1 1 d DU . . Cl6 Cl 0.68825(9) 0.08309(6) 0.43476(4) 0.0724(4) Uani 1 1 d DU . . C10A C 0.8473(6) 0.7845(3) 0.4602(3) 0.094(2) Uani 0.640(3) 1 d PDU D 5 H10C H 0.9058 0.8085 0.4603 0.113 Uiso 0.640(3) 1 calc PR D 5 H10D H 0.8158 0.7820 0.4282 0.113 Uiso 0.640(3) 1 calc PR D 5 Cl7A Cl 0.7743(3) 0.82050(18) 0.49487(14) 0.1186(7) Uani 0.640(3) 1 d PDU D 5 Cl8A Cl 0.8726(2) 0.71004(13) 0.48206(11) 0.1199(9) Uani 0.640(3) 1 d PDU D 5 C10B C 0.8533(6) 0.7842(5) 0.4729(5) 0.094(2) Uani 0.360(3) 1 d PDU D 6 H10E H 0.8984 0.7622 0.4956 0.113 Uiso 0.360(3) 1 calc PR D 6 H10F H 0.8885 0.8117 0.4545 0.113 Uiso 0.360(3) 1 calc PR D 6 Cl7B Cl 0.7748(6) 0.8271(3) 0.5007(3) 0.1186(7) Uani 0.360(3) 1 d PDU D 6 Cl8B Cl 0.7866(4) 0.7310(2) 0.43719(19) 0.1199(9) Uani 0.360(3) 1 d PDU D 6 C102 C 0.3418(12) 0.3592(6) 0.4633(4) 0.295(4) Uani 1 1 d DU . . H10G H 0.3523 0.3510 0.4963 0.443 Uiso 1 1 calc R . . H10H H 0.2856 0.3846 0.4560 0.443 Uiso 1 1 calc R . . H10I H 0.3958 0.3812 0.4543 0.443 Uiso 1 1 calc R . . C103 C 0.3296(13) 0.3015(6) 0.4388(4) 0.295(4) Uani 1 1 d DU . . H10J H 0.3793 0.2730 0.4525 0.354 Uiso 1 1 calc R . . H10K H 0.2692 0.2836 0.4446 0.354 Uiso 1 1 calc R . . O1 O 0.3308(9) 0.3013(4) 0.3924(3) 0.295(4) Uani 1 1 d DU . . C104 C 0.2970(12) 0.2412(6) 0.3717(4) 0.295(4) Uani 1 1 d DU . . H10L H 0.2280 0.2408 0.3648 0.354 Uiso 1 1 calc R . . H10M H 0.3173 0.2064 0.3924 0.354 Uiso 1 1 calc R . . C105 C 0.3414(11) 0.2378(7) 0.3286(4) 0.295(4) Uani 1 1 d DU . . H10N H 0.3227 0.1993 0.3124 0.443 Uiso 1 1 calc R . . H10O H 0.4096 0.2387 0.3362 0.443 Uiso 1 1 calc R . . H10P H 0.3210 0.2730 0.3089 0.443 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 Cr1 0.0366(3) 0.0324(3) 0.0299(3) 0.0017(2) 0.0043(2) 0.0031(2) Cr2 0.0482(3) 0.0306(3) 0.0321(3) -0.0005(3) 0.0088(3) -0.0004(3) Cl1 0.0394(5) 0.0475(5) 0.0461(6) 0.0082(4) 0.0067(4) 0.0015(4) Cl2 0.0559(6) 0.0388(5) 0.0399(6) -0.0018(4) 0.0106(4) -0.0057(4) Cl3 0.0518(6) 0.0391(5) 0.0418(6) 0.0026(4) 0.0042(5) 0.0015(4) Cl4 0.0546(5) 0.0368(5) 0.0340(5) -0.0003(4) 0.0073(4) 0.0053(4) N1 0.0447(16) 0.0369(15) 0.0288(17) 0.0019(13) 0.0030(13) 0.0070(13) N2 0.0384(15) 0.0357(15) 0.0302(17) 0.0009(13) 0.0044(13) 0.0019(13) N3 0.0390(16) 0.0459(17) 0.0285(17) -0.0063(14) 0.0024(13) -0.0017(14) N4 0.0387(15) 0.0336(15) 0.0275(16) -0.0019(12) 0.0009(13) 0.0025(12) N5 0.068(2) 0.0320(15) 0.0327(18) 0.0015(13) 0.0105(15) 0.0030(15) N6 0.0618(19) 0.0333(16) 0.0348(17) -0.0041(13) 0.0176(15) -0.0005(14) N7 0.0542(18) 0.0426(17) 0.0311(18) -0.0042(14) 0.0090(15) -0.0048(15) N8 0.0490(18) 0.0379(15) 0.0331(17) -0.0020(13) 0.0121(14) -0.0024(13) C1 0.0398(18) 0.0344(17) 0.0294(19) -0.0023(15) 0.0059(15) 0.0017(15) C2 0.048(2) 0.044(2) 0.034(2) 0.0073(17) 0.0024(17) 0.0147(17) C3 0.048(2) 0.043(2) 0.030(2) 0.0061(16) 0.0033(17) 0.0044(17) C4 0.0393(19) 0.0404(19) 0.035(2) 0.0093(16) 0.0056(16) 0.0131(15) C5 0.0388(19) 0.0434(19) 0.034(2) 0.0067(16) 0.0044(16) 0.0158(15) C6 0.043(2) 0.061(2) 0.039(2) -0.0014(19) 0.0016(18) 0.0136(18) C7 0.040(2) 0.075(3) 0.051(3) -0.003(2) 0.013(2) 0.007(2) C8 0.034(2) 0.069(3) 0.052(3) -0.005(2) 0.0050(18) 0.0063(19) C10 0.055(2) 0.045(2) 0.030(2) 0.0050(17) 0.0081(18) 0.0117(17) C11 0.053(2) 0.049(2) 0.042(2) -0.0043(19) 0.0083(19) 0.0002(19) C12 0.092(3) 0.043(2) 0.053(3) 0.011(2) 0.014(2) 0.016(2) C9 0.039(2) 0.047(2) 0.042(2) 0.0025(17) 0.0017(17) 0.0110(17) C13 0.042(2) 0.058(2) 0.052(3) -0.0112(19) 0.0089(19) 0.0078(19) C14 0.061(3) 0.078(3) 0.047(3) -0.011(2) 0.003(2) 0.008(2) C15 0.050(2) 0.063(3) 0.061(3) -0.011(2) 0.003(2) 0.002(2) C16 0.0383(18) 0.0409(19) 0.0261(19) 0.0026(16) 0.0073(15) -0.0010(15) C17 0.0376(18) 0.0315(17) 0.032(2) -0.0019(15) 0.0078(15) 0.0000(15) C18 0.0334(18) 0.051(2) 0.030(2) -0.0058(16) 0.0061(16) 0.0004(16) C19 0.0342(19) 0.052(2) 0.044(2) -0.0068(18) 0.0089(17) 0.0007(16) C20 0.049(2) 0.062(2) 0.050(2) 0.000(2) 0.014(2) -0.012(2) C21 0.046(2) 0.081(3) 0.040(2) -0.005(2) 0.0131(19) -0.007(2) C22 0.047(2) 0.063(2) 0.045(2) -0.014(2) 0.0125(19) -0.0063(19) C23 0.039(2) 0.050(2) 0.038(2) -0.0056(17) 0.0070(17) 0.0005(17) C24 0.039(2) 0.050(2) 0.053(2) -0.0091(19) 0.0076(18) -0.0053(18) C25 0.055(3) 0.053(2) 0.075(3) -0.012(2) 0.006(2) -0.004(2) C26 0.056(3) 0.057(3) 0.061(3) -0.009(2) 0.000(2) -0.007(2) C27 0.058(2) 0.045(2) 0.040(2) -0.0054(18) 0.0128(19) -0.0011(18) C28 0.066(3) 0.055(2) 0.044(3) -0.015(2) 0.014(2) -0.019(2) C29 0.088(3) 0.057(3) 0.058(3) -0.012(2) 0.017(3) 0.013(2) C30 0.0400(19) 0.0407(18) 0.027(2) -0.0021(16) 0.0046(15) -0.0040(15) C31 0.0406(19) 0.0415(18) 0.027(2) -0.0012(15) 0.0051(16) -0.0017(15) C32 0.047(2) 0.046(2) 0.037(2) -0.0067(18) 0.0095(17) -0.0065(17) C33 0.036(2) 0.057(2) 0.044(2) -0.0071(19) 0.0041(18) -0.0074(18) C34 0.041(2) 0.057(2) 0.041(2) 0.0003(19) 0.0019(18) 0.0049(18) C35 0.044(2) 0.0391(18) 0.038(2) -0.0014(16) 0.0050(17) -0.0010(16) C36 0.047(2) 0.048(2) 0.052(3) -0.0019(19) -0.0023(19) 0.0126(18) C37 0.060(3) 0.066(3) 0.070(3) -0.012(2) 0.008(2) 0.020(2) C38 0.057(3) 0.051(2) 0.077(3) 0.009(2) -0.007(2) 0.007(2) C39 0.045(2) 0.0361(18) 0.040(2) -0.0078(16) 0.0086(17) -0.0009(16) C40 0.053(2) 0.044(2) 0.051(3) -0.0128(19) 0.009(2) -0.0016(18) C41 0.056(2) 0.047(2) 0.056(3) 0.0095(19) 0.016(2) 0.0094(19) C51 0.053(2) 0.0280(17) 0.035(2) -0.0021(15) 0.0103(16) 0.0082(15) C52 0.089(3) 0.038(2) 0.039(2) 0.0011(18) 0.019(2) -0.007(2) C53 0.086(3) 0.038(2) 0.037(2) -0.0014(17) 0.022(2) -0.013(2) C54 0.074(2) 0.0363(18) 0.028(2) 0.0075(15) 0.0088(18) 0.0033(17) C56 0.105(3) 0.051(2) 0.041(3) -0.001(2) 0.014(2) -0.019(2) C57 0.093(3) 0.067(3) 0.044(3) 0.022(2) -0.017(3) -0.017(3) C58 0.083(3) 0.074(3) 0.058(3) 0.021(2) -0.009(2) 0.011(3) C55A 0.080(2) 0.043(2) 0.041(2) -0.0011(17) 0.0198(19) -0.0048(19) C60A 0.086(3) 0.047(2) 0.056(4) -0.024(2) 0.043(3) -0.009(2) C61A 0.041(4) 0.082(4) 0.062(4) 0.021(3) 0.005(3) -0.006(3) C62A 0.096(4) 0.050(4) 0.050(4) 0.002(3) 0.028(3) 0.004(3) C55B 0.080(2) 0.043(2) 0.041(2) -0.0011(17) 0.0198(19) -0.0048(19) C60B 0.086(3) 0.047(2) 0.056(4) -0.024(2) 0.043(3) -0.009(2) C61B 0.041(4) 0.082(4) 0.062(4) 0.021(3) 0.005(3) -0.006(3) C62B 0.096(4) 0.050(4) 0.050(4) 0.002(3) 0.028(3) 0.004(3) C59A 0.080(3) 0.057(2) 0.041(3) 0.0105(19) -0.001(2) 0.013(2) C63A 0.100(3) 0.067(3) 0.064(3) -0.003(2) -0.002(3) 0.042(3) C64A 0.109(4) 0.119(5) 0.085(4) 0.007(3) 0.005(3) 0.067(3) C65A 0.147(7) 0.053(3) 0.129(6) 0.003(3) 0.019(5) 0.042(4) C59B 0.080(3) 0.057(2) 0.041(3) 0.0105(19) -0.001(2) 0.013(2) C63B 0.100(3) 0.067(3) 0.064(3) -0.003(2) -0.002(3) 0.042(3) C64B 0.109(4) 0.119(5) 0.085(4) 0.007(3) 0.005(3) 0.067(3) C65B 0.147(7) 0.053(3) 0.129(6) 0.003(3) 0.019(5) 0.042(4) C66 0.048(2) 0.0345(19) 0.045(2) -0.0041(17) 0.0142(17) -0.0028(17) C67 0.051(2) 0.0322(18) 0.035(2) 0.0033(16) 0.0141(17) 0.0004(16) C68 0.058(2) 0.048(2) 0.026(2) -0.0036(17) 0.0067(18) -0.0122(17) C69 0.067(2) 0.043(2) 0.033(2) -0.0108(17) 0.0070(19) -0.0095(18) C70 0.080(3) 0.047(2) 0.050(3) -0.001(2) 0.009(2) -0.018(2) C71 0.070(3) 0.064(3) 0.061(3) 0.006(2) -0.001(3) -0.027(2) C72 0.055(2) 0.079(3) 0.050(3) 0.008(2) -0.002(2) -0.017(2) C73 0.057(2) 0.057(2) 0.037(2) 0.0022(19) 0.000(2) -0.0088(19) C74 0.049(3) 0.077(3) 0.082(3) 0.022(3) 0.005(2) -0.003(2) C75 0.073(3) 0.092(4) 0.157(5) 0.031(4) 0.046(4) 0.029(3) C76 0.067(3) 0.125(5) 0.116(4) 0.065(4) -0.034(3) -0.030(3) C77 0.074(3) 0.041(2) 0.051(3) -0.0058(19) 0.017(2) 0.001(2) C78 0.103(4) 0.048(3) 0.090(4) -0.015(3) 0.029(3) 0.005(3) C79 0.064(3) 0.068(3) 0.049(3) -0.002(2) 0.014(2) 0.003(2) C80 0.048(2) 0.0387(19) 0.034(2) -0.0028(16) 0.0089(17) -0.0048(16) C81 0.053(2) 0.0335(18) 0.035(2) -0.0044(16) 0.0088(17) -0.0053(16) C82 0.058(2) 0.040(2) 0.034(2) -0.0032(17) 0.0084(18) 0.0007(18) C83 0.063(3) 0.056(2) 0.047(2) -0.006(2) 0.022(2) 0.001(2) C84 0.054(2) 0.062(3) 0.054(3) 0.006(2) 0.017(2) 0.017(2) C85 0.052(2) 0.050(2) 0.038(2) 0.0004(18) 0.0119(17) 0.0026(18) C86 0.057(2) 0.0349(19) 0.039(2) -0.0035(17) 0.0097(18) 0.0017(17) C87 0.068(3) 0.041(2) 0.052(3) 0.003(2) 0.007(2) 0.000(2) C88 0.054(2) 0.049(2) 0.053(3) -0.001(2) 0.006(2) 0.0027(19) C89 0.063(3) 0.084(3) 0.054(3) 0.015(3) 0.008(2) 0.008(2) C90 0.090(3) 0.087(3) 0.076(3) 0.028(3) 0.037(3) 0.036(3) C91 0.084(4) 0.107(4) 0.089(4) 0.003(4) -0.017(3) 0.008(3) C100 0.063(3) 0.055(2) 0.047(3) -0.002(2) 0.005(2) -0.002(2) Cl5 0.0674(7) 0.0579(7) 0.0763(9) 0.0092(6) -0.0031(6) -0.0064(6) Cl6 0.0802(8) 0.0716(7) 0.0668(8) -0.0264(6) 0.0147(6) -0.0056(6) C10A 0.110(4) 0.102(4) 0.076(5) -0.003(3) 0.031(4) 0.029(3) Cl7A 0.1277(13) 0.0990(13) 0.1415(17) -0.0185(12) 0.0642(12) 0.0127(11) Cl8A 0.136(2) 0.0991(16) 0.134(2) -0.0148(14) 0.0534(15) 0.0230(14) C10B 0.110(4) 0.102(4) 0.076(5) -0.003(3) 0.031(4) 0.029(3) Cl7B 0.1277(13) 0.0990(13) 0.1415(17) -0.0185(12) 0.0642(12) 0.0127(11) Cl8B 0.136(2) 0.0991(16) 0.134(2) -0.0148(14) 0.0534(15) 0.0230(14) C102 0.353(8) 0.273(7) 0.246(7) -0.074(6) -0.011(7) 0.018(6) C103 0.353(8) 0.273(7) 0.246(7) -0.074(6) -0.011(7) 0.018(6) O1 0.353(8) 0.273(7) 0.246(7) -0.074(6) -0.011(7) 0.018(6) C104 0.353(8) 0.273(7) 0.246(7) -0.074(6) -0.011(7) 0.018(6) C105 0.353(8) 0.273(7) 0.246(7) -0.074(6) -0.011(7) 0.018(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C1 2.093(4) . ? Cr1 N4 2.124(3) . ? Cr1 Cl4 2.2645(15) . ? Cr1 Cl1 2.3500(17) . ? Cr1 Cl2 2.3996(16) . ? Cr1 Cl3 2.4126(15) . ? Cr2 N8 2.050(3) . ? Cr2 C51 2.120(4) . ? Cr2 Cl3 2.3824(15) . ? Cr2 Cl2 2.4241(16) . ? Cr2 Cl1 2.6311(17) . ? N1 C1 1.366(5) . ? N1 C2 1.394(5) . ? N1 C4 1.457(5) . ? N2 C1 1.356(5) . ? N2 C3 1.381(5) . ? N2 C16 1.444(5) . ? N3 C17 1.342(5) . ? N3 C18 1.436(5) . ? N3 H903 0.8800 . ? N4 C17 1.308(5) . ? N4 C30 1.463(5) . ? N5 C51 1.372(5) . ? N5 C52 1.378(5) . ? N5 C54 1.442(5) . ? N6 C51 1.362(5) . ? N6 C53 1.381(5) . ? N6 C66 1.439(5) . ? N7 C67 1.292(5) . ? N7 C68 1.402(5) . ? N7 H907 0.8800 . ? N8 C67 1.340(5) . ? N8 C80 1.447(5) . ? C2 C3 1.327(6) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.379(4) . ? C4 C5 1.415(5) . ? C5 C6 1.397(6) . ? C5 C10 1.502(6) . ? C6 C7 1.368(6) . ? C6 H6 0.9500 . ? C7 C8 1.370(6) . ? C7 H7 0.9500 . ? C8 C9 1.398(5) . ? C8 H8 0.9500 . ? C10 C11 1.535(5) . ? C10 C12 1.536(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C9 C13 1.5274(14) . ? C13 C14 1.5243(15) . ? C13 C15 1.5374(18) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.512(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 C19 1.401(5) . ? C18 C23 1.402(5) . ? C19 C20 1.385(6) . ? C19 C24 1.517(6) . ? C20 C21 1.394(6) . ? C20 H20 0.9500 . ? C21 C22 1.362(6) . ? C21 H21 0.9500 . ? C22 C23 1.405(6) . ? C22 H22 0.9500 . ? C23 C27 1.523(6) . ? C24 C26 1.523(6) . ? C24 C25 1.524(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.534(6) . ? C27 C28 1.537(6) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.406(5) . ? C30 C31 1.412(5) . ? C31 C32 1.400(5) . ? C31 C39 1.512(5) . ? C32 C33 1.375(6) . ? C32 H32 0.9500 . ? C33 C34 1.372(6) . ? C33 H33 0.9500 . ? C34 C35 1.394(5) . ? C34 H34 0.9500 . ? C35 C36 1.537(5) . ? C36 C38 1.526(6) . ? C36 C37 1.548(6) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.527(6) . ? C39 C40 1.527(5) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C52 C53 1.336(6) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C59A 1.393(5) . ? C54 C55A 1.405(4) . ? C56 C57 1.360(7) . ? C56 C55A 1.403(5) . ? C56 H56 0.9500 . ? C57 C58 1.352(7) . ? C57 H57 0.9500 . ? C58 C59A 1.397(6) . ? C58 H58 0.9500 . ? C55A C60A 1.5274(14) . ? C60A C61A 1.5240(16) . ? C60A C62A 1.5374(17) . ? C60A H60A 1.0000 . ? C61A H61A 0.9800 . ? C61A H61B 0.9800 . ? C61A H61C 0.9800 . ? C62A H62A 0.9800 . ? C62A H62B 0.9800 . ? C62A H62C 0.9800 . ? C60B C61B 1.5240(15) . ? C60B C62B 1.5374(18) . ? C60B H60B 1.0000 . ? C61B H61D 0.9800 . ? C61B H61E 0.9800 . ? C61B H61F 0.9800 . ? C62B H62D 0.9800 . ? C62B H62E 0.9800 . ? C62B H62F 0.9800 . ? C59A C63A 1.5273(15) . ? C63A C64A 1.5240(16) . ? C63A C65A 1.5374(17) . ? C63A H63A 1.0000 . ? C64A H64A 0.9800 . ? C64A H64B 0.9800 . ? C64A H64C 0.9800 . ? C65A H65A 0.9800 . ? C65A H65B 0.9800 . ? C65A H65C 0.9800 . ? C63B C64B 1.5240(16) . ? C63B C65B 1.5374(18) . ? C63B H63B 1.0000 . ? C64B H64D 0.9800 . ? C64B H64E 0.9800 . ? C64B H64F 0.9800 . ? C65B H65D 0.9800 . ? C65B H65E 0.9800 . ? C65B H65F 0.9800 . ? C66 C67 1.533(5) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C68 C73 1.397(6) . ? C68 C69 1.424(6) . ? C69 C70 1.397(6) . ? C69 C77 1.511(6) . ? C70 C71 1.376(7) . ? C70 H70 0.9500 . ? C71 C72 1.369(7) . ? C71 H71 0.9500 . ? C72 C73 1.400(6) . ? C72 H72 0.9500 . ? C73 C74 1.508(7) . ? C74 C76 1.524(8) . ? C74 C75 1.549(8) . ? C74 H74 1.0000 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C79 1.519(6) . ? C77 C78 1.531(6) . ? C77 H77 1.0000 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C85 1.404(6) . ? C80 C81 1.411(5) . ? C81 C82 1.393(6) . ? C81 C86 1.519(6) . ? C82 C83 1.366(6) . ? C82 H82 0.9500 . ? C83 C84 1.366(6) . ? C83 H83 0.9500 . ? C84 C85 1.397(6) . ? C84 H84 0.9500 . ? C85 C89 1.507(6) . ? C86 C88 1.518(6) . ? C86 C87 1.525(5) . ? C86 H86 1.0000 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 C91 1.518(8) . ? C89 C90 1.535(7) . ? C89 H89 1.0000 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C100 Cl6 1.759(4) . ? C100 Cl5 1.764(4) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C10A Cl7A 1.746(6) . ? C10A Cl8A 1.757(7) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C10B Cl7B 1.751(8) . ? C10B Cl8B 1.757(8) . ? C10B H10E 0.9900 . ? C10B H10F 0.9900 . ? C102 C103 1.443(12) . ? C102 H10G 0.9800 . ? C102 H10H 0.9800 . ? C102 H10I 0.9800 . ? C103 O1 1.367(11) . ? C103 H10J 0.9900 . ? C103 H10K 0.9900 . ? O1 C104 1.490(12) . ? C104 C105 1.499(14) . ? C104 H10L 0.9900 . ? C104 H10M 0.9900 . ? C105 H10N 0.9800 . ? C105 H10O 0.9800 . ? C105 H10P 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 C1 Cr1 N4 84.41(13) . . ? C1 Cr1 Cl4 94.73(11) . . ? N4 Cr1 Cl4 93.24(9) . . ? C1 Cr1 Cl1 92.06(11) . . ? N4 Cr1 Cl1 172.72(9) . . ? Cl4 Cr1 Cl1 93.39(5) . . ? C1 Cr1 Cl2 93.90(11) . . ? N4 Cr1 Cl2 86.97(9) . . ? Cl4 Cr1 Cl2 171.35(4) . . ? Cl1 Cr1 Cl2 86.93(5) . . ? C1 Cr1 Cl3 176.66(10) . . ? N4 Cr1 Cl3 96.20(9) . . ? Cl4 Cr1 Cl3 88.52(6) . . ? Cl1 Cr1 Cl3 86.97(5) . . ? Cl2 Cr1 Cl3 82.86(6) . . ? N8 Cr2 C51 89.76(14) . . ? N8 Cr2 Cl3 169.29(10) . . ? C51 Cr2 Cl3 96.33(12) . . ? N8 Cr2 Cl2 91.19(10) . . ? C51 Cr2 Cl2 178.21(10) . . ? Cl3 Cr2 Cl2 82.97(6) . . ? N8 Cr2 Cl1 106.45(10) . . ? C51 Cr2 Cl1 97.86(11) . . ? Cl3 Cr2 Cl1 81.49(6) . . ? Cl2 Cr2 Cl1 80.42(5) . . ? Cr1 Cl1 Cr2 77.00(6) . . ? Cr1 Cl2 Cr2 80.24(6) . . ? Cr2 Cl3 Cr1 80.82(6) . . ? C1 N1 C2 110.5(3) . . ? C1 N1 C4 128.6(3) . . ? C2 N1 C4 120.8(3) . . ? C1 N2 C3 111.5(3) . . ? C1 N2 C16 125.1(3) . . ? C3 N2 C16 123.0(3) . . ? C17 N3 C18 131.2(3) . . ? C17 N3 H903 114.4 . . ? C18 N3 H903 114.4 . . ? C17 N4 C30 113.1(3) . . ? C17 N4 Cr1 122.4(2) . . ? C30 N4 Cr1 124.3(2) . . ? C51 N5 C52 111.3(3) . . ? C51 N5 C54 126.9(3) . . ? C52 N5 C54 121.6(3) . . ? C51 N6 C53 111.8(3) . . ? C51 N6 C66 123.2(3) . . ? C53 N6 C66 124.7(3) . . ? C67 N7 C68 123.0(3) . . ? C67 N7 H907 118.5 . . ? C68 N7 H907 118.5 . . ? C67 N8 C80 114.8(3) . . ? C67 N8 Cr2 125.9(3) . . ? C80 N8 Cr2 119.0(2) . . ? N2 C1 N1 103.9(3) . . ? N2 C1 Cr1 119.9(3) . . ? N1 C1 Cr1 136.0(3) . . ? C3 C2 N1 107.1(3) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 107.1(3) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C9 C4 C5 123.4(3) . . ? C9 C4 N1 118.6(3) . . ? C5 C4 N1 117.8(3) . . ? C6 C5 C4 115.7(4) . . ? C6 C5 C10 120.7(4) . . ? C4 C5 C10 123.5(3) . . ? C7 C6 C5 122.4(4) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C6 C7 C8 119.6(4) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 121.8(4) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C5 C10 C11 113.4(3) . . ? C5 C10 C12 110.4(3) . . ? C11 C10 C12 108.7(3) . . ? C5 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C9 C8 117.0(3) . . ? C4 C9 C13 122.9(2) . . ? C8 C9 C13 119.8(3) . . ? C14 C13 C9 110.76(11) . . ? C14 C13 C15 109.17(12) . . ? C9 C13 C15 111.87(12) . . ? C14 C13 H13 108.3 . . ? C9 C13 H13 108.3 . . ? C15 C13 H13 108.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 113.9(3) . . ? N2 C16 H16A 108.8 . . ? C17 C16 H16A 108.8 . . ? N2 C16 H16B 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N4 C17 N3 122.3(3) . . ? N4 C17 C16 120.4(3) . . ? N3 C17 C16 117.2(3) . . ? C19 C18 C23 122.6(4) . . ? C19 C18 N3 117.0(3) . . ? C23 C18 N3 120.2(3) . . ? C20 C19 C18 117.8(4) . . ? C20 C19 C24 121.1(4) . . ? C18 C19 C24 120.8(4) . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.5(4) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C18 C23 C22 116.8(4) . . ? C18 C23 C27 124.6(4) . . ? C22 C23 C27 118.3(4) . . ? C19 C24 C26 109.1(3) . . ? C19 C24 C25 116.1(4) . . ? C26 C24 C25 108.9(3) . . ? C19 C24 H24 107.5 . . ? C26 C24 H24 107.5 . . ? C25 C24 H24 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.0(4) . . ? C23 C27 C28 113.1(3) . . ? C29 C27 C28 109.0(4) . . ? C23 C27 H27 107.9 . . ? C29 C27 H27 107.9 . . ? C28 C27 H27 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 122.2(3) . . ? C35 C30 N4 121.9(3) . . ? C31 C30 N4 115.5(3) . . ? C32 C31 C30 116.6(3) . . ? C32 C31 C39 120.5(3) . . ? C30 C31 C39 122.9(3) . . ? C33 C32 C31 122.1(4) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C34 C33 C32 120.0(4) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 121.5(4) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C34 C35 C30 117.6(3) . . ? C34 C35 C36 117.7(3) . . ? C30 C35 C36 124.6(3) . . ? C38 C36 C35 111.3(4) . . ? C38 C36 C37 109.1(4) . . ? C35 C36 C37 110.6(4) . . ? C38 C36 H36 108.6 . . ? C35 C36 H36 108.6 . . ? C37 C36 H36 108.6 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C31 C39 C41 113.8(3) . . ? C31 C39 C40 112.4(3) . . ? C41 C39 C40 108.8(3) . . ? C31 C39 H39 107.2 . . ? C41 C39 H39 107.2 . . ? C40 C39 H39 107.2 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N6 C51 N5 103.0(3) . . ? N6 C51 Cr2 116.8(3) . . ? N5 C51 Cr2 140.2(3) . . ? C53 C52 N5 107.2(4) . . ? C53 C52 H52 126.4 . . ? N5 C52 H52 126.4 . . ? C52 C53 N6 106.7(4) . . ? C52 C53 H53 126.6 . . ? N6 C53 H53 126.6 . . ? C59A C54 C55A 123.5(3) . . ? C59A C54 N5 119.5(3) . . ? C55A C54 N5 117.0(3) . . ? C57 C56 C55A 121.3(4) . . ? C57 C56 H56 119.4 . . ? C55A C56 H56 119.4 . . ? C58 C57 C56 121.7(5) . . ? C58 C57 H57 119.2 . . ? C56 C57 H57 119.2 . . ? C57 C58 C59A 121.0(5) . . ? C57 C58 H58 119.5 . . ? C59A C58 H58 119.5 . . ? C56 C55A C54 115.8(3) . . ? C56 C55A C60A 126.6(2) . . ? C54 C55A C60A 117.0(2) . . ? C61A C60A C55A 110.88(11) . . ? C61A C60A C62A 109.18(13) . . ? C55A C60A C62A 111.88(12) . . ? C61A C60A H60A 108.3 . . ? C55A C60A H60A 108.3 . . ? C62A C60A H60A 108.3 . . ? C60A C61A H61A 109.5 . . ? C60A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C60A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? C60A C62A H62A 109.5 . . ? C60A C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C60A C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? C61B C60B C62B 109.20(13) . . ? C61B C60B H60B 108.3 . . ? C62B C60B H60B 108.3 . . ? C60B C61B H61D 109.5 . . ? C60B C61B H61E 109.5 . . ? H61D C61B H61E 109.5 . . ? C60B C61B H61F 109.5 . . ? H61D C61B H61F 109.5 . . ? H61E C61B H61F 109.5 . . ? C60B C62B H62D 109.5 . . ? C60B C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? C60B C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? C54 C59A C58 116.8(3) . . ? C54 C59A C63A 119.0(2) . . ? C58 C59A C63A 124.1(3) . . ? C64A C63A C59A 110.93(12) . . ? C64A C63A C65A 109.20(13) . . ? C59A C63A C65A 111.79(13) . . ? C64A C63A H63A 108.3 . . ? C59A C63A H63A 108.3 . . ? C65A C63A H63A 108.3 . . ? 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 . . ? C63A C65A H65A 109.5 . . ? C63A C65A H65B 109.5 . . ? H65A C65A H65B 109.5 . . ? C63A C65A H65C 109.5 . . ? H65A C65A H65C 109.5 . . ? H65B C65A H65C 109.5 . . ? C64B C63B C65B 109.19(14) . . ? C64B C63B H63B 108.3 . . ? C65B C63B H63B 108.3 . . ? 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 . . ? C63B C65B H65D 109.5 . . ? C63B C65B H65E 109.5 . . ? H65D C65B H65E 109.5 . . ? C63B C65B H65F 109.5 . . ? H65D C65B H65F 109.5 . . ? H65E C65B H65F 109.5 . . ? N6 C66 C67 114.8(3) . . ? N6 C66 H66A 108.6 . . ? C67 C66 H66A 108.6 . . ? N6 C66 H66B 108.6 . . ? C67 C66 H66B 108.6 . . ? H66A C66 H66B 107.6 . . ? N7 C67 N8 125.2(3) . . ? N7 C67 C66 120.8(3) . . ? N8 C67 C66 114.0(3) . . ? C73 C68 N7 123.4(4) . . ? C73 C68 C69 120.2(4) . . ? N7 C68 C69 116.1(4) . . ? C70 C69 C68 118.3(4) . . ? C70 C69 C77 121.7(4) . . ? C68 C69 C77 120.0(4) . . ? C71 C70 C69 121.5(4) . . ? C71 C70 H70 119.2 . . ? C69 C70 H70 119.2 . . ? C72 C71 C70 119.5(4) . . ? C72 C71 H71 120.2 . . ? C70 C71 H71 120.2 . . ? C71 C72 C73 122.0(5) . . ? C71 C72 H72 119.0 . . ? C73 C72 H72 119.0 . . ? C68 C73 C72 118.4(4) . . ? C68 C73 C74 122.7(4) . . ? C72 C73 C74 118.8(4) . . ? C73 C74 C76 110.2(5) . . ? C73 C74 C75 111.8(4) . . ? C76 C74 C75 111.6(5) . . ? C73 C74 H74 107.7 . . ? C76 C74 H74 107.7 . . ? C75 C74 H74 107.7 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C69 C77 C79 111.7(4) . . ? C69 C77 C78 112.7(4) . . ? C79 C77 C78 111.4(4) . . ? C69 C77 H77 106.9 . . ? C79 C77 H77 106.9 . . ? C78 C77 H77 106.9 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C85 C80 C81 119.9(4) . . ? C85 C80 N8 120.3(3) . . ? C81 C80 N8 119.8(3) . . ? C82 C81 C80 118.5(4) . . ? C82 C81 C86 118.9(3) . . ? C80 C81 C86 122.6(3) . . ? C83 C82 C81 121.5(4) . . ? C83 C82 H82 119.2 . . ? C81 C82 H82 119.2 . . ? C84 C83 C82 119.9(4) . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C83 C84 C85 121.5(4) . . ? C83 C84 H84 119.3 . . ? C85 C84 H84 119.3 . . ? C84 C85 C80 118.5(4) . . ? C84 C85 C89 119.3(4) . . ? C80 C85 C89 122.1(4) . . ? C88 C86 C81 110.0(3) . . ? C88 C86 C87 110.2(3) . . ? C81 C86 C87 112.6(3) . . ? C88 C86 H86 108.0 . . ? C81 C86 H86 108.0 . . ? C87 C86 H86 108.0 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C85 C89 C91 108.2(4) . . ? C85 C89 C90 113.4(4) . . ? C91 C89 C90 110.2(4) . . ? C85 C89 H89 108.3 . . ? C91 C89 H89 108.3 . . ? C90 C89 H89 108.3 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C89 C91 H91A 109.5 . . ? C89 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C89 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? Cl6 C100 Cl5 111.1(2) . . ? Cl6 C100 H10A 109.4 . . ? Cl5 C100 H10A 109.4 . . ? Cl6 C100 H10B 109.4 . . ? Cl5 C100 H10B 109.4 . . ? H10A C100 H10B 108.0 . . ? Cl7A C10A Cl8A 107.8(4) . . ? Cl7A C10A H10C 110.1 . . ? Cl8A C10A H10C 110.1 . . ? Cl7A C10A H10D 110.1 . . ? Cl8A C10A H10D 110.1 . . ? H10C C10A H10D 108.5 . . ? Cl7B C10B Cl8B 106.9(6) . . ? Cl7B C10B H10E 110.3 . . ? Cl8B C10B H10E 110.3 . . ? Cl7B C10B H10F 110.3 . . ? Cl8B C10B H10F 110.3 . . ? H10E C10B H10F 108.6 . . ? C103 C102 H10G 109.5 . . ? C103 C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? C103 C102 H10I 109.5 . . ? H10G C102 H10I 109.5 . . ? H10H C102 H10I 109.5 . . ? O1 C103 C102 119.1(12) . . ? O1 C103 H10J 107.5 . . ? C102 C103 H10J 107.5 . . ? O1 C103 H10K 107.5 . . ? C102 C103 H10K 107.5 . . ? H10J C103 H10K 107.0 . . ? C103 O1 C104 111.4(10) . . ? O1 C104 C105 103.7(11) . . ? O1 C104 H10L 111.0 . . ? C105 C104 H10L 111.0 . . ? O1 C104 H10M 111.0 . . ? C105 C104 H10M 111.0 . . ? H10L C104 H10M 109.0 . . ? C104 C105 H10N 109.5 . . ? C104 C105 H10O 109.5 . . ? H10N C105 H10O 109.5 . . ? C104 C105 H10P 109.5 . . ? H10N C105 H10P 109.5 . . ? H10O C105 H10P 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.870 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.075 #==END