# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yi-Chou Tsai' _publ_contact_author_email yictsai@mx.nthu.edu.tw _publ_section_title ; Reductive N-N Bond Cleavage and Coupling of Organic Azides Mediated by Chromium(I) and Vanadium(I) -Diketiminate ; loop_ _publ_author_name 'Yi-Chou Tsai.' 'Kuan-Ming Lin.' 'Yun-Jen Shieh.' 'Hong-Zhang Chen.' ; Ting-Shen Kuo ; 'Po-Yang Wang.' # Attachment 'cpd_9_CCDC_764151.cif' data_7329 _database_code_depnum_ccdc_archive 'CCDC 764151' #TrackingRef 'cpd_9_CCDC_764151.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H98 Cr2 N10 O2' _chemical_formula_sum 'C66 H98 Cr2 N10 O2' _chemical_formula_weight 1167.54 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' Cr Cr 0.3209 0.6236 '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' Si Si 0.0817 0.0704 '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 12.5550(2) _cell_length_b 15.3520(2) _cell_length_c 20.1740(4) _cell_angle_alpha 75.3030(10) _cell_angle_beta 74.1560(10) _cell_angle_gamma 67.1920(10) _cell_volume 3399.93(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 59084 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour green(dark) _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6874 _exptl_absorpt_correction_T_max 0.9635 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36768 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.43 _reflns_number_total 12143 _reflns_number_gt 9066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1605P)^2^+4.7169P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12143 _refine_ls_number_parameters 746 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0907 _refine_ls_wR_factor_ref 0.2796 _refine_ls_wR_factor_gt 0.2529 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.060 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 0.15255(6) 0.32791(5) 0.47691(4) 0.0379(2) Uani 1 1 d . . . Cr2 Cr 0.54544(6) 0.82461(5) 0.97794(4) 0.0375(2) Uani 1 1 d . . . O1 O 0.1272(4) 0.3950(3) 0.35802(18) 0.0623(10) Uani 1 1 d . . . O2 O 0.6073(4) 0.8903(3) 0.85731(19) 0.0624(10) Uani 1 1 d . D . N1 N 0.1327(3) 0.1987(3) 0.4842(2) 0.0419(9) Uani 1 1 d . . . N2 N 0.3337(3) 0.2642(3) 0.4597(2) 0.0422(9) Uani 1 1 d . . . N3 N 0.1679(4) 0.4558(3) 0.4849(2) 0.0511(10) Uani 1 1 d . . . N4 N 0.0965(3) 0.5316(3) 0.48747(19) 0.0374(8) Uani 1 1 d . . . N5 N 0.0297(4) 0.6093(3) 0.4896(3) 0.0555(11) Uani 1 1 d . . . N6 N 0.4414(3) 0.7582(2) 0.96314(19) 0.0394(8) Uani 1 1 d . . . N7 N 0.6846(3) 0.6969(2) 0.98481(19) 0.0388(8) Uani 1 1 d . . . N8 N 0.6369(4) 0.8919(3) 1.0082(3) 0.0568(11) Uani 1 1 d . . . N9 N 0.6166(3) 0.9710(3) 1.0105(2) 0.0390(8) Uani 1 1 d . . . N10 N 0.6014(4) 1.0502(3) 1.0127(3) 0.0568(11) Uani 1 1 d . . . C1 C 0.0192(4) 0.1885(3) 0.5192(2) 0.0447(11) Uani 1 1 d . . . C2 C -0.0638(5) 0.2021(4) 0.4802(3) 0.0527(12) Uani 1 1 d . . . C3 C -0.0419(6) 0.2258(5) 0.4014(3) 0.0659(15) Uani 1 1 d . . . H3 H 0.0420 0.2228 0.3847 0.079 Uiso 1 1 calc R . . C4 C -0.1208(7) 0.3289(5) 0.3770(4) 0.083(2) Uani 1 1 d . . . H4A H -0.1048 0.3430 0.3258 0.125 Uiso 1 1 calc R . . H4B H -0.1040 0.3744 0.3954 0.125 Uiso 1 1 calc R . . H4C H -0.2038 0.3347 0.3942 0.125 Uiso 1 1 calc R . . C5 C -0.0592(8) 0.1538(6) 0.3675(4) 0.098(2) Uani 1 1 d . . . H5A H -0.0423 0.1715 0.3166 0.147 Uiso 1 1 calc R . . H5B H -0.1409 0.1551 0.3831 0.147 Uiso 1 1 calc R . . H5C H -0.0057 0.0892 0.3815 0.147 Uiso 1 1 calc R . . C6 C -0.1736(5) 0.1945(4) 0.5165(3) 0.0630(15) Uani 1 1 d . . . H6 H -0.2315 0.2039 0.4909 0.076 Uiso 1 1 calc R . . C7 C -0.1988(5) 0.1738(4) 0.5887(3) 0.0666(16) Uani 1 1 d . . . H7 H -0.2727 0.1674 0.6124 0.080 Uiso 1 1 calc R . . C8 C -0.1155(5) 0.1623(4) 0.6260(3) 0.0639(15) Uani 1 1 d . . . H8 H -0.1334 0.1490 0.6756 0.077 Uiso 1 1 calc R . . C9 C -0.0060(4) 0.1699(3) 0.5924(3) 0.0508(12) Uani 1 1 d . . . C10 C 0.0822(6) 0.1595(5) 0.6345(3) 0.0695(16) Uani 1 1 d . . . H10 H 0.1331 0.1970 0.6049 0.083 Uiso 1 1 calc R . . C11 C 0.0270(9) 0.2009(9) 0.7024(5) 0.129(4) Uani 1 1 d . . . H11A H 0.0893 0.1924 0.7265 0.193 Uiso 1 1 calc R . . H11B H -0.0260 0.1675 0.7326 0.193 Uiso 1 1 calc R . . H11C H -0.0178 0.2694 0.6916 0.193 Uiso 1 1 calc R . . C12 C 0.1631(11) 0.0574(7) 0.6502(6) 0.154(5) Uani 1 1 d . . . H12A H 0.2178 0.0548 0.6778 0.231 Uiso 1 1 calc R . . H12B H 0.2077 0.0342 0.6063 0.231 Uiso 1 1 calc R . . H12C H 0.1162 0.0170 0.6767 0.231 Uiso 1 1 calc R . . C13 C 0.1954(5) 0.0327(4) 0.4642(3) 0.0626(15) Uani 1 1 d . . . H13A H 0.1269 0.0490 0.4432 0.094 Uiso 1 1 calc R . . H13B H 0.1794 0.0022 0.5130 0.094 Uiso 1 1 calc R . . H13C H 0.2644 -0.0116 0.4384 0.094 Uiso 1 1 calc R . . C14 C 0.2191(4) 0.1217(3) 0.4613(3) 0.0464(11) Uani 1 1 d . . . C15 C 0.3367(4) 0.1179(3) 0.4363(3) 0.0484(12) Uani 1 1 d . . . H15 H 0.3863 0.0655 0.4128 0.058 Uiso 1 1 calc R . . C16 C 0.3915(4) 0.1788(3) 0.4405(2) 0.0436(11) Uani 1 1 d . . . C17 C 0.5261(4) 0.1391(4) 0.4266(3) 0.0639(15) Uani 1 1 d . . . H17A H 0.5571 0.1872 0.3944 0.096 Uiso 1 1 calc R . . H17B H 0.5542 0.0810 0.4058 0.096 Uiso 1 1 calc R . . H17C H 0.5532 0.1235 0.4707 0.096 Uiso 1 1 calc R . . C18 C 0.4043(4) 0.3105(3) 0.4730(3) 0.0477(11) Uani 1 1 d . . . C19 C 0.4284(5) 0.2919(4) 0.5396(3) 0.0559(13) Uani 1 1 d . . . C20 C 0.3678(6) 0.2337(5) 0.6002(3) 0.0714(17) Uani 1 1 d . . . H20 H 0.3256 0.2050 0.5812 0.086 Uiso 1 1 calc R . . C21 C 0.2780(7) 0.2998(8) 0.6504(4) 0.120(3) Uani 1 1 d . . . H21A H 0.2397 0.2623 0.6894 0.179 Uiso 1 1 calc R . . H21B H 0.2186 0.3496 0.6256 0.179 Uiso 1 1 calc R . . H21C H 0.3183 0.3297 0.6683 0.179 Uiso 1 1 calc R . . C22 C 0.4561(8) 0.1531(6) 0.6410(4) 0.106(3) Uani 1 1 d . . . H22A H 0.5148 0.1105 0.6093 0.158 Uiso 1 1 calc R . . H22B H 0.4142 0.1163 0.6784 0.158 Uiso 1 1 calc R . . H22C H 0.4956 0.1808 0.6614 0.158 Uiso 1 1 calc R . . C23 C 0.5041(6) 0.3289(5) 0.5511(4) 0.0745(18) Uani 1 1 d . . . H23 H 0.5202 0.3165 0.5966 0.089 Uiso 1 1 calc R . . C24 C 0.5572(6) 0.3836(5) 0.4976(5) 0.082(2) Uani 1 1 d . . . H24 H 0.6140 0.4045 0.5055 0.099 Uiso 1 1 calc R . . C25 C 0.5282(6) 0.4079(5) 0.4331(4) 0.0783(19) Uani 1 1 d . . . H25 H 0.5617 0.4487 0.3972 0.094 Uiso 1 1 calc R . . C26 C 0.4498(5) 0.3733(4) 0.4199(3) 0.0625(14) Uani 1 1 d . . . C27 C 0.4119(7) 0.4080(5) 0.3501(3) 0.081(2) Uani 1 1 d . . . H27 H 0.3438 0.3872 0.3543 0.097 Uiso 1 1 calc R . . C28 C 0.5066(8) 0.3643(6) 0.2911(4) 0.1043(19) Uani 1 1 d . . . H28A H 0.4771 0.3893 0.2473 0.156 Uiso 1 1 calc R . . H28B H 0.5273 0.2944 0.3013 0.156 Uiso 1 1 calc R . . H28C H 0.5766 0.3807 0.2865 0.156 Uiso 1 1 calc R . . C29 C 0.3684(9) 0.5172(6) 0.3311(4) 0.1043(19) Uani 1 1 d . . . H29A H 0.3438 0.5363 0.2859 0.156 Uiso 1 1 calc R . . H29B H 0.4321 0.5407 0.3280 0.156 Uiso 1 1 calc R . . H29C H 0.3014 0.5446 0.3671 0.156 Uiso 1 1 calc R . . C30 C 0.1845(7) 0.3480(5) 0.2982(3) 0.0725(17) Uani 1 1 d . . . H30A H 0.1457 0.3039 0.2961 0.087 Uiso 1 1 calc R . . H30B H 0.2685 0.3111 0.2997 0.087 Uiso 1 1 calc R . . C31 C 0.1729(10) 0.4272(7) 0.2365(4) 0.110(3) Uani 1 1 d . . . H31A H 0.2423 0.4481 0.2231 0.133 Uiso 1 1 calc R . . H31B H 0.1655 0.4061 0.1961 0.133 Uiso 1 1 calc R . . C32 C 0.0648(9) 0.5058(6) 0.2596(4) 0.102(3) Uani 1 1 d . . . H32A H -0.0058 0.4989 0.2518 0.123 Uiso 1 1 calc R . . H32B H 0.0697 0.5690 0.2347 0.123 Uiso 1 1 calc R . . C33 C 0.0615(6) 0.4946(4) 0.3358(3) 0.0717(17) Uani 1 1 d . . . H33A H 0.0979 0.5368 0.3440 0.086 Uiso 1 1 calc R . . H33B H -0.0209 0.5115 0.3621 0.086 Uiso 1 1 calc R . . C34 C 0.3133(4) 0.8036(3) 0.9777(3) 0.0457(11) Uani 1 1 d . . . C35 C 0.2524(5) 0.7913(4) 1.0463(3) 0.0535(13) Uani 1 1 d . B . C36 C 0.3190(6) 0.7369(5) 1.1063(3) 0.0677(16) Uani 1 1 d . . . H36 H 0.3977 0.7448 1.0875 0.081 Uiso 1 1 calc R A 1 C37 C 0.2721(9) 0.7873(9) 1.1681(5) 0.132(4) Uani 1 1 d . B . H37A H 0.2762 0.8520 1.1537 0.198 Uiso 1 1 calc R . . H37B H 0.3193 0.7515 1.2040 0.198 Uiso 1 1 calc R . . H37C H 0.1899 0.7913 1.1869 0.198 Uiso 1 1 calc R . . C38 C 0.3494(16) 0.6305(9) 1.1203(7) 0.077(4) Uani 0.55 1 d P B 1 H38A H 0.3789 0.6062 1.0759 0.115 Uiso 0.55 1 calc PR B 1 H38B H 0.2790 0.6144 1.1454 0.115 Uiso 0.55 1 calc PR B 1 H38C H 0.4104 0.6012 1.1488 0.115 Uiso 0.55 1 calc PR B 1 C38A C 0.2654(19) 0.6530(14) 1.1393(10) 0.086(5) Uani 0.45 1 d P B 2 H38D H 0.2878 0.6102 1.1053 0.129 Uiso 0.45 1 calc PR B 2 H38E H 0.1793 0.6807 1.1512 0.129 Uiso 0.45 1 calc PR B 2 H38F H 0.2961 0.6166 1.1816 0.129 Uiso 0.45 1 calc PR B 2 C39 C 0.1300(6) 0.8302(4) 1.0599(4) 0.0706(17) Uani 1 1 d . . . H39 H 0.0877 0.8206 1.1064 0.085 Uiso 1 1 calc R B . C40 C 0.0691(6) 0.8822(5) 1.0070(4) 0.082(2) Uani 1 1 d . B . H40 H -0.0146 0.9070 1.0168 0.098 Uiso 1 1 calc R . . C41 C 0.1303(5) 0.8980(4) 0.9404(4) 0.0719(17) Uani 1 1 d . . . H41 H 0.0880 0.9356 0.9044 0.086 Uiso 1 1 calc R B . C42 C 0.2533(5) 0.8604(4) 0.9239(3) 0.0637(15) Uani 1 1 d . B . C43 C 0.3138(6) 0.8833(6) 0.8501(4) 0.098(3) Uani 1 1 d D . . H43 H 0.3980 0.8462 0.8471 0.118 Uiso 1 1 d R B . C44 C 0.2930(19) 0.9910(9) 0.8342(5) 0.105(5) Uani 0.75 1 d PD B 3 H44A H 0.3315 1.0058 0.7868 0.158 Uiso 0.75 1 d PR B 3 H44B H 0.3284 1.0045 0.8652 0.158 Uiso 0.75 1 d PR B 3 H44C H 0.2109 1.0294 0.8399 0.158 Uiso 0.75 1 d PR B 3 C45 C 0.2694(11) 0.8503(10) 0.8004(5) 0.113(5) Uani 0.75 1 d PD B 3 H45A H 0.3085 0.8657 0.7533 0.169 Uiso 0.75 1 d PR B 3 H45B H 0.1859 0.8825 0.8044 0.169 Uiso 0.75 1 d PR B 3 H45C H 0.2860 0.7823 0.8123 0.169 Uiso 0.75 1 d PR B 3 C44A C 0.318(7) 0.982(2) 0.810(2) 0.105(5) Uani 0.25 1 d PD B 4 H44D H 0.3137 1.0155 0.8458 0.158 Uiso 0.25 1 d PR B 4 H44E H 0.2460 1.0086 0.7935 0.158 Uiso 0.25 1 d PR B 4 H44F H 0.3825 0.9870 0.7725 0.158 Uiso 0.25 1 d PR B 4 C45A C 0.320(4) 0.852(3) 0.7823(13) 0.113(5) Uani 0.25 1 d PD B 4 H45D H 0.3675 0.8826 0.7457 0.169 Uiso 0.25 1 d PR B 4 H45E H 0.2428 0.8720 0.7715 0.169 Uiso 0.25 1 d PR B 4 H45F H 0.3556 0.7841 0.7862 0.169 Uiso 0.25 1 d PR B 4 C46 C 0.4030(5) 0.6325(4) 0.9278(3) 0.0535(12) Uani 1 1 d . . . H46A H 0.3375 0.6851 0.9098 0.080 Uiso 1 1 calc R . . H46B H 0.3721 0.5957 0.9708 0.080 Uiso 1 1 calc R . . H46C H 0.4469 0.5904 0.8929 0.080 Uiso 1 1 calc R . . C47 C 0.4841(4) 0.6730(3) 0.9431(2) 0.0407(10) Uani 1 1 d . . . C48 C 0.6027(4) 0.6137(3) 0.9384(3) 0.0434(11) Uani 1 1 d . . . H48 H 0.6252 0.5613 0.9146 0.052 Uiso 1 1 calc R . . C49 C 0.6917(4) 0.6196(3) 0.9629(2) 0.0422(10) Uani 1 1 d . . . C50 C 0.7991(5) 0.5304(3) 0.9673(3) 0.0576(14) Uani 1 1 d . . . H50A H 0.8679 0.5482 0.9633 0.086 Uiso 1 1 calc R . . H50B H 0.8126 0.4961 0.9292 0.086 Uiso 1 1 calc R . . H50C H 0.7866 0.4889 1.0123 0.086 Uiso 1 1 calc R . . C51 C 0.7775(4) 0.6877(3) 1.0191(3) 0.0449(11) Uani 1 1 d . . . C52 C 0.8802(4) 0.7044(4) 0.9801(3) 0.0508(12) Uani 1 1 d . . . C53 C 0.9025(5) 0.7322(5) 0.9006(3) 0.0683(16) Uani 1 1 d . . . H53 H 0.8339 0.7326 0.8843 0.082 Uiso 1 1 calc R . . C54 C 1.0136(8) 0.6595(7) 0.8651(4) 0.104(3) Uani 1 1 d . . . H54A H 1.0246 0.6800 0.8143 0.156 Uiso 1 1 calc R . . H54B H 1.0049 0.5963 0.8770 0.156 Uiso 1 1 calc R . . H54C H 1.0823 0.6558 0.8813 0.156 Uiso 1 1 calc R . . C55 C 0.9079(7) 0.8331(5) 0.8791(4) 0.086(2) Uani 1 1 d . . . H55A H 0.9220 0.8499 0.8280 0.129 Uiso 1 1 calc R . . H55B H 0.9722 0.8358 0.8963 0.129 Uiso 1 1 calc R . . H55C H 0.8331 0.8786 0.8991 0.129 Uiso 1 1 calc R . . C56 C 0.9651(5) 0.6973(4) 1.0150(3) 0.0621(14) Uani 1 1 d . . . H56 H 1.0354 0.7086 0.9892 0.074 Uiso 1 1 calc R . . C57 C 0.9486(6) 0.6743(4) 1.0864(3) 0.0675(16) Uani 1 1 d . . . H57 H 1.0075 0.6695 1.1096 0.081 Uiso 1 1 calc R . . C58 C 0.8468(6) 0.6582(4) 1.1245(3) 0.0658(15) Uani 1 1 d . . . H58 H 0.8365 0.6424 1.1740 0.079 Uiso 1 1 calc R . . C59 C 0.7588(5) 0.6647(4) 1.0920(3) 0.0538(13) Uani 1 1 d . . . C60 C 0.6472(6) 0.6482(5) 1.1363(3) 0.0734(18) Uani 1 1 d . . . H60 H 0.5942 0.6582 1.1040 0.088 Uiso 1 1 calc R . . C61 C 0.6708(11) 0.5479(8) 1.1759(6) 0.161(5) Uani 1 1 d . . . H61A H 0.7119 0.5023 1.1432 0.241 Uiso 1 1 calc R . . H61B H 0.5960 0.5390 1.2008 0.241 Uiso 1 1 calc R . . H61C H 0.7200 0.5368 1.2096 0.241 Uiso 1 1 calc R . . C62 C 0.5828(8) 0.7196(8) 1.1857(5) 0.123(3) Uani 1 1 d . . . H62A H 0.5114 0.7070 1.2136 0.184 Uiso 1 1 calc R . . H62B H 0.5611 0.7846 1.1589 0.184 Uiso 1 1 calc R . . H62C H 0.6340 0.7135 1.2168 0.184 Uiso 1 1 calc R . . C63 C 0.6048(6) 0.9867(4) 0.8337(3) 0.0701(17) Uani 1 1 d . D . H63A H 0.6410 1.0044 0.8637 0.084 Uiso 1 1 calc R . . H63B H 0.5224 1.0310 0.8355 0.084 Uiso 1 1 calc R . . C64 C 0.6721(8) 0.9930(6) 0.7605(4) 0.097(2) Uani 1 1 d . . . H64A H 0.6430 1.0578 0.7331 0.116 Uiso 1 1 calc R C 5 H64B H 0.7576 0.9741 0.7585 0.116 Uiso 1 1 calc R C 5 C65 C 0.645(3) 0.9237(16) 0.7381(11) 0.106(9) Uani 0.40 1 d P D 5 H65A H 0.7035 0.9008 0.6966 0.127 Uiso 0.40 1 calc PR D 5 H65B H 0.5657 0.9526 0.7257 0.127 Uiso 0.40 1 calc PR D 5 C65A C 0.7215(14) 0.8872(12) 0.7437(6) 0.081(3) Uani 0.60 1 d P D 6 H65C H 0.7120 0.8868 0.6966 0.097 Uiso 0.60 1 calc PR D 6 H65D H 0.8056 0.8553 0.7469 0.097 Uiso 0.60 1 calc PR D 6 C66 C 0.6473(6) 0.8419(5) 0.7984(3) 0.0741(17) Uani 1 1 d . . . H66A H 0.5936 0.8090 0.7978 0.089 Uiso 1 1 calc R D 5 H66B H 0.7279 0.7947 0.7978 0.089 Uiso 1 1 calc R D 5 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 0.0368(4) 0.0266(4) 0.0405(4) -0.0024(3) -0.0072(3) -0.0026(3) Cr2 0.0429(4) 0.0240(4) 0.0445(4) -0.0028(3) -0.0092(3) -0.0117(3) O1 0.081(3) 0.051(2) 0.0423(19) -0.0034(16) -0.0158(18) -0.0095(19) O2 0.084(3) 0.045(2) 0.048(2) -0.0037(16) -0.0010(18) -0.0212(19) N1 0.039(2) 0.0295(18) 0.047(2) -0.0003(16) -0.0077(16) -0.0052(15) N2 0.039(2) 0.0311(19) 0.048(2) -0.0033(16) -0.0062(16) -0.0066(15) N3 0.040(2) 0.031(2) 0.077(3) -0.0119(19) -0.014(2) -0.0017(18) N4 0.0331(19) 0.033(2) 0.043(2) -0.0052(15) -0.0073(15) -0.0090(17) N5 0.044(2) 0.035(2) 0.076(3) -0.010(2) -0.005(2) -0.0054(19) N6 0.044(2) 0.0319(19) 0.044(2) -0.0045(15) -0.0095(16) -0.0149(16) N7 0.042(2) 0.0273(17) 0.046(2) -0.0017(15) -0.0119(16) -0.0118(15) N8 0.061(3) 0.029(2) 0.086(3) -0.011(2) -0.032(2) -0.0091(18) N9 0.0346(19) 0.032(2) 0.052(2) -0.0085(16) -0.0134(16) -0.0085(15) N10 0.053(3) 0.034(2) 0.086(3) -0.017(2) -0.014(2) -0.0140(18) C1 0.049(3) 0.028(2) 0.050(3) -0.0013(19) -0.002(2) -0.0135(19) C2 0.051(3) 0.042(3) 0.062(3) 0.000(2) -0.011(2) -0.019(2) C3 0.062(3) 0.078(4) 0.058(3) -0.004(3) -0.016(3) -0.025(3) C4 0.086(5) 0.084(5) 0.075(4) 0.014(4) -0.029(4) -0.031(4) C5 0.123(7) 0.110(6) 0.080(5) -0.023(4) -0.022(5) -0.055(5) C6 0.047(3) 0.058(3) 0.082(4) -0.009(3) -0.013(3) -0.018(2) C7 0.052(3) 0.061(3) 0.075(4) 0.002(3) 0.000(3) -0.024(3) C8 0.067(4) 0.050(3) 0.059(3) 0.001(3) 0.000(3) -0.018(3) C9 0.048(3) 0.037(2) 0.055(3) 0.000(2) -0.006(2) -0.009(2) C10 0.074(4) 0.078(4) 0.046(3) 0.004(3) -0.011(3) -0.024(3) C11 0.120(8) 0.178(10) 0.099(6) -0.066(7) 0.002(6) -0.052(7) C12 0.179(11) 0.117(8) 0.158(9) -0.024(7) -0.125(9) 0.022(7) C13 0.068(4) 0.035(3) 0.076(4) -0.011(2) -0.005(3) -0.014(2) C14 0.052(3) 0.031(2) 0.048(3) -0.0046(19) -0.011(2) -0.007(2) C15 0.046(3) 0.030(2) 0.056(3) -0.010(2) -0.001(2) -0.0024(19) C16 0.038(2) 0.035(2) 0.046(3) -0.0069(19) -0.0035(19) -0.0025(19) C17 0.039(3) 0.051(3) 0.085(4) -0.014(3) -0.003(3) -0.002(2) C18 0.035(2) 0.039(2) 0.059(3) -0.011(2) -0.006(2) -0.0030(19) C19 0.053(3) 0.047(3) 0.063(3) -0.009(2) -0.019(3) -0.006(2) C20 0.066(4) 0.084(4) 0.057(3) -0.002(3) -0.020(3) -0.019(3) C21 0.078(5) 0.158(9) 0.084(5) -0.012(5) -0.010(4) -0.007(5) C22 0.096(6) 0.090(6) 0.099(6) 0.017(4) -0.031(5) -0.011(4) C23 0.067(4) 0.063(4) 0.095(5) -0.016(3) -0.040(4) -0.005(3) C24 0.070(4) 0.060(4) 0.125(7) -0.018(4) -0.037(4) -0.017(3) C25 0.064(4) 0.064(4) 0.108(6) -0.012(4) -0.008(4) -0.030(3) C26 0.052(3) 0.056(3) 0.075(4) -0.011(3) -0.003(3) -0.021(3) C27 0.099(5) 0.084(5) 0.063(4) -0.003(3) 0.003(4) -0.054(4) C28 0.127(5) 0.087(4) 0.080(4) 0.003(3) -0.001(3) -0.040(4) C29 0.127(5) 0.087(4) 0.080(4) 0.003(3) -0.001(3) -0.040(4) C30 0.092(5) 0.074(4) 0.049(3) -0.020(3) -0.002(3) -0.028(3) C31 0.153(9) 0.126(7) 0.047(4) -0.012(4) -0.007(4) -0.051(7) C32 0.143(8) 0.099(6) 0.059(4) 0.016(4) -0.039(5) -0.040(6) C33 0.087(4) 0.055(3) 0.056(3) 0.011(3) -0.025(3) -0.013(3) C34 0.041(2) 0.031(2) 0.064(3) -0.005(2) -0.010(2) -0.0137(19) C35 0.055(3) 0.045(3) 0.060(3) -0.016(2) 0.006(2) -0.023(2) C36 0.065(4) 0.078(4) 0.054(3) -0.011(3) 0.003(3) -0.028(3) C37 0.118(7) 0.191(11) 0.104(7) -0.084(7) -0.011(6) -0.040(7) C38 0.110(11) 0.048(6) 0.064(8) -0.003(5) -0.014(8) -0.026(7) C38A 0.106(14) 0.083(12) 0.073(11) 0.008(9) -0.036(11) -0.038(11) C39 0.059(4) 0.057(3) 0.089(5) -0.022(3) 0.012(3) -0.025(3) C40 0.055(4) 0.065(4) 0.121(6) -0.025(4) -0.003(4) -0.019(3) C41 0.053(3) 0.056(3) 0.102(5) -0.004(3) -0.028(3) -0.010(3) C42 0.051(3) 0.057(3) 0.076(4) 0.004(3) -0.019(3) -0.016(3) C43 0.062(4) 0.118(6) 0.071(5) 0.034(4) -0.027(3) -0.005(4) C44 0.123(12) 0.160(9) 0.056(9) 0.037(6) -0.038(9) -0.094(8) C45 0.124(12) 0.092(6) 0.050(6) 0.007(6) 0.011(6) 0.008(8) C44A 0.123(12) 0.160(9) 0.056(9) 0.037(6) -0.038(9) -0.094(8) C45A 0.124(12) 0.092(6) 0.050(6) 0.007(6) 0.011(6) 0.008(8) C46 0.060(3) 0.041(3) 0.068(3) -0.010(2) -0.021(3) -0.020(2) C47 0.054(3) 0.032(2) 0.038(2) -0.0004(18) -0.011(2) -0.019(2) C48 0.052(3) 0.026(2) 0.052(3) -0.0088(19) -0.012(2) -0.0117(19) C49 0.049(3) 0.028(2) 0.045(2) -0.0021(18) -0.009(2) -0.0094(19) C50 0.058(3) 0.035(3) 0.073(4) -0.011(2) -0.019(3) -0.004(2) C51 0.046(3) 0.029(2) 0.058(3) -0.004(2) -0.018(2) -0.0079(19) C52 0.049(3) 0.046(3) 0.057(3) -0.002(2) -0.020(2) -0.014(2) C53 0.053(3) 0.096(5) 0.059(3) 0.001(3) -0.012(3) -0.036(3) C54 0.104(6) 0.122(7) 0.076(5) -0.026(5) 0.012(4) -0.044(5) C55 0.082(5) 0.094(5) 0.077(4) 0.024(4) -0.024(4) -0.044(4) C56 0.052(3) 0.058(3) 0.076(4) -0.001(3) -0.026(3) -0.015(3) C57 0.068(4) 0.061(4) 0.079(4) 0.002(3) -0.041(3) -0.020(3) C58 0.078(4) 0.062(3) 0.056(3) 0.005(3) -0.033(3) -0.018(3) C59 0.060(3) 0.044(3) 0.051(3) 0.000(2) -0.019(2) -0.011(2) C60 0.075(4) 0.088(5) 0.050(3) 0.010(3) -0.015(3) -0.031(4) C61 0.158(10) 0.111(8) 0.166(10) 0.009(7) 0.054(8) -0.074(7) C62 0.085(6) 0.152(9) 0.114(7) -0.055(7) 0.004(5) -0.017(6) C63 0.087(4) 0.049(3) 0.067(4) 0.010(3) -0.013(3) -0.030(3) C64 0.114(6) 0.085(5) 0.069(5) 0.020(4) -0.013(4) -0.033(5) C65 0.13(2) 0.079(14) 0.057(11) 0.003(9) -0.017(13) 0.010(14) C65A 0.096(9) 0.110(11) 0.044(6) -0.016(7) 0.003(6) -0.053(8) C66 0.081(4) 0.077(4) 0.053(3) -0.019(3) -0.002(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.058(4) . ? Cr1 N2 2.065(4) . ? Cr1 N5 2.097(4) 2_566 ? Cr1 N3 2.095(4) . ? Cr2 N6 2.057(4) . ? Cr2 N7 2.063(4) . ? Cr2 N10 2.091(4) 2_677 ? Cr2 N8 2.093(4) . ? O1 C30 1.436(7) . ? O1 C33 1.447(7) . ? O2 C63 1.425(6) . ? O2 C66 1.432(7) . ? N1 C14 1.339(6) . ? N1 C1 1.456(6) . ? N2 C16 1.328(6) . ? N2 C18 1.441(6) . ? N3 N4 1.165(5) . ? N4 N5 1.165(5) . ? N5 Cr1 2.097(4) 2_566 ? N6 C47 1.330(6) . ? N6 C34 1.462(6) . ? N7 C49 1.332(6) . ? N7 C51 1.457(6) . ? N8 N9 1.151(5) . ? N9 N10 1.167(5) . ? N10 Cr2 2.091(4) 2_677 ? C1 C9 1.401(7) . ? C1 C2 1.395(7) . ? C2 C6 1.408(7) . ? C2 C3 1.509(8) . ? C3 C5 1.546(10) . ? C3 C4 1.545(9) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.383(8) . ? C6 H6 0.9500 . ? C7 C8 1.384(9) . ? C7 H7 0.9500 . ? C8 C9 1.392(8) . ? C8 H8 0.9500 . ? C9 C10 1.510(8) . ? C10 C12 1.509(11) . ? C10 C11 1.531(10) . ? 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 C14 1.492(7) . ? C13 H13A 0.9809 . ? C13 H13B 0.9810 . ? C13 H13C 0.9810 . ? C14 C15 1.407(7) . ? C15 C16 1.388(7) . ? C15 H15 0.9500 . ? C16 C17 1.528(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.394(8) . ? C18 C26 1.404(7) . ? C19 C23 1.372(9) . ? C19 C20 1.529(8) . ? C20 C21 1.527(11) . ? C20 C22 1.535(9) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.377(10) . ? C23 H23 0.9500 . ? C24 C25 1.367(10) . ? C24 H24 0.9500 . ? C25 C26 1.395(9) . ? C25 H25 0.9500 . ? C26 C27 1.510(9) . ? C27 C28 1.515(10) . ? C27 C29 1.527(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 C31 1.497(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.478(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.493(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.391(7) . ? C34 C42 1.402(8) . ? C35 C39 1.391(8) . ? C35 C36 1.536(9) . ? C36 C38 1.494(13) . ? C36 C37 1.494(10) . ? C36 C38A 1.596(19) . ? 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 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39 C40 1.378(10) . ? C39 H39 0.9500 . ? C40 C41 1.368(10) . ? C40 H40 0.9500 . ? C41 C42 1.398(8) . ? C41 H41 0.9500 . ? C42 C43 1.497(9) . ? C43 C44 1.533(13) . ? C43 C44A 1.533(13) . ? C43 C45A 1.533(14) . ? C43 C45 1.534(14) . ? C43 H43 0.9800 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C44 H44D 0.6445 . ? C44 H44E 1.0594 . ? C44 H44F 1.4260 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C45 H45D 1.5606 . ? C45 H45E 0.6954 . ? C45 H45F 1.1888 . ? C44A H44A 0.5544 . ? C44A H44B 1.2908 . ? C44A H44C 1.3153 . ? C44A H44D 0.9600 . ? C44A H44E 0.9600 . ? C44A H44F 0.9600 . ? C45A H45A 0.6040 . ? C45A H45B 1.5239 . ? C45A H45C 1.2585 . ? C45A H45D 0.9600 . ? C45A H45E 0.9600 . ? C45A H45F 0.9600 . ? C46 C47 1.510(7) . ? C46 H46A 0.9805 . ? C46 H46B 0.9805 . ? C46 H46C 0.9805 . ? C47 C48 1.403(7) . ? C48 C49 1.381(7) . ? C48 H48 0.9500 . ? C49 C50 1.508(7) . ? C50 H50A 0.9809 . ? C50 H50B 0.9809 . ? C50 H50C 0.9809 . ? C51 C52 1.395(7) . ? C51 C59 1.398(7) . ? C52 C56 1.388(7) . ? C52 C53 1.528(8) . ? C53 C55 1.522(9) . ? C53 C54 1.536(10) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.369(8) . ? C56 H56 0.9500 . ? C57 C58 1.377(9) . ? C57 H57 0.9500 . ? C58 C59 1.393(8) . ? C58 H58 0.9500 . ? C59 C60 1.517(8) . ? C60 C61 1.500(11) . ? C60 C62 1.509(11) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.487(9) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.44(3) . ? C64 C65A 1.588(17) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.51(2) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C65A C66 1.456(13) . ? C65A H65C 0.9900 . ? C65A H65D 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 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 N1 Cr1 N2 91.07(15) . . ? N1 Cr1 N5 90.26(16) . 2_566 ? N2 Cr1 N5 171.16(18) . 2_566 ? N1 Cr1 N3 171.94(17) . . ? N2 Cr1 N3 90.14(15) . . ? N5 Cr1 N3 87.35(16) 2_566 . ? N6 Cr2 N7 91.38(15) . . ? N6 Cr2 N10 89.51(16) . 2_677 ? N7 Cr2 N10 171.44(17) . 2_677 ? N6 Cr2 N8 171.48(18) . . ? N7 Cr2 N8 90.52(16) . . ? N10 Cr2 N8 87.40(17) 2_677 . ? C30 O1 C33 109.7(4) . . ? C63 O2 C66 108.9(4) . . ? C14 N1 C1 117.7(4) . . ? C14 N1 Cr1 124.2(3) . . ? C1 N1 Cr1 118.1(3) . . ? C16 N2 C18 116.1(4) . . ? C16 N2 Cr1 124.1(3) . . ? C18 N2 Cr1 119.7(3) . . ? N4 N3 Cr1 129.8(3) . . ? N3 N4 N5 176.4(5) . . ? N4 N5 Cr1 136.0(4) . 2_566 ? C47 N6 C34 116.9(4) . . ? C47 N6 Cr2 123.4(3) . . ? C34 N6 Cr2 119.6(3) . . ? C49 N7 C51 117.4(4) . . ? C49 N7 Cr2 123.6(3) . . ? C51 N7 Cr2 118.9(3) . . ? N9 N8 Cr2 131.6(4) . . ? N8 N9 N10 176.9(5) . . ? N9 N10 Cr2 135.3(4) . 2_677 ? C9 C1 C2 121.4(4) . . ? C9 C1 N1 118.5(4) . . ? C2 C1 N1 120.0(4) . . ? C6 C2 C1 118.0(5) . . ? C6 C2 C3 118.9(5) . . ? C1 C2 C3 123.2(5) . . ? C2 C3 C5 112.7(5) . . ? C2 C3 C4 110.7(5) . . ? C5 C3 C4 110.2(6) . . ? C2 C3 H3 107.6 . . ? C5 C3 H3 107.7 . . ? C4 C3 H3 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.4 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.3(6) . . ? C7 C6 H6 119.3 . . ? C2 C6 H6 119.4 . . ? C8 C7 C6 119.4(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 121.4(5) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C1 118.5(5) . . ? C8 C9 C10 120.3(5) . . ? C1 C9 C10 121.2(5) . . ? C9 C10 C12 112.9(6) . . ? C9 C10 C11 114.1(6) . . ? C12 C10 C11 109.5(7) . . ? C9 C10 H10 106.6 . . ? C12 C10 H10 106.7 . . ? C11 C10 H10 106.6 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.4 . . ? C10 C12 H12B 109.4 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.6 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 109.4 . . ? C14 C13 H13C 109.6 . . ? H13A C13 H13C 109.4 . . ? H13B C13 H13C 109.4 . . ? N1 C14 C15 123.0(4) . . ? N1 C14 C13 120.8(5) . . ? C15 C14 C13 116.1(4) . . ? C16 C15 C14 130.0(4) . . ? C16 C15 H15 115.0 . . ? C14 C15 H15 115.0 . . ? N2 C16 C15 123.7(4) . . ? N2 C16 C17 120.3(5) . . ? C15 C16 C17 115.8(4) . . ? C16 C17 H17A 109.4 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C26 119.5(5) . . ? C19 C18 N2 119.2(4) . . ? C26 C18 N2 121.2(5) . . ? C23 C19 C18 119.6(6) . . ? C23 C19 C20 120.1(6) . . ? C18 C19 C20 120.3(5) . . ? C19 C20 C21 109.5(6) . . ? C19 C20 C22 112.0(6) . . ? C21 C20 C22 108.6(6) . . ? C19 C20 H20 108.9 . . ? C21 C20 H20 109.0 . . ? C22 C20 H20 108.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 C24 121.0(7) . . ? C19 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 120.1(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.5(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C18 118.9(6) . . ? C25 C26 C27 119.0(6) . . ? C18 C26 C27 121.9(5) . . ? C26 C27 C28 113.1(7) . . ? C26 C27 C29 112.5(6) . . ? C28 C27 C29 110.0(6) . . ? C26 C27 H27 106.9 . . ? C28 C27 H27 106.9 . . ? C29 C27 H27 107.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.4 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.4 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 C31 105.0(6) . . ? O1 C30 H30A 110.7 . . ? C31 C30 H30A 110.7 . . ? O1 C30 H30B 110.7 . . ? C31 C30 H30B 110.8 . . ? H30A C30 H30B 108.8 . . ? C32 C31 C30 105.3(6) . . ? C32 C31 H31A 110.6 . . ? C30 C31 H31A 110.7 . . ? C32 C31 H31B 110.7 . . ? C30 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? C31 C32 C33 103.4(6) . . ? C31 C32 H32A 111.0 . . ? C33 C32 H32A 111.1 . . ? C31 C32 H32B 111.1 . . ? C33 C32 H32B 111.1 . . ? H32A C32 H32B 109.0 . . ? O1 C33 C32 106.5(6) . . ? O1 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? O1 C33 H33B 110.5 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C35 C34 C42 120.7(5) . . ? C35 C34 N6 118.7(4) . . ? C42 C34 N6 120.6(5) . . ? C39 C35 C34 118.9(6) . . ? C39 C35 C36 120.4(5) . . ? C34 C35 C36 120.7(5) . . ? C38 C36 C37 117.3(8) . . ? C38 C36 C35 115.9(8) . . ? C37 C36 C35 112.4(6) . . ? C38 C36 C38A 36.5(8) . . ? C37 C36 C38A 97.0(10) . . ? C35 C36 C38A 102.1(8) . . ? C38 C36 H36 102.9 . . ? C37 C36 H36 102.8 . . ? C35 C36 H36 102.8 . . ? C38A C36 H36 139.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.4 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.4 . . ? 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 . . ? C36 C38A H38D 109.5 . . ? C36 C38A H38E 109.4 . . ? H38D C38A H38E 109.5 . . ? C36 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C35 C39 C40 121.1(6) . . ? C35 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C41 C40 C39 119.4(6) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C40 C41 C42 121.7(6) . . ? C40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C41 C42 C34 118.0(6) . . ? C41 C42 C43 118.5(6) . . ? C34 C42 C43 123.5(5) . . ? C42 C43 C44 107.8(8) . . ? C42 C43 C44A 127(2) . . ? C44 C43 C44A 19(2) . . ? C42 C43 C45A 132.1(18) . . ? C44 C43 C45A 107.6(19) . . ? C44A C43 C45A 91(3) . . ? C42 C43 C45 110.0(7) . . ? C44 C43 C45 113.4(9) . . ? C44A C43 C45 102(2) . . ? C45A C43 C45 24.3(16) . . ? C42 C43 H43 107.4 . . ? C44 C43 H43 110.7 . . ? C44A C43 H43 100.9 . . ? C45A C43 H43 88.9 . . ? C45 C43 H43 107.5 . . ? C43 C44 H44A 107.7 . . ? C43 C44 H44B 107.9 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 112.8 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C44 H44D 129.9 . . ? H44A C44 H44D 93.3 . . ? H44B C44 H44D 23.1 . . ? H44C C44 H44D 101.3 . . ? C43 C44 H44E 97.1 . . ? H44A C44 H44E 61.0 . . ? H44B C44 H44E 155.0 . . ? H44C C44 H44E 58.8 . . ? H44D C44 H44E 132.3 . . ? C43 C44 H44F 95.3 . . ? H44A C44 H44F 19.5 . . ? H44B C44 H44F 100.4 . . ? H44C C44 H44F 128.8 . . ? H44D C44 H44F 90.3 . . ? H44E C44 H44F 76.6 . . ? C43 C45 H45A 109.2 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.7 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C45 H45D 81.9 . . ? H45A C45 H45D 27.9 . . ? H45B C45 H45D 126.2 . . ? H45C C45 H45D 115.4 . . ? C43 C45 H45E 135.9 . . ? H45A C45 H45E 53.7 . . ? H45B C45 H45E 57.3 . . ? H45C C45 H45E 114.4 . . ? H45D C45 H45E 77.7 . . ? C43 C45 H45F 97.8 . . ? H45A C45 H45F 70.6 . . ? H45B C45 H45F 150.2 . . ? H45C C45 H45F 47.8 . . ? H45D C45 H45F 68.0 . . ? H45E C45 H45F 109.8 . . ? C43 C44A H44A 152.6 . . ? C43 C44A H44B 92.3 . . ? H44A C44A H44B 109.8 . . ? C43 C44A H44C 94.7 . . ? H44A C44A H44C 106.7 . . ? H44B C44A H44C 74.0 . . ? C43 C44A H44D 105.0 . . ? H44A C44A H44D 99.7 . . ? H44B C44A H44D 15.4 . . ? H44C C44A H44D 64.9 . . ? C43 C44A H44E 101.8 . . ? H44A C44A H44E 80.8 . . ? H44B C44A H44E 121.6 . . ? H44C C44A H44E 48.9 . . ? H44D C44A H44E 109.5 . . ? C43 C44A H44F 121.0 . . ? H44A C44A H44F 36.5 . . ? H44B C44A H44F 110.3 . . ? H44C C44A H44F 143.1 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C43 C45A H45A 145.8 . . ? C43 C45A H45B 85.0 . . ? H45A C45A H45B 82.8 . . ? C43 C45A H45C 95.0 . . ? H45A C45A H45C 109.6 . . ? H45B C45A H45C 67.8 . . ? C43 C45A H45D 106.7 . . ? H45A C45A H45D 60.1 . . ? H45B C45A H45D 130.1 . . ? H45C C45A H45D 152.2 . . ? C43 C45A H45E 111.9 . . ? H45A C45A H45E 54.6 . . ? H45B C45A H45E 28.9 . . ? H45C C45A H45E 76.9 . . ? H45D C45A H45E 109.5 . . ? C43 C45A H45F 109.7 . . ? H45A C45A H45F 104.5 . . ? H45B C45A H45F 111.5 . . ? H45C C45A H45F 45.2 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.4 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.4 . . ? H46B C46 H46C 109.4 . . ? N6 C47 C48 123.6(4) . . ? N6 C47 C46 120.3(4) . . ? C48 C47 C46 116.1(4) . . ? C49 C48 C47 130.0(4) . . ? C49 C48 H48 115.0 . . ? C47 C48 H48 115.0 . . ? N7 C49 C48 123.7(4) . . ? N7 C49 C50 120.0(4) . . ? C48 C49 C50 116.2(4) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.6 . . ? H50A C50 H50B 109.4 . . ? C49 C50 H50C 109.6 . . ? H50A C50 H50C 109.4 . . ? H50B C50 H50C 109.4 . . ? C52 C51 C59 121.4(5) . . ? C52 C51 N7 120.6(4) . . ? C59 C51 N7 118.0(4) . . ? C56 C52 C51 118.7(5) . . ? C56 C52 C53 118.3(5) . . ? C51 C52 C53 123.0(5) . . ? C55 C53 C52 110.5(5) . . ? C55 C53 C54 111.4(6) . . ? C52 C53 C54 112.2(6) . . ? C55 C53 H53 107.5 . . ? C52 C53 H53 107.5 . . ? C54 C53 H53 107.5 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.4 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C52 120.7(6) . . ? C57 C56 H56 119.7 . . ? C52 C56 H56 119.7 . . ? C58 C57 C56 120.3(5) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C58 C59 121.3(5) . . ? C57 C58 H58 119.4 . . ? C59 C58 H58 119.3 . . ? C58 C59 C51 117.7(5) . . ? C58 C59 C60 119.4(5) . . ? C51 C59 C60 122.9(5) . . ? C61 C60 C59 112.3(6) . . ? C61 C60 C62 110.3(7) . . ? C59 C60 C62 111.4(6) . . ? C61 C60 H60 107.5 . . ? C59 C60 H60 107.6 . . ? C62 C60 H60 107.5 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.4 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O2 C63 C64 107.6(6) . . ? O2 C63 H63A 110.2 . . ? C64 C63 H63A 110.2 . . ? O2 C63 H63B 110.2 . . ? C64 C63 H63B 110.2 . . ? H63A C63 H63B 108.5 . . ? C65 C64 C63 99.0(11) . . ? C65 C64 C65A 35.4(10) . . ? C63 C64 C65A 105.5(6) . . ? C65 C64 H64A 111.9 . . ? C63 C64 H64A 112.0 . . ? C65A C64 H64A 134.5 . . ? C65 C64 H64B 112.1 . . ? C63 C64 H64B 111.9 . . ? C65A C64 H64B 77.6 . . ? H64A C64 H64B 109.7 . . ? C64 C65 C66 106.8(16) . . ? C64 C65 H65A 110.3 . . ? C66 C65 H65A 110.3 . . ? C64 C65 H65B 110.4 . . ? C66 C65 H65B 110.5 . . ? H65A C65 H65B 108.6 . . ? C66 C65A C64 101.8(9) . . ? C66 C65A H65C 111.3 . . ? C64 C65A H65C 111.4 . . ? C66 C65A H65D 111.5 . . ? C64 C65A H65D 111.5 . . ? H65C C65A H65D 109.3 . . ? O2 C66 C65A 108.9(7) . . ? O2 C66 C65 101.9(10) . . ? C65A C66 C65 36.5(11) . . ? O2 C66 H66A 111.4 . . ? C65A C66 H66A 133.4 . . ? C65 C66 H66A 111.3 . . ? O2 C66 H66B 111.4 . . ? C65A C66 H66B 75.8 . . ? C65 C66 H66B 111.5 . . ? H66A C66 H66B 109.3 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.587 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.137 # Attachment 'cpd_11_CCDC_764153.cif' data_7408 _database_code_depnum_ccdc_archive 'CCDC 764152' #TrackingRef 'cpd_11_CCDC_764153.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H59 N4 Si2 V' _chemical_formula_sum 'C35 H59 N4 Si2 V' _chemical_formula_weight 642.98 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2715(3) _cell_length_b 19.3946(5) _cell_length_c 16.4428(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.0740(10) _cell_angle_gamma 90.00 _cell_volume 3853.07(18) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 32833 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour green(dark) _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8545 _exptl_absorpt_correction_T_max 0.9822 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33957 _diffrn_reflns_av_R_equivalents 0.1146 _diffrn_reflns_av_sigmaI/netI 0.1048 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7027 _reflns_number_gt 4369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1051P)^2^+0.2007P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.029(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7027 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1358 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2081 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.004 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 V1 V 0.54228(5) 0.19927(4) 0.28506(4) 0.0314(3) Uani 1 1 d . . . Si1 Si 0.33026(10) 0.09439(7) 0.22147(8) 0.0459(4) Uani 1 1 d . . . Si2 Si 0.46010(10) 0.35494(7) 0.33905(8) 0.0420(4) Uani 1 1 d . . . N1 N 0.4089(3) 0.16904(18) 0.2076(2) 0.0353(8) Uani 1 1 d . . . N2 N 0.6252(3) 0.21909(17) 0.1948(2) 0.0324(8) Uani 1 1 d . . . N3 N 0.6032(3) 0.13924(17) 0.35368(19) 0.0322(8) Uani 1 1 d . . . N4 N 0.5153(3) 0.27468(19) 0.3279(2) 0.0417(9) Uani 1 1 d . . . C1 C 0.4257(4) 0.0252(3) 0.2668(3) 0.0611(15) Uani 1 1 d . . . H1A H 0.4760 0.0146 0.2299 0.092 Uiso 1 1 calc R . . H1B H 0.3838 -0.0153 0.2750 0.092 Uiso 1 1 calc R . . H1C H 0.4666 0.0403 0.3188 0.092 Uiso 1 1 calc R . . C2 C 0.2326(4) 0.1151(3) 0.2924(3) 0.0735(18) Uani 1 1 d . . . H2A H 0.1832 0.1510 0.2687 0.110 Uiso 1 1 calc R . . H2B H 0.2734 0.1303 0.3445 0.110 Uiso 1 1 calc R . . H2C H 0.1907 0.0747 0.3006 0.110 Uiso 1 1 calc R . . C3 C 0.2543(5) 0.0605(3) 0.1220(3) 0.0730(17) Uani 1 1 d . . . H3A H 0.2037 0.0949 0.0959 0.110 Uiso 1 1 calc R . . H3B H 0.2138 0.0200 0.1321 0.110 Uiso 1 1 calc R . . H3C H 0.3060 0.0491 0.0865 0.110 Uiso 1 1 calc R . . C4 C 0.2587(4) 0.2274(3) 0.1100(3) 0.0513(13) Uani 1 1 d . . . H4A H 0.2113 0.2111 0.1465 0.077 Uiso 1 1 calc R . . H4B H 0.2447 0.2016 0.0594 0.077 Uiso 1 1 calc R . . H4C H 0.2443 0.2753 0.0983 0.077 Uiso 1 1 calc R . . C5 C 0.3786(3) 0.2182(2) 0.1506(3) 0.0386(11) Uani 1 1 d . . . C6 C 0.4531(3) 0.2633(2) 0.1228(3) 0.0390(11) Uani 1 1 d . . . H6 H 0.4219 0.3010 0.0924 0.047 Uiso 1 1 calc R . . C7 C 0.5698(4) 0.2587(2) 0.1351(2) 0.0368(10) Uani 1 1 d . . . C8 C 0.6300(4) 0.2994(3) 0.0789(3) 0.0524(13) Uani 1 1 d . . . H8A H 0.6939 0.2741 0.0695 0.079 Uiso 1 1 calc R . . H8B H 0.6528 0.3429 0.1041 0.079 Uiso 1 1 calc R . . H8C H 0.5817 0.3071 0.0271 0.079 Uiso 1 1 calc R . . C9 C 0.7362(3) 0.1970(2) 0.1892(2) 0.0347(10) Uani 1 1 d . . . C10 C 0.7471(3) 0.1393(2) 0.1394(3) 0.0408(11) Uani 1 1 d . . . C11 C 0.6481(4) 0.1027(3) 0.0888(3) 0.0546(14) Uani 1 1 d . . . H11 H 0.5811 0.1210 0.1057 0.066 Uiso 1 1 calc R . . C12 C 0.6503(6) 0.0258(3) 0.1033(4) 0.086(2) Uani 1 1 d . . . H12A H 0.5858 0.0053 0.0710 0.129 Uiso 1 1 calc R . . H12B H 0.6510 0.0168 0.1608 0.129 Uiso 1 1 calc R . . H12C H 0.7155 0.0066 0.0873 0.129 Uiso 1 1 calc R . . C13 C 0.6405(6) 0.1173(4) -0.0034(4) 0.092(2) Uani 1 1 d . . . H13A H 0.5769 0.0943 -0.0338 0.138 Uiso 1 1 calc R . . H13B H 0.7061 0.1007 -0.0214 0.138 Uiso 1 1 calc R . . H13C H 0.6337 0.1661 -0.0130 0.138 Uiso 1 1 calc R . . C14 C 0.8533(4) 0.1164(3) 0.1368(3) 0.0504(13) Uani 1 1 d . . . H14 H 0.8632 0.0788 0.1037 0.061 Uiso 1 1 calc R . . C15 C 0.9441(4) 0.1478(3) 0.1819(3) 0.0538(13) Uani 1 1 d . . . H15 H 1.0145 0.1309 0.1798 0.065 Uiso 1 1 calc R . . C16 C 0.9322(4) 0.2041(3) 0.2303(3) 0.0481(12) Uani 1 1 d . . . H16 H 0.9948 0.2249 0.2603 0.058 Uiso 1 1 calc R . . C17 C 0.8275(3) 0.2307(2) 0.2352(3) 0.0375(10) Uani 1 1 d . . . C18 C 0.8151(4) 0.2929(3) 0.2881(3) 0.0482(12) Uani 1 1 d . . . H18 H 0.7376 0.3076 0.2757 0.058 Uiso 1 1 calc R . . C19 C 0.8864(5) 0.3530(3) 0.2683(4) 0.0734(17) Uani 1 1 d . . . H19A H 0.8760 0.3918 0.3024 0.110 Uiso 1 1 calc R . . H19B H 0.8652 0.3655 0.2112 0.110 Uiso 1 1 calc R . . H19C H 0.9629 0.3396 0.2788 0.110 Uiso 1 1 calc R . . C20 C 0.8423(5) 0.2765(3) 0.3800(3) 0.0722(17) Uani 1 1 d . . . H20A H 0.8327 0.3171 0.4112 0.108 Uiso 1 1 calc R . . H20B H 0.9175 0.2610 0.3937 0.108 Uiso 1 1 calc R . . H20C H 0.7936 0.2409 0.3929 0.108 Uiso 1 1 calc R . . C21 C 0.6471(3) 0.1176(2) 0.4340(2) 0.0310(9) Uani 1 1 d . . . C22 C 0.7564(3) 0.0904(2) 0.4497(2) 0.0344(10) Uani 1 1 d . . . C23 C 0.8166(3) 0.0781(2) 0.3786(3) 0.0407(11) Uani 1 1 d . . . H23 H 0.7944 0.1147 0.3380 0.049 Uiso 1 1 calc R . . C24 C 0.7782(5) 0.0101(3) 0.3375(3) 0.0655(15) Uani 1 1 d . . . H24A H 0.8159 0.0022 0.2919 0.098 Uiso 1 1 calc R . . H24B H 0.6999 0.0119 0.3178 0.098 Uiso 1 1 calc R . . H24C H 0.7947 -0.0266 0.3768 0.098 Uiso 1 1 calc R . . C25 C 0.9432(4) 0.0795(3) 0.4009(4) 0.0695(17) Uani 1 1 d . . . H25A H 0.9744 0.0717 0.3521 0.104 Uiso 1 1 calc R . . H25B H 0.9676 0.0441 0.4407 0.104 Uiso 1 1 calc R . . H25C H 0.9667 0.1237 0.4238 0.104 Uiso 1 1 calc R . . C26 C 0.8004(4) 0.0710(2) 0.5293(3) 0.0410(11) Uani 1 1 d . . . H26 H 0.8724 0.0541 0.5405 0.049 Uiso 1 1 calc R . . C27 C 0.7408(4) 0.0760(2) 0.5930(3) 0.0465(12) Uani 1 1 d . . . H27 H 0.7728 0.0635 0.6465 0.056 Uiso 1 1 calc R . . C28 C 0.6338(4) 0.0996(2) 0.5765(3) 0.0422(11) Uani 1 1 d . . . H28 H 0.5933 0.1018 0.6192 0.051 Uiso 1 1 calc R . . C29 C 0.5839(3) 0.1203(2) 0.4975(2) 0.0341(10) Uani 1 1 d . . . C30 C 0.4647(3) 0.1451(2) 0.4834(3) 0.0422(11) Uani 1 1 d . . . H30 H 0.4413 0.1514 0.4238 0.051 Uiso 1 1 calc R . . C31 C 0.3869(4) 0.0917(3) 0.5115(3) 0.0541(13) Uani 1 1 d . . . H31A H 0.3951 0.0484 0.4849 0.081 Uiso 1 1 calc R . . H31B H 0.3118 0.1072 0.4968 0.081 Uiso 1 1 calc R . . H31C H 0.4051 0.0860 0.5703 0.081 Uiso 1 1 calc R . . C32 C 0.4537(4) 0.2142(3) 0.5240(4) 0.0625(15) Uani 1 1 d . . . H32A H 0.3774 0.2282 0.5139 0.094 Uiso 1 1 calc R . . H32B H 0.4973 0.2479 0.5014 0.094 Uiso 1 1 calc R . . H32C H 0.4792 0.2103 0.5824 0.094 Uiso 1 1 calc R . . C33 C 0.5052(5) 0.4155(3) 0.2642(3) 0.0632(15) Uani 1 1 d . . . H33A H 0.5844 0.4196 0.2755 0.095 Uiso 1 1 calc R . . H33B H 0.4725 0.4599 0.2692 0.095 Uiso 1 1 calc R . . H33C H 0.4821 0.3983 0.2091 0.095 Uiso 1 1 calc R . . C34 C 0.3066(4) 0.3460(3) 0.3186(4) 0.0650(15) Uani 1 1 d . . . H34A H 0.2845 0.3143 0.3576 0.098 Uiso 1 1 calc R . . H34B H 0.2828 0.3288 0.2636 0.098 Uiso 1 1 calc R . . H34C H 0.2733 0.3901 0.3241 0.098 Uiso 1 1 calc R . . C35 C 0.5057(6) 0.3931(3) 0.4434(3) 0.0748(18) Uani 1 1 d . . . H35A H 0.5849 0.3977 0.4538 0.112 Uiso 1 1 calc R . . H35B H 0.4834 0.3635 0.4844 0.112 Uiso 1 1 calc R . . H35C H 0.4725 0.4377 0.4457 0.112 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 V1 0.0299(4) 0.0382(5) 0.0262(4) 0.0029(3) 0.0053(3) 0.0049(3) Si1 0.0387(7) 0.0497(9) 0.0468(8) 0.0069(6) 0.0008(6) -0.0048(6) Si2 0.0507(8) 0.0376(8) 0.0379(7) -0.0012(6) 0.0088(6) 0.0037(6) N1 0.0329(18) 0.040(2) 0.0322(19) 0.0036(16) 0.0041(15) 0.0058(16) N2 0.0291(18) 0.039(2) 0.0290(19) 0.0028(15) 0.0047(15) 0.0013(15) N3 0.0324(18) 0.036(2) 0.0291(19) 0.0002(15) 0.0087(14) 0.0022(15) N4 0.044(2) 0.045(2) 0.035(2) -0.0010(17) 0.0055(16) 0.0015(17) C1 0.060(3) 0.048(4) 0.073(4) 0.017(3) 0.006(3) -0.003(2) C2 0.038(3) 0.120(5) 0.060(4) 0.015(3) 0.003(2) -0.006(3) C3 0.091(4) 0.051(4) 0.066(4) 0.003(3) -0.016(3) -0.009(3) C4 0.037(3) 0.055(3) 0.056(3) 0.005(2) -0.007(2) 0.005(2) C5 0.040(2) 0.039(3) 0.035(2) -0.004(2) 0.000(2) 0.005(2) C6 0.045(3) 0.036(3) 0.035(2) 0.010(2) 0.0027(19) 0.010(2) C7 0.046(3) 0.037(3) 0.029(2) 0.0020(19) 0.0084(19) 0.000(2) C8 0.056(3) 0.054(3) 0.048(3) 0.020(2) 0.011(2) 0.000(2) C9 0.033(2) 0.043(3) 0.029(2) 0.010(2) 0.0090(18) 0.0051(19) C10 0.040(2) 0.048(3) 0.037(3) 0.001(2) 0.0139(19) 0.002(2) C11 0.045(3) 0.065(4) 0.055(3) -0.017(3) 0.014(2) -0.005(2) C12 0.107(5) 0.074(5) 0.072(4) 0.002(3) -0.001(4) -0.036(4) C13 0.122(6) 0.085(5) 0.056(4) 0.003(3) -0.019(4) -0.026(4) C14 0.050(3) 0.056(3) 0.052(3) -0.008(2) 0.026(2) 0.003(2) C15 0.039(3) 0.066(4) 0.061(3) 0.004(3) 0.022(2) 0.010(2) C16 0.035(2) 0.058(4) 0.050(3) 0.012(3) 0.003(2) -0.002(2) C17 0.038(2) 0.043(3) 0.032(2) 0.008(2) 0.0070(19) 0.002(2) C18 0.046(3) 0.049(3) 0.046(3) -0.003(2) 0.001(2) -0.002(2) C19 0.104(5) 0.046(4) 0.073(4) 0.001(3) 0.023(3) -0.013(3) C20 0.097(4) 0.068(4) 0.053(3) -0.011(3) 0.018(3) -0.017(3) C21 0.037(2) 0.027(2) 0.028(2) 0.0029(17) 0.0042(17) -0.0025(18) C22 0.035(2) 0.031(3) 0.034(2) 0.0040(19) -0.0005(18) 0.0001(18) C23 0.036(2) 0.047(3) 0.039(3) 0.005(2) 0.0047(19) 0.008(2) C24 0.072(4) 0.061(4) 0.069(4) -0.013(3) 0.027(3) 0.006(3) C25 0.039(3) 0.104(5) 0.066(4) 0.019(3) 0.008(2) 0.013(3) C26 0.043(2) 0.037(3) 0.040(3) 0.004(2) -0.001(2) 0.005(2) C27 0.056(3) 0.046(3) 0.032(3) 0.008(2) -0.006(2) -0.003(2) C28 0.060(3) 0.041(3) 0.027(2) 0.0023(19) 0.010(2) -0.009(2) C29 0.043(2) 0.028(2) 0.031(2) -0.0017(18) 0.0041(18) -0.0054(18) C30 0.046(3) 0.048(3) 0.035(2) 0.001(2) 0.014(2) -0.001(2) C31 0.052(3) 0.060(4) 0.054(3) -0.002(3) 0.019(2) -0.010(2) C32 0.062(3) 0.052(4) 0.079(4) -0.004(3) 0.027(3) 0.005(3) C33 0.073(4) 0.049(4) 0.068(4) 0.009(3) 0.014(3) -0.003(3) C34 0.059(3) 0.064(4) 0.076(4) -0.003(3) 0.023(3) 0.015(3) C35 0.119(5) 0.056(4) 0.045(3) -0.012(3) 0.004(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N4 1.681(4) . ? V1 N3 1.701(3) . ? V1 N2 1.978(3) . ? V1 N1 1.979(3) . ? Si1 N1 1.777(4) . ? Si1 C1 1.850(5) . ? Si1 C3 1.855(5) . ? Si1 C2 1.856(6) . ? Si2 N4 1.720(4) . ? Si2 C33 1.854(5) . ? Si2 C34 1.863(5) . ? Si2 C35 1.862(5) . ? N1 C5 1.343(5) . ? N2 C7 1.336(5) . ? N2 C9 1.446(5) . ? N3 C21 1.401(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.516(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.399(6) . ? C6 C7 1.414(6) . ? C6 H6 0.9300 . ? C7 C8 1.503(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C17 1.400(6) . ? C9 C10 1.409(6) . ? C10 C14 1.385(6) . ? C10 C11 1.522(6) . ? C11 C12 1.508(8) . ? C11 C13 1.529(8) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.368(7) . ? C14 H14 0.9300 . ? C15 C16 1.374(7) . ? C15 H15 0.9300 . ? C16 C17 1.400(6) . ? C16 H16 0.9300 . ? C17 C18 1.510(6) . ? C18 C20 1.522(7) . ? C18 C19 1.528(7) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C29 1.406(6) . ? C21 C22 1.422(5) . ? C22 C26 1.378(6) . ? C22 C23 1.508(6) . ? C23 C24 1.518(7) . ? C23 C25 1.533(6) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.382(6) . ? C26 H26 0.9300 . ? C27 C28 1.371(6) . ? C27 H27 0.9300 . ? C28 C29 1.394(6) . ? C28 H28 0.9300 . ? C29 C30 1.519(6) . ? C30 C32 1.513(7) . ? C30 C31 1.533(6) . ? C30 H30 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? 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 N4 V1 N3 114.40(16) . . ? N4 V1 N2 108.07(16) . . ? N3 V1 N2 114.00(14) . . ? N4 V1 N1 109.07(16) . . ? N3 V1 N1 116.26(15) . . ? N2 V1 N1 92.89(13) . . ? N1 Si1 C1 108.9(2) . . ? N1 Si1 C3 112.1(2) . . ? C1 Si1 C3 106.4(3) . . ? N1 Si1 C2 109.3(2) . . ? C1 Si1 C2 109.7(3) . . ? C3 Si1 C2 110.5(3) . . ? N4 Si2 C33 109.5(2) . . ? N4 Si2 C34 107.5(2) . . ? C33 Si2 C34 110.4(3) . . ? N4 Si2 C35 113.4(2) . . ? C33 Si2 C35 106.5(3) . . ? C34 Si2 C35 109.6(3) . . ? C5 N1 Si1 125.3(3) . . ? C5 N1 V1 109.6(3) . . ? Si1 N1 V1 124.43(18) . . ? C7 N2 C9 119.2(3) . . ? C7 N2 V1 113.7(3) . . ? C9 N2 V1 127.1(2) . . ? C21 N3 V1 152.0(3) . . ? V1 N4 Si2 160.3(2) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 123.7(4) . . ? N1 C5 C4 121.3(4) . . ? C6 C5 C4 114.9(4) . . ? C5 C6 C7 128.1(4) . . ? C5 C6 H6 115.9 . . ? C7 C6 H6 115.9 . . ? N2 C7 C6 120.9(4) . . ? N2 C7 C8 120.8(4) . . ? C6 C7 C8 118.3(4) . . ? 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 . . ? C17 C9 C10 122.5(4) . . ? C17 C9 N2 120.1(4) . . ? C10 C9 N2 117.3(4) . . ? C14 C10 C9 117.3(4) . . ? C14 C10 C11 120.0(4) . . ? C9 C10 C11 122.7(4) . . ? C12 C11 C10 112.6(4) . . ? C12 C11 C13 109.7(5) . . ? C10 C11 C13 111.1(4) . . ? C12 C11 H11 107.8 . . ? C10 C11 H11 107.8 . . ? C13 C11 H11 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C10 121.5(5) . . ? C15 C14 H14 119.3 . . ? C10 C14 H14 119.3 . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 121.3(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C9 116.9(4) . . ? C16 C17 C18 120.9(4) . . ? C9 C17 C18 122.1(4) . . ? C17 C18 C20 112.2(4) . . ? C17 C18 C19 111.6(4) . . ? C20 C18 C19 109.7(4) . . ? C17 C18 H18 107.7 . . ? C20 C18 H18 107.7 . . ? C19 C18 H18 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C29 121.2(3) . . ? N3 C21 C22 118.5(3) . . ? C29 C21 C22 120.3(4) . . ? C26 C22 C21 118.3(4) . . ? C26 C22 C23 122.0(4) . . ? C21 C22 C23 119.5(3) . . ? C22 C23 C24 109.0(4) . . ? C22 C23 C25 115.2(4) . . ? C24 C23 C25 110.2(4) . . ? C22 C23 H23 107.4 . . ? C24 C23 H23 107.4 . . ? C25 C23 H23 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 C27 122.0(4) . . ? C22 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C28 C27 C26 119.2(4) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 122.0(4) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C21 118.1(4) . . ? C28 C29 C30 119.2(4) . . ? C21 C29 C30 122.7(4) . . ? C32 C30 C29 111.7(4) . . ? C32 C30 C31 110.9(4) . . ? C29 C30 C31 112.0(4) . . ? C32 C30 H30 107.3 . . ? C29 C30 H30 107.3 . . ? C31 C30 H30 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.474 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.175 # Attachment 'cpd_10_CCDC_764152.cif' data_7409 _database_code_depnum_ccdc_archive 'CCDC 764153' #TrackingRef 'cpd_10_CCDC_764152.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H59 N4 Si2 V' _chemical_formula_sum 'C35 H59 N4 Si2 V' _chemical_formula_weight 642.98 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 18.3009(6) _cell_length_b 10.2668(3) _cell_length_c 20.8551(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.0850(10) _cell_angle_gamma 90.00 _cell_volume 3896.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 18833 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9142 _exptl_absorpt_correction_T_max 0.9839 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22517 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.33 _reflns_number_total 6905 _reflns_number_gt 4270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1175P)^2^+1.9610P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0186(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6905 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2253 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.018 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 V1 V 0.25890(4) 0.79717(7) 0.12365(3) 0.0323(3) Uani 1 1 d . . . Si1 Si 0.39802(8) 0.62767(15) 0.06970(8) 0.0550(4) Uani 1 1 d . . . Si2 Si 0.17001(8) 0.89592(14) -0.01220(7) 0.0503(4) Uani 1 1 d . . . N1 N 0.30931(17) 0.8879(3) 0.19998(16) 0.0328(8) Uani 1 1 d . . . N2 N 0.19889(18) 0.6830(3) 0.17464(17) 0.0330(8) Uani 1 1 d . . . N3 N 0.3198(2) 0.7023(3) 0.09066(18) 0.0419(9) Uani 1 1 d . . . N4 N 0.2038(2) 0.8861(4) 0.06874(18) 0.0431(9) Uani 1 1 d . . . C1 C 0.3308(2) 1.0232(4) 0.2084(2) 0.0386(11) Uani 1 1 d . . . C2 C 0.3017(3) 1.0952(5) 0.2574(2) 0.0439(12) Uani 1 1 d . . . C3 C 0.2483(3) 1.0409(5) 0.2997(3) 0.0591(14) Uani 1 1 d . . . H3 H 0.2392 0.9479 0.2870 0.071 Uiso 1 1 calc R . . C4 C 0.2760(5) 1.0424(8) 0.3711(3) 0.112(3) Uani 1 1 d . . . H4A H 0.2390 1.0034 0.3959 0.169 Uiso 1 1 calc R . . H4B H 0.2853 1.1325 0.3853 0.169 Uiso 1 1 calc R . . H4C H 0.3217 0.9922 0.3782 0.169 Uiso 1 1 calc R . . C5 C 0.1744(4) 1.1128(7) 0.2884(4) 0.094(2) Uani 1 1 d . . . H5A H 0.1396 1.0744 0.3157 0.141 Uiso 1 1 calc R . . H5B H 0.1548 1.1047 0.2430 0.141 Uiso 1 1 calc R . . H5C H 0.1816 1.2050 0.2994 0.141 Uiso 1 1 calc R . . C6 C 0.3240(3) 1.2246(5) 0.2668(3) 0.0537(13) Uani 1 1 d . . . H6 H 0.3063 1.2736 0.3005 0.064 Uiso 1 1 calc R . . C7 C 0.3709(3) 1.2824(5) 0.2280(3) 0.0566(14) Uani 1 1 d . . . H7 H 0.3848 1.3709 0.2346 0.068 Uiso 1 1 calc R . . C8 C 0.3977(3) 1.2115(5) 0.1797(3) 0.0516(13) Uani 1 1 d . . . H8 H 0.4299 1.2524 0.1530 0.062 Uiso 1 1 calc R . . C9 C 0.3787(2) 1.0810(5) 0.1687(2) 0.0424(11) Uani 1 1 d . . . C10 C 0.4110(3) 1.0098(5) 0.1148(2) 0.0493(12) Uani 1 1 d . . . H10 H 0.3949 0.9168 0.1162 0.059 Uiso 1 1 calc R . . C11 C 0.3818(3) 1.0644(6) 0.0491(3) 0.0709(17) Uani 1 1 d . . . H11A H 0.4027 1.0153 0.0152 0.106 Uiso 1 1 calc R . . H11B H 0.3957 1.1563 0.0466 0.106 Uiso 1 1 calc R . . H11C H 0.3281 1.0568 0.0433 0.106 Uiso 1 1 calc R . . C12 C 0.4958(3) 1.0114(7) 0.1240(3) 0.0779(19) Uani 1 1 d . . . H12A H 0.5148 0.9628 0.0889 0.117 Uiso 1 1 calc R . . H12B H 0.5133 0.9709 0.1654 0.117 Uiso 1 1 calc R . . H12C H 0.5133 1.1017 0.1236 0.117 Uiso 1 1 calc R . . C13 C 0.4047(3) 0.8340(5) 0.2886(3) 0.0589(15) Uani 1 1 d . . . H13A H 0.4176 0.9254 0.2825 0.088 Uiso 1 1 calc R . . H13B H 0.4450 0.7781 0.2777 0.088 Uiso 1 1 calc R . . H13C H 0.3963 0.8196 0.3337 0.088 Uiso 1 1 calc R . . C14 C 0.3357(2) 0.8013(4) 0.2454(2) 0.0395(11) Uani 1 1 d . . . C15 C 0.3022(2) 0.6818(4) 0.2555(2) 0.0390(11) Uani 1 1 d . . . H15 H 0.3297 0.6245 0.2846 0.047 Uiso 1 1 calc R . . C16 C 0.2333(2) 0.6340(4) 0.2287(2) 0.0378(10) Uani 1 1 d . . . C17 C 0.1999(3) 0.5259(5) 0.2644(2) 0.0514(13) Uani 1 1 d . . . H17A H 0.1473 0.5430 0.2657 0.077 Uiso 1 1 calc R . . H17B H 0.2242 0.5212 0.3086 0.077 Uiso 1 1 calc R . . H17C H 0.2062 0.4430 0.2424 0.077 Uiso 1 1 calc R . . C18 C 0.1258(2) 0.6372(4) 0.1507(2) 0.0379(11) Uani 1 1 d . . . C19 C 0.1183(3) 0.5206(5) 0.1147(2) 0.0433(11) Uani 1 1 d . . . C20 C 0.1822(3) 0.4364(5) 0.1003(2) 0.0508(13) Uani 1 1 d . . . H20 H 0.2282 0.4749 0.1225 0.061 Uiso 1 1 calc R . . C21 C 0.1884(4) 0.4354(6) 0.0277(3) 0.0727(17) Uani 1 1 d . . . H21A H 0.2299 0.3807 0.0187 0.109 Uiso 1 1 calc R . . H21B H 0.1961 0.5245 0.0129 0.109 Uiso 1 1 calc R . . H21C H 0.1429 0.4005 0.0050 0.109 Uiso 1 1 calc R . . C22 C 0.1755(4) 0.2970(5) 0.1241(3) 0.0733(17) Uani 1 1 d . . . H22A H 0.2181 0.2463 0.1139 0.110 Uiso 1 1 calc R . . H22B H 0.1304 0.2576 0.1030 0.110 Uiso 1 1 calc R . . H22C H 0.1735 0.2974 0.1709 0.110 Uiso 1 1 calc R . . C23 C 0.0474(3) 0.4843(6) 0.0903(2) 0.0567(14) Uani 1 1 d . . . H23 H 0.0404 0.4059 0.0662 0.068 Uiso 1 1 calc R . . C24 C -0.0120(3) 0.5580(6) 0.1000(3) 0.0618(15) Uani 1 1 d . . . H24 H -0.0596 0.5309 0.0824 0.074 Uiso 1 1 calc R . . C25 C -0.0040(3) 0.6707(6) 0.1347(3) 0.0615(15) Uani 1 1 d . . . H25 H -0.0464 0.7206 0.1410 0.074 Uiso 1 1 calc R . . C26 C 0.0653(2) 0.7149(5) 0.1616(2) 0.0462(12) Uani 1 1 d . . . C27 C 0.0727(3) 0.8373(5) 0.2001(3) 0.0562(14) Uani 1 1 d . . . H27 H 0.1261 0.8582 0.2092 0.067 Uiso 1 1 calc R . . C28 C 0.0418(5) 0.8168(8) 0.2639(5) 0.121(2) Uani 1 1 d . . . H28A H 0.0470 0.8972 0.2893 0.181 Uiso 1 1 calc R . . H28B H 0.0687 0.7463 0.2877 0.181 Uiso 1 1 calc R . . H28C H -0.0103 0.7936 0.2560 0.181 Uiso 1 1 calc R . . C29 C 0.0343(5) 0.9535(8) 0.1655(4) 0.121(2) Uani 1 1 d . . . H29A H 0.0412 1.0309 0.1930 0.181 Uiso 1 1 calc R . . H29B H -0.0183 0.9350 0.1565 0.181 Uiso 1 1 calc R . . H29C H 0.0554 0.9692 0.1250 0.181 Uiso 1 1 calc R . . C30 C 0.4325(4) 0.7123(6) -0.0002(3) 0.084(2) Uani 1 1 d . . . H30A H 0.3943 0.7113 -0.0369 0.126 Uiso 1 1 calc R . . H30B H 0.4764 0.6676 -0.0121 0.126 Uiso 1 1 calc R . . H30C H 0.4449 0.8027 0.0116 0.126 Uiso 1 1 calc R . . C31 C 0.4699(3) 0.6304(7) 0.1397(4) 0.096(2) Uani 1 1 d . . . H31A H 0.4804 0.7208 0.1527 0.144 Uiso 1 1 calc R . . H31B H 0.5148 0.5894 0.1275 0.144 Uiso 1 1 calc R . . H31C H 0.4524 0.5824 0.1757 0.144 Uiso 1 1 calc R . . C32 C 0.3796(4) 0.4550(6) 0.0463(4) 0.0824(19) Uani 1 1 d . . . H32A H 0.3422 0.4516 0.0091 0.124 Uiso 1 1 calc R . . H32B H 0.3619 0.4079 0.0825 0.124 Uiso 1 1 calc R . . H32C H 0.4250 0.4144 0.0350 0.124 Uiso 1 1 calc R . . C33 C 0.2336(4) 0.8132(7) -0.0627(3) 0.089(2) Uani 1 1 d . . . H33A H 0.2391 0.7218 -0.0496 0.134 Uiso 1 1 calc R . . H33B H 0.2816 0.8563 -0.0570 0.134 Uiso 1 1 calc R . . H33C H 0.2135 0.8179 -0.1081 0.134 Uiso 1 1 calc R . . C34 C 0.1602(4) 1.0681(6) -0.0379(3) 0.0768(19) Uani 1 1 d . . . H34A H 0.2085 1.1105 -0.0327 0.115 Uiso 1 1 calc R . . H34B H 0.1270 1.1131 -0.0114 0.115 Uiso 1 1 calc R . . H34C H 0.1400 1.0720 -0.0833 0.115 Uiso 1 1 calc R . . C35 C 0.0789(4) 0.8128(7) -0.0230(3) 0.093(2) Uani 1 1 d . . . H35A H 0.0848 0.7217 -0.0094 0.139 Uiso 1 1 calc R . . H35B H 0.0592 0.8163 -0.0686 0.139 Uiso 1 1 calc R . . H35C H 0.0450 0.8567 0.0032 0.139 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 V1 0.0331(4) 0.0340(4) 0.0298(4) 0.0008(3) 0.0038(3) -0.0006(3) Si1 0.0490(9) 0.0540(9) 0.0647(10) 0.0055(7) 0.0189(7) 0.0148(7) Si2 0.0639(9) 0.0468(9) 0.0378(8) 0.0031(6) -0.0063(7) -0.0028(7) N1 0.0322(19) 0.037(2) 0.0287(19) 0.0007(16) 0.0022(15) -0.0004(15) N2 0.0333(19) 0.033(2) 0.0320(19) 0.0010(16) 0.0022(15) 0.0017(15) N3 0.042(2) 0.040(2) 0.045(2) 0.0000(18) 0.0122(18) 0.0013(17) N4 0.045(2) 0.048(2) 0.036(2) 0.0012(18) 0.0014(17) -0.0069(18) C1 0.034(2) 0.043(3) 0.037(2) 0.001(2) -0.005(2) -0.003(2) C2 0.051(3) 0.040(3) 0.039(3) 0.004(2) -0.001(2) 0.004(2) C3 0.083(4) 0.046(3) 0.053(3) -0.001(3) 0.028(3) 0.002(3) C4 0.170(8) 0.119(6) 0.051(4) 0.011(4) 0.027(5) -0.002(6) C5 0.081(5) 0.080(5) 0.131(7) 0.005(4) 0.058(4) 0.008(4) C6 0.064(3) 0.044(3) 0.052(3) -0.006(2) 0.000(3) 0.001(3) C7 0.060(3) 0.039(3) 0.068(4) 0.001(3) -0.002(3) -0.009(2) C8 0.045(3) 0.048(3) 0.062(3) 0.003(3) 0.002(2) -0.010(2) C9 0.036(2) 0.043(3) 0.047(3) 0.002(2) -0.002(2) -0.005(2) C10 0.044(3) 0.048(3) 0.058(3) 0.001(2) 0.016(2) -0.011(2) C11 0.090(4) 0.072(4) 0.052(3) 0.005(3) 0.015(3) -0.009(3) C12 0.047(3) 0.086(5) 0.104(5) -0.010(4) 0.023(3) -0.011(3) C13 0.053(3) 0.057(3) 0.061(3) 0.006(3) -0.021(3) -0.004(2) C14 0.036(2) 0.042(3) 0.039(2) -0.002(2) -0.0030(19) 0.006(2) C15 0.045(3) 0.036(3) 0.035(2) 0.004(2) -0.001(2) 0.002(2) C16 0.047(3) 0.033(2) 0.034(2) -0.001(2) 0.007(2) 0.000(2) C17 0.067(3) 0.046(3) 0.041(3) 0.008(2) 0.004(2) -0.010(2) C18 0.035(2) 0.045(3) 0.034(2) 0.005(2) 0.0049(19) -0.009(2) C19 0.047(3) 0.048(3) 0.035(2) 0.005(2) 0.003(2) -0.012(2) C20 0.063(3) 0.045(3) 0.044(3) -0.012(2) 0.004(2) -0.006(2) C21 0.095(5) 0.069(4) 0.057(4) -0.008(3) 0.021(3) -0.001(3) C22 0.100(5) 0.054(4) 0.064(4) -0.002(3) -0.002(3) 0.002(3) C23 0.057(3) 0.065(4) 0.047(3) 0.000(3) 0.003(3) -0.023(3) C24 0.047(3) 0.081(4) 0.056(3) 0.004(3) 0.000(3) -0.026(3) C25 0.035(3) 0.084(4) 0.067(4) 0.014(3) 0.010(3) -0.003(3) C26 0.035(3) 0.052(3) 0.053(3) 0.009(2) 0.010(2) -0.002(2) C27 0.046(3) 0.059(3) 0.065(4) -0.003(3) 0.015(3) 0.013(2) C28 0.136(5) 0.098(4) 0.129(5) -0.032(4) 0.015(4) -0.001(4) C29 0.136(5) 0.098(4) 0.129(5) -0.032(4) 0.015(4) -0.001(4) C30 0.081(4) 0.082(5) 0.100(5) 0.015(4) 0.062(4) 0.019(3) C31 0.062(4) 0.098(5) 0.123(6) 0.010(5) -0.013(4) 0.018(4) C32 0.088(5) 0.062(4) 0.102(5) -0.001(4) 0.033(4) 0.021(3) C33 0.140(6) 0.088(5) 0.040(3) 0.006(3) 0.010(4) 0.032(4) C34 0.104(5) 0.056(4) 0.064(4) 0.004(3) -0.019(4) 0.002(3) C35 0.091(5) 0.104(5) 0.076(4) 0.014(4) -0.030(4) -0.032(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 V1 N3 1.681(4) . ? V1 N4 1.708(4) . ? V1 N1 1.985(3) . ? V1 N2 1.990(4) . ? Si1 N3 1.720(4) . ? Si1 C32 1.860(6) . ? Si1 C31 1.859(7) . ? Si1 C30 1.864(6) . ? Si2 N4 1.738(4) . ? Si2 C34 1.851(6) . ? Si2 C33 1.855(7) . ? Si2 C35 1.865(6) . ? N1 C14 1.350(5) . ? N1 C1 1.449(6) . ? N2 C16 1.331(5) . ? N2 C18 1.455(5) . ? C1 C9 1.399(6) . ? C1 C2 1.412(6) . ? C2 C6 1.397(7) . ? C2 C3 1.493(7) . ? C3 C4 1.521(8) . ? C3 C5 1.537(8) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.374(7) . ? C6 H6 0.9500 . ? C7 C8 1.376(7) . ? C7 H7 0.9500 . ? C8 C9 1.398(7) . ? C8 H8 0.9500 . ? C9 C10 1.513(7) . ? C10 C11 1.524(7) . ? C10 C12 1.545(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 C14 1.510(6) . ? C13 H13A 0.9801 . ? C13 H13B 0.9801 . ? C13 H13C 0.9801 . ? C14 C15 1.398(6) . ? C15 C16 1.411(6) . ? C15 H15 0.9500 . ? C16 C17 1.503(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C26 1.402(6) . ? C18 C19 1.413(6) . ? C19 C23 1.393(6) . ? C19 C20 1.510(7) . ? C20 C22 1.524(7) . ? C20 C21 1.530(7) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.357(8) . ? C23 H23 0.9500 . ? C24 C25 1.365(8) . ? C24 H24 0.9500 . ? C25 C26 1.407(7) . ? C25 H25 0.9500 . ? C26 C27 1.490(7) . ? C27 C28 1.514(11) . ? C27 C29 1.526(9) . ? 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 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 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 N3 V1 N4 113.90(18) . . ? N3 V1 N1 109.15(16) . . ? N4 V1 N1 118.56(16) . . ? N3 V1 N2 107.74(16) . . ? N4 V1 N2 110.69(16) . . ? N1 V1 N2 94.81(14) . . ? N3 Si1 C32 111.0(2) . . ? N3 Si1 C31 109.4(3) . . ? C32 Si1 C31 108.3(3) . . ? N3 Si1 C30 110.5(2) . . ? C32 Si1 C30 107.8(3) . . ? C31 Si1 C30 109.7(4) . . ? N4 Si2 C34 110.5(2) . . ? N4 Si2 C33 110.1(2) . . ? C34 Si2 C33 108.7(3) . . ? N4 Si2 C35 108.2(3) . . ? C34 Si2 C35 110.1(3) . . ? C33 Si2 C35 109.1(4) . . ? C14 N1 C1 118.3(3) . . ? C14 N1 V1 110.7(3) . . ? C1 N1 V1 130.1(3) . . ? C16 N2 C18 120.3(4) . . ? C16 N2 V1 115.9(3) . . ? C18 N2 V1 123.1(3) . . ? V1 N3 Si1 165.4(3) . . ? V1 N4 Si2 143.7(3) . . ? C9 C1 C2 120.9(4) . . ? C9 C1 N1 120.9(4) . . ? C2 C1 N1 118.1(4) . . ? C6 C2 C1 118.2(5) . . ? C6 C2 C3 118.2(5) . . ? C1 C2 C3 123.6(4) . . ? C2 C3 C4 113.7(5) . . ? C2 C3 C5 110.6(5) . . ? C4 C3 C5 110.0(6) . . ? C2 C3 H3 107.4 . . ? C4 C3 H3 107.4 . . ? C5 C3 H3 107.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.3(5) . . ? C7 C6 H6 119.3 . . ? C2 C6 H6 119.4 . . ? C8 C7 C6 119.8(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 121.7(5) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C1 118.1(5) . . ? C8 C9 C10 118.4(4) . . ? C1 C9 C10 123.6(4) . . ? C9 C10 C11 111.3(4) . . ? C9 C10 C12 111.7(4) . . ? C11 C10 C12 111.1(5) . . ? C9 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C12 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 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 123.7(4) . . ? N1 C14 C13 119.1(4) . . ? C15 C14 C13 117.2(4) . . ? C14 C15 C16 129.2(4) . . ? C14 C15 H15 115.4 . . ? C16 C15 H15 115.4 . . ? N2 C16 C15 121.8(4) . . ? N2 C16 C17 121.2(4) . . ? C15 C16 C17 117.0(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C18 C19 122.3(4) . . ? C26 C18 N2 118.3(4) . . ? C19 C18 N2 119.3(4) . . ? C23 C19 C18 117.1(5) . . ? C23 C19 C20 119.0(5) . . ? C18 C19 C20 123.9(4) . . ? C19 C20 C22 112.5(5) . . ? C19 C20 C21 109.9(4) . . ? C22 C20 C21 109.5(4) . . ? C19 C20 H20 108.3 . . ? C22 C20 H20 108.3 . . ? C21 C20 H20 108.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.7(5) . . ? C24 C23 H23 119.1 . . ? C19 C23 H23 119.2 . . ? C23 C24 C25 120.7(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 121.7(5) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C18 C26 C25 116.5(5) . . ? C18 C26 C27 122.6(4) . . ? C25 C26 C27 120.8(5) . . ? C26 C27 C28 109.7(5) . . ? C26 C27 C29 113.2(5) . . ? C28 C27 C29 109.2(6) . . ? C26 C27 H27 108.3 . . ? C28 C27 H27 108.2 . . ? C29 C27 H27 108.2 . . ? 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 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.841 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.206 data_7790 _database_code_depnum_ccdc_archive 'CCDC 764154' #TrackingRef 'CCDC 764154.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H63 Cr N6 O' _chemical_formula_sum 'C47 H63 Cr N6 O' _chemical_formula_weight 780.03 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.8881(5) _cell_length_b 12.8734(5) _cell_length_c 16.1682(8) _cell_angle_alpha 105.496(2) _cell_angle_beta 90.870(2) _cell_angle_gamma 91.470(2) _cell_volume 2182.58(17) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 25734 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 838 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8868 _exptl_absorpt_correction_T_max 0.8957 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27281 _diffrn_reflns_av_R_equivalents 0.1139 _diffrn_reflns_av_sigmaI/netI 0.1372 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.43 _reflns_number_total 7841 _reflns_number_gt 4194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1166P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.037(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7841 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1541 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.1980 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 Cr1 Cr 0.32844(7) 0.21654(6) 0.77610(5) 0.0364(3) Uani 1 1 d . . . N1 N 0.2012(3) 0.3191(3) 0.8314(2) 0.0370(9) Uani 1 1 d . . . N2 N 0.2118(3) 0.1499(3) 0.6800(2) 0.0372(9) Uani 1 1 d . . . N3 N 0.3893(4) 0.1137(3) 0.8311(2) 0.0391(10) Uani 1 1 d . . . N4 N 0.5147(4) 0.1080(3) 0.8415(3) 0.0454(11) Uani 1 1 d . . . N5 N 0.5768(4) 0.1732(3) 0.8109(3) 0.0438(10) Uani 1 1 d . . . N6 N 0.5057(3) 0.2402(3) 0.7777(2) 0.0386(10) Uani 1 1 d . . . C1 C 0.2447(4) 0.4169(4) 0.8936(3) 0.0382(12) Uani 1 1 d . . . C2 C 0.2573(5) 0.5126(4) 0.8662(3) 0.0447(13) Uani 1 1 d . . . C3 C 0.2258(5) 0.5163(4) 0.7755(4) 0.0541(14) Uani 1 1 d . . . H3 H 0.2438 0.4458 0.7371 0.065 Uiso 1 1 calc R . . C4 C 0.0898(6) 0.5362(5) 0.7625(4) 0.0756(19) Uani 1 1 d . . . H4A H 0.0747 0.5373 0.7041 0.113 Uiso 1 1 calc R . . H4B H 0.0688 0.6043 0.8003 0.113 Uiso 1 1 calc R . . H4C H 0.0405 0.4796 0.7750 0.113 Uiso 1 1 calc R . . C5 C 0.3026(6) 0.6021(5) 0.7465(5) 0.077(2) Uani 1 1 d . . . H5A H 0.2797 0.6001 0.6885 0.116 Uiso 1 1 calc R . . H5B H 0.3883 0.5873 0.7494 0.116 Uiso 1 1 calc R . . H5C H 0.2877 0.6722 0.7835 0.116 Uiso 1 1 calc R . . C6 C 0.3004(5) 0.6057(4) 0.9273(4) 0.0586(15) Uani 1 1 d . . . H6 H 0.3116 0.6694 0.9112 0.070 Uiso 1 1 calc R . . C7 C 0.3267(5) 0.6050(5) 1.0108(4) 0.0623(16) Uani 1 1 d . . . H7 H 0.3534 0.6685 1.0504 0.075 Uiso 1 1 calc R . . C8 C 0.3140(5) 0.5132(4) 1.0361(4) 0.0562(14) Uani 1 1 d . . . H8 H 0.3331 0.5143 1.0926 0.067 Uiso 1 1 calc R . . C9 C 0.2727(4) 0.4169(4) 0.9785(3) 0.0431(12) Uani 1 1 d . . . C10 C 0.2565(5) 0.3171(4) 1.0112(3) 0.0459(13) Uani 1 1 d . . . H10 H 0.2193 0.2595 0.9645 0.055 Uiso 1 1 calc R . . C11 C 0.3801(5) 0.2788(5) 1.0354(4) 0.0573(15) Uani 1 1 d . . . H11A H 0.3673 0.2153 1.0550 0.086 Uiso 1 1 calc R . . H11B H 0.4193 0.3346 1.0803 0.086 Uiso 1 1 calc R . . H11C H 0.4314 0.2623 0.9861 0.086 Uiso 1 1 calc R . . C12 C 0.1700(5) 0.3372(5) 1.0870(4) 0.0605(15) Uani 1 1 d . . . H12A H 0.1603 0.2726 1.1055 0.091 Uiso 1 1 calc R . . H12B H 0.0914 0.3574 1.0697 0.091 Uiso 1 1 calc R . . H12C H 0.2039 0.3942 1.1334 0.091 Uiso 1 1 calc R . . C13 C -0.0081(4) 0.3619(4) 0.8855(3) 0.0460(13) Uani 1 1 d . . . H13A H 0.0217 0.4354 0.9051 0.069 Uiso 1 1 calc R . . H13B H -0.0143 0.3315 0.9335 0.069 Uiso 1 1 calc R . . H13C H -0.0877 0.3596 0.8585 0.069 Uiso 1 1 calc R . . C14 C 0.0795(4) 0.2979(4) 0.8217(3) 0.0365(11) Uani 1 1 d . . . C15 C 0.0292(4) 0.2162(4) 0.7545(3) 0.0380(11) Uani 1 1 d . . . H15 H -0.0546 0.2016 0.7568 0.046 Uiso 1 1 calc R . . C16 C 0.0895(4) 0.1537(4) 0.6840(3) 0.0407(12) Uani 1 1 d . . . C17 C 0.0116(5) 0.0866(4) 0.6087(3) 0.0528(14) Uani 1 1 d . . . H17A H 0.0381 0.1015 0.5566 0.079 Uiso 1 1 calc R . . H17B H -0.0731 0.1045 0.6175 0.079 Uiso 1 1 calc R . . H17C H 0.0206 0.0114 0.6045 0.079 Uiso 1 1 calc R . . C18 C 0.2662(4) 0.0936(4) 0.6000(3) 0.0402(12) Uani 1 1 d . . . C19 C 0.2792(4) -0.0195(4) 0.5777(3) 0.0428(12) Uani 1 1 d . . . C20 C 0.2458(5) -0.0874(4) 0.6375(3) 0.0480(13) Uani 1 1 d . . . H20 H 0.2025 -0.0421 0.6861 0.058 Uiso 1 1 calc R . . C21 C 0.3628(5) -0.1273(5) 0.6726(4) 0.0618(16) Uani 1 1 d . . . H21A H 0.3403 -0.1697 0.7110 0.093 Uiso 1 1 calc R . . H21B H 0.4134 -0.0664 0.7030 0.093 Uiso 1 1 calc R . . H21C H 0.4076 -0.1706 0.6258 0.093 Uiso 1 1 calc R . . C22 C 0.1616(6) -0.1841(5) 0.5943(4) 0.0685(17) Uani 1 1 d . . . H22A H 0.1426 -0.2245 0.6347 0.103 Uiso 1 1 calc R . . H22B H 0.2024 -0.2294 0.5463 0.103 Uiso 1 1 calc R . . H22C H 0.0871 -0.1592 0.5747 0.103 Uiso 1 1 calc R . . C23 C 0.3269(5) -0.0691(4) 0.4980(3) 0.0473(13) Uani 1 1 d . . . H23 H 0.3342 -0.1436 0.4817 0.057 Uiso 1 1 calc R . . C24 C 0.3633(5) -0.0104(4) 0.4432(3) 0.0524(14) Uani 1 1 d . . . H24 H 0.3953 -0.0452 0.3904 0.063 Uiso 1 1 calc R . . C25 C 0.3530(5) 0.1005(5) 0.4655(3) 0.0530(14) Uani 1 1 d . . . H25 H 0.3774 0.1389 0.4271 0.064 Uiso 1 1 calc R . . C26 C 0.3070(4) 0.1555(4) 0.5439(3) 0.0421(12) Uani 1 1 d . . . C27 C 0.2992(5) 0.2769(4) 0.5687(3) 0.0550(15) Uani 1 1 d . . . H27 H 0.3117 0.3013 0.6312 0.066 Uiso 1 1 calc R . . C28 C 0.4004(6) 0.3333(5) 0.5295(4) 0.0685(17) Uani 1 1 d . . . H28A H 0.3912 0.4099 0.5480 0.103 Uiso 1 1 calc R . . H28B H 0.3937 0.3094 0.4680 0.103 Uiso 1 1 calc R . . H28C H 0.4796 0.3157 0.5480 0.103 Uiso 1 1 calc R . . C29 C 0.1732(6) 0.3143(5) 0.5492(4) 0.0705(18) Uani 1 1 d . . . H29A H 0.1723 0.3916 0.5672 0.106 Uiso 1 1 calc R . . H29B H 0.1119 0.2851 0.5794 0.106 Uiso 1 1 calc R . . H29C H 0.1558 0.2898 0.4886 0.106 Uiso 1 1 calc R . . C30 C 0.3230(4) 0.0432(4) 0.8704(3) 0.0382(11) Uani 1 1 d . . . C31 C 0.3819(4) -0.0203(4) 0.9157(3) 0.0418(12) Uani 1 1 d . . . H31 H 0.4673 -0.0188 0.9196 0.050 Uiso 1 1 calc R . . C32 C 0.3138(5) -0.0860(4) 0.9552(3) 0.0451(13) Uani 1 1 d . . . H32 H 0.3544 -0.1267 0.9861 0.054 Uiso 1 1 calc R . . C33 C 0.1867(5) -0.0916(4) 0.9492(3) 0.0452(13) Uani 1 1 d . . . C34 C 0.1147(5) -0.1619(4) 0.9943(4) 0.0586(15) Uani 1 1 d . . . H34A H 0.0337 -0.1346 1.0059 0.088 Uiso 1 1 calc R . . H34B H 0.1560 -0.1612 1.0473 0.088 Uiso 1 1 calc R . . H34C H 0.1087 -0.2344 0.9581 0.088 Uiso 1 1 calc R . . C35 C 0.1296(5) -0.0284(4) 0.9035(3) 0.0482(13) Uani 1 1 d . . . H35 H 0.0444 -0.0312 0.8983 0.058 Uiso 1 1 calc R . . C36 C 0.1959(5) 0.0382(4) 0.8654(3) 0.0448(13) Uani 1 1 d . . . H36 H 0.1547 0.0804 0.8360 0.054 Uiso 1 1 calc R . . C37 C 0.5805(4) 0.3071(4) 0.7405(3) 0.0387(12) Uani 1 1 d . . . C38 C 0.6912(5) 0.2738(4) 0.7031(3) 0.0475(13) Uani 1 1 d . . . H38 H 0.7199 0.2062 0.7028 0.057 Uiso 1 1 calc R . . C39 C 0.7591(5) 0.3409(4) 0.6661(4) 0.0525(14) Uani 1 1 d . . . H39 H 0.8341 0.3177 0.6423 0.063 Uiso 1 1 calc R . . C40 C 0.7202(5) 0.4409(4) 0.6631(4) 0.0551(15) Uani 1 1 d . . . C41 C 0.7936(6) 0.5108(5) 0.6184(5) 0.081(2) Uani 1 1 d . . . H41A H 0.8643 0.4729 0.5930 0.121 Uiso 1 1 calc R . . H41B H 0.8196 0.5767 0.6594 0.121 Uiso 1 1 calc R . . H41C H 0.7432 0.5270 0.5745 0.121 Uiso 1 1 calc R . . C42 C 0.6104(5) 0.4745(4) 0.7023(4) 0.0591(16) Uani 1 1 d . . . H42 H 0.5827 0.5426 0.7033 0.071 Uiso 1 1 calc R . . C43 C 0.5414(5) 0.4087(4) 0.7398(4) 0.0506(14) Uani 1 1 d . . . H43 H 0.4675 0.4328 0.7650 0.061 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 0.0371(5) 0.0345(5) 0.0361(5) 0.0070(4) -0.0040(3) 0.0027(3) N1 0.042(2) 0.027(2) 0.039(2) 0.0049(18) 0.0008(18) 0.0007(17) N2 0.039(2) 0.035(2) 0.035(2) 0.0047(19) -0.0045(18) 0.0014(17) N3 0.042(2) 0.039(2) 0.037(2) 0.0118(19) -0.0022(19) 0.0044(18) N4 0.039(2) 0.046(3) 0.054(3) 0.019(2) -0.005(2) 0.006(2) N5 0.040(2) 0.042(2) 0.051(3) 0.017(2) -0.005(2) 0.0001(19) N6 0.038(2) 0.036(2) 0.040(2) 0.0075(19) -0.0068(19) -0.0010(18) C1 0.035(3) 0.033(3) 0.044(3) 0.005(2) 0.005(2) 0.000(2) C2 0.049(3) 0.034(3) 0.049(3) 0.007(3) 0.011(3) 0.004(2) C3 0.064(4) 0.037(3) 0.062(4) 0.014(3) 0.012(3) 0.011(3) C4 0.084(5) 0.077(4) 0.076(5) 0.035(4) 0.011(4) 0.015(4) C5 0.087(5) 0.059(4) 0.097(5) 0.038(4) 0.018(4) 0.013(3) C6 0.064(4) 0.040(3) 0.068(4) 0.006(3) 0.016(3) -0.005(3) C7 0.066(4) 0.041(3) 0.067(4) -0.008(3) 0.004(3) -0.011(3) C8 0.059(4) 0.054(4) 0.045(3) -0.003(3) -0.002(3) -0.005(3) C9 0.039(3) 0.048(3) 0.040(3) 0.007(3) 0.003(2) 0.003(2) C10 0.051(3) 0.046(3) 0.038(3) 0.007(2) -0.006(3) -0.004(2) C11 0.058(4) 0.067(4) 0.046(3) 0.011(3) -0.004(3) 0.008(3) C12 0.061(4) 0.062(4) 0.057(4) 0.014(3) 0.005(3) 0.000(3) C13 0.046(3) 0.042(3) 0.045(3) 0.002(3) 0.005(2) 0.005(2) C14 0.036(3) 0.033(3) 0.041(3) 0.012(2) 0.000(2) 0.004(2) C15 0.036(3) 0.038(3) 0.040(3) 0.011(2) -0.003(2) 0.002(2) C16 0.042(3) 0.037(3) 0.043(3) 0.011(2) -0.008(2) 0.004(2) C17 0.041(3) 0.057(3) 0.053(3) 0.004(3) -0.008(3) 0.002(3) C18 0.037(3) 0.046(3) 0.034(3) 0.004(2) -0.009(2) 0.003(2) C19 0.039(3) 0.044(3) 0.041(3) 0.003(3) -0.004(2) 0.004(2) C20 0.052(3) 0.043(3) 0.047(3) 0.009(3) 0.001(3) 0.002(2) C21 0.071(4) 0.054(3) 0.059(4) 0.013(3) -0.003(3) 0.008(3) C22 0.079(4) 0.055(4) 0.071(4) 0.016(3) -0.001(3) -0.001(3) C23 0.048(3) 0.040(3) 0.048(3) 0.002(3) -0.004(3) 0.003(2) C24 0.060(4) 0.052(4) 0.039(3) -0.002(3) 0.004(3) 0.008(3) C25 0.056(3) 0.061(4) 0.041(3) 0.012(3) 0.001(3) 0.000(3) C26 0.046(3) 0.042(3) 0.038(3) 0.010(3) -0.005(2) 0.003(2) C27 0.077(4) 0.054(3) 0.037(3) 0.017(3) 0.000(3) 0.004(3) C28 0.086(5) 0.055(4) 0.063(4) 0.015(3) -0.004(3) -0.010(3) C29 0.084(5) 0.059(4) 0.075(4) 0.028(3) 0.005(4) 0.012(3) C30 0.047(3) 0.031(3) 0.035(3) 0.006(2) -0.003(2) 0.000(2) C31 0.040(3) 0.038(3) 0.044(3) 0.005(2) -0.003(2) 0.000(2) C32 0.058(3) 0.036(3) 0.039(3) 0.008(2) -0.002(3) 0.001(2) C33 0.055(3) 0.034(3) 0.044(3) 0.005(2) 0.007(3) -0.002(2) C34 0.060(4) 0.044(3) 0.072(4) 0.016(3) 0.018(3) 0.000(3) C35 0.039(3) 0.044(3) 0.057(3) 0.005(3) 0.002(3) -0.001(2) C36 0.047(3) 0.042(3) 0.046(3) 0.012(3) -0.008(2) 0.007(2) C37 0.038(3) 0.043(3) 0.034(3) 0.011(2) -0.008(2) -0.001(2) C38 0.051(3) 0.042(3) 0.052(3) 0.017(3) 0.003(3) -0.003(3) C39 0.043(3) 0.053(3) 0.061(4) 0.014(3) 0.002(3) 0.004(3) C40 0.055(4) 0.054(3) 0.061(4) 0.024(3) -0.005(3) -0.006(3) C41 0.067(4) 0.080(5) 0.113(6) 0.056(5) 0.010(4) -0.006(3) C42 0.058(4) 0.043(3) 0.082(4) 0.026(3) -0.003(3) 0.003(3) C43 0.042(3) 0.045(3) 0.064(4) 0.013(3) -0.007(3) 0.007(2) _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 1.907(4) . ? Cr1 N6 1.945(4) . ? Cr1 N2 1.984(4) . ? Cr1 N1 1.990(4) . ? N1 C14 1.344(6) . ? N1 C1 1.448(6) . ? N2 C16 1.335(6) . ? N2 C18 1.447(6) . ? N3 N4 1.380(5) . ? N3 C30 1.427(6) . ? N4 N5 1.268(5) . ? N5 N6 1.379(5) . ? N6 C37 1.421(6) . ? C1 C9 1.402(7) . ? C1 C2 1.420(6) . ? C2 C6 1.399(7) . ? C2 C3 1.514(7) . ? C3 C4 1.530(8) . ? C3 C5 1.543(7) . ? C3 H3 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.379(8) . ? C6 H6 0.9300 . ? C7 C8 1.355(8) . ? C7 H7 0.9300 . ? C8 C9 1.396(7) . ? C8 H8 0.9300 . ? C9 C10 1.521(7) . ? C10 C11 1.526(7) . ? C10 C12 1.529(7) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.506(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.389(6) . ? C15 C16 1.392(7) . ? C15 H15 0.9300 . ? C16 C17 1.522(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.415(7) . ? C18 C26 1.425(7) . ? C19 C23 1.392(7) . ? C19 C20 1.509(7) . ? C20 C22 1.529(7) . ? C20 C21 1.541(7) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.365(7) . ? C23 H23 0.9300 . ? C24 C25 1.383(7) . ? C24 H24 0.9300 . ? C25 C26 1.384(7) . ? C25 H25 0.9300 . ? C26 C27 1.512(7) . ? C27 C29 1.522(8) . ? C27 C28 1.540(8) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C36 1.384(7) . ? C30 C31 1.396(6) . ? C31 C32 1.395(7) . ? C31 H31 0.9300 . ? C32 C33 1.384(7) . ? C32 H32 0.9300 . ? C33 C35 1.388(7) . ? C33 C34 1.516(7) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.379(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.384(7) . ? C37 C43 1.389(7) . ? C38 C39 1.381(7) . ? C38 H38 0.9300 . ? C39 C40 1.379(7) . ? C39 H39 0.9300 . ? C40 C42 1.386(8) . ? C40 C41 1.516(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.380(7) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? 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 N6 76.48(16) . . ? N3 Cr1 N2 112.17(16) . . ? N6 Cr1 N2 130.82(17) . . ? N3 Cr1 N1 120.50(16) . . ? N6 Cr1 N1 128.49(16) . . ? N2 Cr1 N1 90.19(16) . . ? C14 N1 C1 118.7(4) . . ? C14 N1 Cr1 124.2(3) . . ? C1 N1 Cr1 116.7(3) . . ? C16 N2 C18 118.7(4) . . ? C16 N2 Cr1 125.2(3) . . ? C18 N2 Cr1 116.0(3) . . ? N4 N3 C30 112.0(3) . . ? N4 N3 Cr1 118.5(3) . . ? C30 N3 Cr1 129.3(3) . . ? N5 N4 N3 114.0(4) . . ? N4 N5 N6 113.7(4) . . ? N5 N6 C37 110.8(4) . . ? N5 N6 Cr1 117.2(3) . . ? C37 N6 Cr1 131.5(3) . . ? C9 C1 C2 121.1(4) . . ? C9 C1 N1 120.8(4) . . ? C2 C1 N1 118.2(4) . . ? C6 C2 C1 117.1(5) . . ? C6 C2 C3 120.3(4) . . ? C1 C2 C3 122.6(4) . . ? C2 C3 C4 112.9(5) . . ? C2 C3 C5 113.1(5) . . ? C4 C3 C5 108.1(4) . . ? C2 C3 H3 107.5 . . ? C4 C3 H3 107.5 . . ? C5 C3 H3 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.4(5) . . ? C7 C6 H6 119.3 . . ? C2 C6 H6 119.3 . . ? C8 C7 C6 120.9(5) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.9(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C1 118.7(5) . . ? C8 C9 C10 118.6(4) . . ? C1 C9 C10 122.8(4) . . ? C9 C10 C11 111.3(4) . . ? C9 C10 C12 111.4(4) . . ? C11 C10 C12 110.6(4) . . ? C9 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C12 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 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 122.3(4) . . ? N1 C14 C13 120.5(4) . . ? C15 C14 C13 117.2(4) . . ? C14 C15 C16 127.6(4) . . ? C14 C15 H15 116.2 . . ? C16 C15 H15 116.2 . . ? N2 C16 C15 122.9(4) . . ? N2 C16 C17 119.1(4) . . ? C15 C16 C17 118.0(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C26 120.6(5) . . ? C19 C18 N2 121.2(4) . . ? C26 C18 N2 118.1(4) . . ? C23 C19 C18 118.2(5) . . ? C23 C19 C20 119.2(5) . . ? C18 C19 C20 122.6(5) . . ? C19 C20 C22 112.4(4) . . ? C19 C20 C21 110.3(4) . . ? C22 C20 C21 109.4(4) . . ? C19 C20 H20 108.2 . . ? C22 C20 H20 108.2 . . ? C21 C20 H20 108.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.2(5) . . ? C24 C23 H23 119.4 . . ? C19 C23 H23 119.4 . . ? C23 C24 C25 120.6(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 121.4(5) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C25 C26 C18 117.8(5) . . ? C25 C26 C27 121.0(5) . . ? C18 C26 C27 121.2(5) . . ? C26 C27 C29 112.7(5) . . ? C26 C27 C28 113.4(5) . . ? C29 C27 C28 110.4(4) . . ? C26 C27 H27 106.6 . . ? C29 C27 H27 106.6 . . ? C28 C27 H27 106.6 . . ? 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 . . ? C36 C30 C31 118.1(4) . . ? C36 C30 N3 119.6(4) . . ? C31 C30 N3 122.3(4) . . ? C32 C31 C30 120.6(5) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 121.1(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C35 117.6(4) . . ? C32 C33 C34 120.0(5) . . ? C35 C33 C34 122.3(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C33 121.8(5) . . ? C36 C35 H35 119.1 . . ? C33 C35 H35 119.1 . . ? C35 C36 C30 120.7(4) . . ? C35 C36 H36 119.6 . . ? C30 C36 H36 119.6 . . ? C38 C37 C43 118.1(5) . . ? C38 C37 N6 122.2(4) . . ? C43 C37 N6 119.7(5) . . ? C39 C38 C37 119.9(5) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 122.6(5) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C39 C40 C42 117.1(5) . . ? C39 C40 C41 121.5(5) . . ? C42 C40 C41 121.4(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 . . ? C43 C42 C40 121.1(5) . . ? C43 C42 H42 119.4 . . ? C40 C42 H42 119.4 . . ? C42 C43 C37 121.1(5) . . ? C42 C43 H43 119.4 . . ? C37 C43 H43 119.4 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.474 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.135 # Attachment 'cpd_8_CCDC_764155.cif' data_a7326 _database_code_depnum_ccdc_archive 'CCDC 764155' #TrackingRef 'cpd_8_CCDC_764155.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H59 Cr N3 Si2' _chemical_formula_sum 'C35 H59 Cr N3 Si2' _chemical_formula_weight 630.03 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' Si Si 0.0817 0.0704 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1132(9) _cell_length_b 20.144(2) _cell_length_c 20.551(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.350(2) _cell_angle_gamma 90.00 _cell_volume 3772.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29834 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6633 _reflns_number_gt 5058 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0871P)^2^+3.4899P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6633 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.006 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 0.1708(3) 0.60478(15) 0.09039(15) 0.0300(7) Uani 1 1 d . . . C2 C 0.3104(3) 0.59448(15) 0.06297(15) 0.0326(7) Uani 1 1 d . . . C3 C 0.3777(3) 0.64532(17) 0.01696(17) 0.0382(8) Uani 1 1 d . . . H3 H 0.3492 0.6894 0.0327 0.046 Uiso 1 1 calc R . . C4 C 0.3177(4) 0.6384(2) -0.05203(18) 0.0560(10) Uani 1 1 d . . . H4A H 0.3622 0.6711 -0.0795 0.084 Uiso 1 1 calc R . . H4B H 0.2133 0.6447 -0.0518 0.084 Uiso 1 1 calc R . . H4C H 0.3397 0.5948 -0.0683 0.084 Uiso 1 1 calc R . . C5 C 0.5457(4) 0.6435(2) 0.0152(2) 0.0534(10) Uani 1 1 d . . . H5A H 0.5806 0.6767 -0.0144 0.080 Uiso 1 1 calc R . . H5B H 0.5776 0.6005 0.0010 0.080 Uiso 1 1 calc R . . H5C H 0.5841 0.6522 0.0580 0.080 Uiso 1 1 calc R . . C6 C 0.3834(4) 0.53540(18) 0.07701(18) 0.0447(9) Uani 1 1 d . . . H6 H 0.4753 0.5276 0.0591 0.054 Uiso 1 1 calc R . . C7 C 0.3219(4) 0.48832(18) 0.11696(19) 0.0506(10) Uani 1 1 d . . . H7 H 0.3728 0.4494 0.1262 0.061 Uiso 1 1 calc R . . C8 C 0.1861(4) 0.49852(17) 0.14320(18) 0.0471(9) Uani 1 1 d . . . H8 H 0.1455 0.4659 0.1696 0.056 Uiso 1 1 calc R . . C9 C 0.1071(4) 0.55667(16) 0.13127(16) 0.0365(8) Uani 1 1 d . . . C10 C -0.0442(4) 0.56392(17) 0.16146(18) 0.0454(9) Uani 1 1 d . . . H10 H -0.0836 0.6076 0.1496 0.055 Uiso 1 1 calc R . . C11 C -0.1520(5) 0.5103(2) 0.1370(2) 0.0675(13) Uani 1 1 d . . . H11A H -0.2461 0.5170 0.1567 0.101 Uiso 1 1 calc R . . H11B H -0.1153 0.4672 0.1484 0.101 Uiso 1 1 calc R . . H11C H -0.1618 0.5135 0.0905 0.101 Uiso 1 1 calc R . . C12 C -0.0389(5) 0.5590(2) 0.2357(2) 0.0654(12) Uani 1 1 d . . . H12A H -0.1361 0.5641 0.2527 0.098 Uiso 1 1 calc R . . H12B H 0.0233 0.5933 0.2528 0.098 Uiso 1 1 calc R . . H12C H -0.0006 0.5164 0.2481 0.098 Uiso 1 1 calc R . . C13 C -0.0628(4) 0.60943(17) -0.00036(18) 0.0435(9) Uani 1 1 d . . . H13A H 0.0102 0.5752 0.0028 0.065 Uiso 1 1 calc R . . H13B H -0.0800 0.6200 -0.0453 0.065 Uiso 1 1 calc R . . H13C H -0.1524 0.5941 0.0189 0.065 Uiso 1 1 calc R . . C14 C -0.0099(3) 0.67061(15) 0.03514(15) 0.0298(7) Uani 1 1 d . . . C15 C -0.0801(3) 0.73005(16) 0.01808(15) 0.0322(7) Uani 1 1 d . . . H15 H -0.1686 0.7258 -0.0043 0.039 Uiso 1 1 calc R . . C16 C -0.0337(3) 0.79471(15) 0.03052(15) 0.0301(7) Uani 1 1 d . . . C17 C -0.1234(4) 0.85000(17) 0.00025(18) 0.0414(8) Uani 1 1 d . . . H17A H -0.0592 0.8850 -0.0137 0.062 Uiso 1 1 calc R . . H17B H -0.1910 0.8670 0.0318 0.062 Uiso 1 1 calc R . . H17C H -0.1770 0.8331 -0.0365 0.062 Uiso 1 1 calc R . . C18 C 0.1455(3) 0.87522(15) 0.06308(16) 0.0343(7) Uani 1 1 d . . . C19 C 0.2507(3) 0.88788(17) 0.01438(18) 0.0403(8) Uani 1 1 d . . . C20 C 0.2944(4) 0.83554(19) -0.03513(18) 0.0467(9) Uani 1 1 d . . . H20 H 0.2778 0.7922 -0.0149 0.056 Uiso 1 1 calc R . . C21 C 0.2003(5) 0.8380(3) -0.0966(2) 0.0770(14) Uani 1 1 d . . . H21A H 0.0985 0.8359 -0.0850 0.116 Uiso 1 1 calc R . . H21B H 0.2241 0.8010 -0.1240 0.116 Uiso 1 1 calc R . . H21C H 0.2189 0.8786 -0.1195 0.116 Uiso 1 1 calc R . . C22 C 0.4555(4) 0.8382(3) -0.0544(2) 0.0700(13) Uani 1 1 d . . . H22A H 0.4753 0.8038 -0.0855 0.105 Uiso 1 1 calc R . . H22B H 0.5159 0.8317 -0.0164 0.105 Uiso 1 1 calc R . . H22C H 0.4767 0.8806 -0.0733 0.105 Uiso 1 1 calc R . . C23 C 0.3127(4) 0.95099(19) 0.0123(2) 0.0574(11) Uani 1 1 d . . . H23 H 0.3820 0.9608 -0.0194 0.069 Uiso 1 1 calc R . . C24 C 0.2732(5) 0.9987(2) 0.0561(3) 0.0662(13) Uani 1 1 d . . . H24 H 0.3160 1.0405 0.0539 0.079 Uiso 1 1 calc R . . C25 C 0.1722(5) 0.98602(19) 0.1030(2) 0.0602(11) Uani 1 1 d . . . H25 H 0.1479 1.0193 0.1324 0.072 Uiso 1 1 calc R . . C26 C 0.1040(4) 0.92369(17) 0.10790(18) 0.0445(9) Uani 1 1 d . . . C27 C -0.0101(5) 0.91263(19) 0.15944(19) 0.0560(11) Uani 1 1 d . . . H27 H -0.0463 0.8671 0.1547 0.067 Uiso 1 1 calc R . . C28 C -0.1428(6) 0.9596(2) 0.1523(3) 0.0809(15) Uani 1 1 d . . . H28A H -0.2127 0.9502 0.1858 0.121 Uiso 1 1 calc R . . H28B H -0.1881 0.9530 0.1104 0.121 Uiso 1 1 calc R . . H28C H -0.1105 1.0048 0.1561 0.121 Uiso 1 1 calc R . . C29 C 0.0563(7) 0.9189(2) 0.2271(2) 0.0889(17) Uani 1 1 d . . . H29A H -0.0181 0.9110 0.2590 0.133 Uiso 1 1 calc R . . H29B H 0.0956 0.9628 0.2327 0.133 Uiso 1 1 calc R . . H29C H 0.1335 0.8868 0.2323 0.133 Uiso 1 1 calc R . . C30 C 0.2485(5) 0.7939(2) 0.34298(19) 0.0664(12) Uani 1 1 d . . . H30A H 0.2209 0.8376 0.3290 0.100 Uiso 1 1 calc R . . H30B H 0.3500 0.7938 0.3558 0.100 Uiso 1 1 calc R . . H30C H 0.1891 0.7810 0.3793 0.100 Uiso 1 1 calc R . . C31 C 0.2768(5) 0.6510(2) 0.3068(2) 0.0604(11) Uani 1 1 d . . . H31A H 0.2647 0.6182 0.2733 0.091 Uiso 1 1 calc R . . H31B H 0.2168 0.6396 0.3434 0.091 Uiso 1 1 calc R . . H31C H 0.3778 0.6526 0.3202 0.091 Uiso 1 1 calc R . . C32 C 0.0186(4) 0.73430(19) 0.2572(2) 0.0493(9) Uani 1 1 d . . . H32A H -0.0024 0.7041 0.2222 0.074 Uiso 1 1 calc R . . H32B H -0.0118 0.7782 0.2450 0.074 Uiso 1 1 calc R . . H32C H -0.0337 0.7207 0.2954 0.074 Uiso 1 1 calc R . . C33 C 0.5968(5) 0.6814(3) 0.2052(2) 0.0772(14) Uani 1 1 d . . . H33A H 0.5740 0.6609 0.2461 0.116 Uiso 1 1 calc R . . H33B H 0.7007 0.6886 0.2026 0.116 Uiso 1 1 calc R . . H33C H 0.5658 0.6529 0.1703 0.116 Uiso 1 1 calc R . . C34 C 0.5442(5) 0.8018(2) 0.1194(2) 0.0668(12) Uani 1 1 d . . . H34A H 0.4940 0.8435 0.1155 0.100 Uiso 1 1 calc R . . H34B H 0.5139 0.7730 0.0846 0.100 Uiso 1 1 calc R . . H34C H 0.6482 0.8090 0.1170 0.100 Uiso 1 1 calc R . . C35 C 0.5776(5) 0.8178(3) 0.2634(3) 0.0876(17) Uani 1 1 d . . . H35A H 0.5562 0.7996 0.3054 0.131 Uiso 1 1 calc R . . H35B H 0.5350 0.8613 0.2599 0.131 Uiso 1 1 calc R . . H35C H 0.6820 0.8209 0.2581 0.131 Uiso 1 1 calc R . . N1 N 0.0996(3) 0.66742(12) 0.07825(12) 0.0266(5) Uani 1 1 d . . . N2 N 0.0845(3) 0.80906(12) 0.06670(12) 0.0283(6) Uani 1 1 d . . . N3 N 0.3121(3) 0.75336(13) 0.20431(13) 0.0346(6) Uani 1 1 d . . . Si1 Si 0.22029(11) 0.73409(5) 0.27474(5) 0.0396(3) Uani 1 1 d . . . Si2 Si 0.49890(11) 0.76286(6) 0.19878(5) 0.0468(3) Uani 1 1 d . . . Cr1 Cr 0.18720(5) 0.74561(2) 0.12651(2) 0.02734(17) 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 0.0351(16) 0.0227(15) 0.0320(17) -0.0047(13) -0.0066(13) -0.0020(13) C2 0.0337(16) 0.0282(17) 0.0360(18) -0.0062(14) -0.0062(14) 0.0008(13) C3 0.0326(17) 0.0356(19) 0.046(2) -0.0086(15) 0.0043(15) -0.0016(14) C4 0.052(2) 0.068(3) 0.048(2) 0.008(2) 0.0034(18) -0.013(2) C5 0.0367(19) 0.062(3) 0.062(3) -0.013(2) 0.0067(18) -0.0050(18) C6 0.0424(19) 0.040(2) 0.051(2) -0.0072(17) -0.0015(17) 0.0142(16) C7 0.063(2) 0.033(2) 0.056(2) 0.0031(17) -0.006(2) 0.0154(17) C8 0.067(2) 0.0262(18) 0.048(2) 0.0044(16) 0.0015(18) 0.0020(17) C9 0.0449(18) 0.0253(17) 0.0392(19) -0.0040(14) -0.0034(15) -0.0022(14) C10 0.050(2) 0.0308(19) 0.055(2) 0.0012(16) 0.0104(18) -0.0022(16) C11 0.057(2) 0.052(3) 0.094(4) -0.001(2) 0.007(2) -0.018(2) C12 0.072(3) 0.057(3) 0.067(3) 0.002(2) 0.020(2) -0.005(2) C13 0.0422(18) 0.0364(19) 0.052(2) -0.0094(17) -0.0120(16) -0.0066(15) C14 0.0281(15) 0.0300(17) 0.0314(17) -0.0044(13) -0.0013(13) -0.0070(13) C15 0.0262(15) 0.0367(18) 0.0335(18) -0.0007(14) -0.0095(13) -0.0035(13) C16 0.0282(15) 0.0310(17) 0.0311(17) 0.0036(13) -0.0049(13) 0.0009(13) C17 0.0397(18) 0.039(2) 0.045(2) 0.0049(16) -0.0151(16) 0.0044(15) C18 0.0373(17) 0.0230(16) 0.0422(19) 0.0024(14) -0.0171(14) -0.0004(13) C19 0.0341(17) 0.0350(19) 0.051(2) 0.0114(16) -0.0097(15) -0.0057(14) C20 0.0416(19) 0.046(2) 0.053(2) 0.0104(18) 0.0067(17) -0.0073(16) C21 0.064(3) 0.106(4) 0.061(3) -0.015(3) -0.009(2) 0.007(3) C22 0.052(2) 0.095(4) 0.063(3) 0.001(3) 0.011(2) 0.002(2) C23 0.048(2) 0.041(2) 0.083(3) 0.019(2) -0.006(2) -0.0101(18) C24 0.065(3) 0.029(2) 0.105(4) 0.007(2) -0.022(3) -0.0109(19) C25 0.073(3) 0.029(2) 0.078(3) -0.006(2) -0.019(2) 0.0022(19) C26 0.055(2) 0.0295(19) 0.049(2) -0.0003(16) -0.0179(18) 0.0028(16) C27 0.089(3) 0.033(2) 0.047(2) -0.0084(17) -0.003(2) 0.0082(19) C28 0.100(4) 0.067(3) 0.076(3) -0.001(3) 0.013(3) 0.028(3) C29 0.153(5) 0.059(3) 0.055(3) -0.009(2) -0.018(3) 0.012(3) C30 0.084(3) 0.077(3) 0.038(2) -0.011(2) 0.001(2) -0.008(3) C31 0.064(3) 0.056(3) 0.061(3) 0.020(2) -0.007(2) 0.000(2) C32 0.044(2) 0.046(2) 0.058(3) 0.0041(18) 0.0057(18) -0.0009(17) C33 0.057(3) 0.102(4) 0.073(3) 0.001(3) -0.009(2) 0.028(3) C34 0.055(2) 0.080(3) 0.065(3) 0.000(2) 0.006(2) -0.014(2) C35 0.058(3) 0.123(5) 0.082(4) -0.038(3) -0.009(2) -0.027(3) N1 0.0260(12) 0.0220(13) 0.0319(14) -0.0011(11) -0.0030(11) -0.0019(10) N2 0.0314(13) 0.0211(13) 0.0322(14) 0.0011(11) -0.0067(11) -0.0010(10) N3 0.0360(14) 0.0332(15) 0.0344(15) -0.0010(12) -0.0072(12) -0.0004(11) Si1 0.0461(5) 0.0416(6) 0.0310(5) 0.0022(4) -0.0053(4) 0.0008(4) Si2 0.0342(5) 0.0616(7) 0.0445(6) -0.0078(5) -0.0099(4) -0.0020(4) Cr1 0.0305(3) 0.0236(3) 0.0278(3) -0.0009(2) -0.0088(2) -0.0002(2) _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 1.410(4) . ? C1 C9 1.410(4) . ? C1 N1 1.440(4) . ? C2 C6 1.393(5) . ? C2 C3 1.525(5) . ? C3 C4 1.523(5) . ? C3 C5 1.532(4) . ? C3 H3 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.376(5) . ? C6 H6 0.9300 . ? C7 C8 1.368(5) . ? C7 H7 0.9300 . ? C8 C9 1.396(5) . ? C8 H8 0.9300 . ? C9 C10 1.523(5) . ? C10 C12 1.529(6) . ? C10 C11 1.542(5) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.510(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N1 1.332(4) . ? C14 C15 1.401(4) . ? C15 C16 1.392(4) . ? C15 H15 0.9300 . ? C16 N2 1.336(4) . ? C16 C17 1.513(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C26 1.396(5) . ? C18 C19 1.413(5) . ? C18 N2 1.446(4) . ? C19 C23 1.392(5) . ? C19 C20 1.520(5) . ? C20 C22 1.523(5) . ? C20 C21 1.523(6) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.367(6) . ? C23 H23 0.9300 . ? C24 C25 1.360(6) . ? C24 H24 0.9300 . ? C25 C26 1.405(5) . ? C25 H25 0.9300 . ? C26 C27 1.505(6) . ? C27 C29 1.518(6) . ? C27 C28 1.542(6) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 Si1 1.866(4) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 Si1 1.869(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 Si1 1.871(4) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 Si2 1.873(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 Si2 1.859(4) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 Si2 1.869(4) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? N1 Cr1 2.023(2) . ? N2 Cr1 2.002(2) . ? N3 Si2 1.718(3) . ? N3 Si1 1.720(3) . ? N3 Cr1 1.963(3) . ? 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 C9 120.8(3) . . ? C2 C1 N1 117.8(3) . . ? C9 C1 N1 121.3(3) . . ? C6 C2 C1 118.3(3) . . ? C6 C2 C3 120.6(3) . . ? C1 C2 C3 121.1(3) . . ? C4 C3 C2 111.8(3) . . ? C4 C3 C5 109.2(3) . . ? C2 C3 C5 113.8(3) . . ? C4 C3 H3 107.2 . . ? C2 C3 H3 107.2 . . ? C5 C3 H3 107.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.1(3) . . ? C7 C6 H6 119.4 . . ? C2 C6 H6 119.4 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.6(3) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C1 117.9(3) . . ? C8 C9 C10 118.5(3) . . ? C1 C9 C10 123.6(3) . . ? C9 C10 C12 112.1(3) . . ? C9 C10 C11 112.1(3) . . ? C12 C10 C11 107.3(3) . . ? C9 C10 H10 108.4 . . ? C12 C10 H10 108.4 . . ? C11 C10 H10 108.4 . . ? 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 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 123.1(3) . . ? N1 C14 C13 121.2(3) . . ? C15 C14 C13 115.6(3) . . ? C16 C15 C14 128.0(3) . . ? C16 C15 H15 116.0 . . ? C14 C15 H15 116.0 . . ? N2 C16 C15 123.2(3) . . ? N2 C16 C17 120.1(3) . . ? C15 C16 C17 116.8(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C18 C19 121.9(3) . . ? C26 C18 N2 120.3(3) . . ? C19 C18 N2 117.7(3) . . ? C23 C19 C18 117.7(4) . . ? C23 C19 C20 120.3(3) . . ? C18 C19 C20 122.1(3) . . ? C22 C20 C21 108.8(3) . . ? C22 C20 C19 114.0(3) . . ? C21 C20 C19 112.6(3) . . ? C22 C20 H20 107.0 . . ? C21 C20 H20 107.0 . . ? C19 C20 H20 107.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 120.8(4) . . ? C24 C23 H23 119.6 . . ? C19 C23 H23 119.6 . . ? C25 C24 C23 121.1(4) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 121.3(4) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C18 C26 C25 117.1(4) . . ? C18 C26 C27 123.5(3) . . ? C25 C26 C27 119.4(4) . . ? C26 C27 C29 111.0(4) . . ? C26 C27 C28 112.8(3) . . ? C29 C27 C28 110.2(4) . . ? C26 C27 H27 107.6 . . ? C29 C27 H27 107.6 . . ? C28 C27 H27 107.6 . . ? 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 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C14 N1 C1 119.5(2) . . ? C14 N1 Cr1 125.5(2) . . ? C1 N1 Cr1 114.91(18) . . ? C16 N2 C18 118.7(2) . . ? C16 N2 Cr1 125.1(2) . . ? C18 N2 Cr1 116.20(18) . . ? Si2 N3 Si1 124.60(16) . . ? Si2 N3 Cr1 121.66(16) . . ? Si1 N3 Cr1 112.64(14) . . ? N3 Si1 C30 114.92(18) . . ? N3 Si1 C31 111.36(17) . . ? C30 Si1 C31 106.1(2) . . ? N3 Si1 C32 108.63(16) . . ? C30 Si1 C32 105.9(2) . . ? C31 Si1 C32 109.75(18) . . ? N3 Si2 C34 109.30(17) . . ? N3 Si2 C35 113.28(18) . . ? C34 Si2 C35 106.7(2) . . ? N3 Si2 C33 111.69(19) . . ? C34 Si2 C33 108.9(2) . . ? C35 Si2 C33 106.8(3) . . ? N3 Cr1 N2 135.73(10) . . ? N3 Cr1 N1 133.34(10) . . ? N2 Cr1 N1 90.82(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.011 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.129 # Attachment 'cpd_7_CCDC_764811.cif' data_6852 _database_code_depnum_ccdc_archive 'CCDC 764811' #TrackingRef 'cpd_7_CCDC_764811.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H152 N8 O V2' _chemical_formula_sum 'C102 H152 N8 O V2' _chemical_formula_weight 1608.20 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 19.7038(4) _cell_length_b 10.9155(3) _cell_length_c 23.6118(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.1980(10) _cell_angle_gamma 90.00 _cell_volume 4923.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 34453 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.8786 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35759 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.1287 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.37 _reflns_number_total 8944 _reflns_number_gt 4875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1337P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0169(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8944 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1711 _refine_ls_R_factor_gt 0.0975 _refine_ls_wR_factor_ref 0.2565 _refine_ls_wR_factor_gt 0.2259 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.033 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 0.1449(2) 0.1004(4) 0.98447(18) 0.0379(11) Uani 1 1 d . . . C2 C 0.0882(2) 0.1811(5) 0.9696(2) 0.0446(12) Uani 1 1 d . . . C3 C 0.0763(2) 0.2839(5) 1.0083(2) 0.0597(15) Uani 1 1 d . . . H3 H 0.1137 0.2783 1.0455 0.072 Uiso 1 1 calc R . . C4 C 0.0844(3) 0.4082(6) 0.9807(3) 0.085(2) Uani 1 1 d . . . H4A H 0.0762 0.4739 1.0065 0.127 Uiso 1 1 calc R . . H4B H 0.0502 0.4147 0.9429 0.127 Uiso 1 1 calc R . . H4C H 0.1318 0.4155 0.9750 0.127 Uiso 1 1 calc R . . C5 C 0.0051(3) 0.2756(6) 1.0246(3) 0.0785(19) Uani 1 1 d . . . H5A H 0.0004 0.3448 1.0499 0.118 Uiso 1 1 calc R . . H5B H 0.0028 0.1986 1.0454 0.118 Uiso 1 1 calc R . . H5C H -0.0329 0.2781 0.9890 0.118 Uiso 1 1 calc R . . C6 C 0.0423(2) 0.1674(6) 0.9144(2) 0.0584(15) Uani 1 1 d . . . H6 H 0.0037 0.2219 0.9033 0.070 Uiso 1 1 calc R . . C7 C 0.0509(3) 0.0785(6) 0.8760(2) 0.0615(15) Uani 1 1 d . . . H7 H 0.0178 0.0696 0.8395 0.074 Uiso 1 1 calc R . . C8 C 0.1077(3) 0.0025(6) 0.8908(2) 0.0601(15) Uani 1 1 d . . . H8 H 0.1142 -0.0578 0.8636 0.072 Uiso 1 1 calc R . . C9 C 0.1562(2) 0.0111(5) 0.94468(19) 0.0464(13) Uani 1 1 d . . . C10 C 0.2205(3) -0.0699(5) 0.9580(2) 0.0524(14) Uani 1 1 d . . . H10 H 0.2579 -0.0273 0.9878 0.063 Uiso 1 1 calc R . . C11 C 0.2048(4) -0.1913(7) 0.9840(3) 0.091(2) Uani 1 1 d . . . H11A H 0.2471 -0.2422 0.9928 0.136 Uiso 1 1 calc R . . H11B H 0.1674 -0.2339 0.9559 0.136 Uiso 1 1 calc R . . H11C H 0.1898 -0.1759 1.0200 0.136 Uiso 1 1 calc R . . C12 C 0.2477(3) -0.0915(6) 0.9041(2) 0.0768(18) Uani 1 1 d . . . H12A H 0.2895 -0.1434 0.9143 0.115 Uiso 1 1 calc R . . H12B H 0.2596 -0.0128 0.8891 0.115 Uiso 1 1 calc R . . H12C H 0.2115 -0.1322 0.8741 0.115 Uiso 1 1 calc R . . C13 C 0.1125(2) -0.0153(5) 1.0824(2) 0.0502(13) Uani 1 1 d . . . H13A H 0.0961 -0.0540 1.0440 0.075 Uiso 1 1 calc R . . H13B H 0.0786 0.0467 1.0876 0.075 Uiso 1 1 calc R . . H13C H 0.1175 -0.0776 1.1130 0.075 Uiso 1 1 calc R . . C14 C 0.1829(2) 0.0453(4) 1.08626(19) 0.0372(11) Uani 1 1 d . . . C15 C 0.2340(2) 0.0307(4) 1.13940(19) 0.0395(11) Uani 1 1 d . . . H15 H 0.2163 0.0040 1.1713 0.047 Uiso 1 1 calc R . . C16 C 0.3070(2) 0.0492(4) 1.15297(17) 0.0367(11) Uani 1 1 d . . . C17 C 0.3487(2) -0.0080(5) 1.2082(2) 0.0518(13) Uani 1 1 d . . . H17A H 0.3930 0.0361 1.2217 0.078 Uiso 1 1 calc R . . H17B H 0.3582 -0.0939 1.2009 0.078 Uiso 1 1 calc R . . H17C H 0.3221 -0.0036 1.2382 0.078 Uiso 1 1 calc R . . C18 C 0.4141(2) 0.1044(5) 1.12785(18) 0.0385(11) Uani 1 1 d . . . C19 C 0.4424(2) 0.0047(5) 1.10354(19) 0.0419(12) Uani 1 1 d . . . C20 C 0.3978(2) -0.0952(5) 1.0682(2) 0.0534(14) Uani 1 1 d . . . H20 H 0.3476 -0.0705 1.0616 0.064 Uiso 1 1 calc R . . C21 C 0.4142(3) -0.1080(7) 1.0096(3) 0.0831(19) Uani 1 1 d . . . H21A H 0.3847 -0.1724 0.9872 0.125 Uiso 1 1 calc R . . H21B H 0.4636 -0.1298 1.0151 0.125 Uiso 1 1 calc R . . H21C H 0.4048 -0.0302 0.9885 0.125 Uiso 1 1 calc R . . C22 C 0.4072(3) -0.2202(6) 1.1001(3) 0.0787(18) Uani 1 1 d . . . H22A H 0.3771 -0.2815 1.0758 0.118 Uiso 1 1 calc R . . H22B H 0.3942 -0.2123 1.1374 0.118 Uiso 1 1 calc R . . H22C H 0.4562 -0.2461 1.1073 0.118 Uiso 1 1 calc R . . C23 C 0.5147(2) -0.0014(5) 1.1121(2) 0.0514(13) Uani 1 1 d . . . H23 H 0.5347 -0.0689 1.0966 0.062 Uiso 1 1 calc R . . C24 C 0.5579(2) 0.0879(6) 1.1426(2) 0.0548(14) Uani 1 1 d . . . H24 H 0.6072 0.0819 1.1480 0.066 Uiso 1 1 calc R . . C25 C 0.5295(2) 0.1853(5) 1.1650(2) 0.0485(13) Uani 1 1 d . . . H25 H 0.5597 0.2472 1.1854 0.058 Uiso 1 1 calc R . . C26 C 0.4574(2) 0.1965(5) 1.15868(19) 0.0411(12) Uani 1 1 d . . . C27 C 0.4298(2) 0.3055(5) 1.1857(2) 0.0493(13) Uani 1 1 d . . . H27 H 0.3776 0.2979 1.1768 0.059 Uiso 1 1 calc R . . C28 C 0.4579(3) 0.3044(6) 1.2529(2) 0.0720(17) Uani 1 1 d . . . H28A H 0.4391 0.3749 1.2697 0.108 Uiso 1 1 calc R . . H28B H 0.5091 0.3089 1.2628 0.108 Uiso 1 1 calc R . . H28C H 0.4433 0.2285 1.2687 0.108 Uiso 1 1 calc R . . C29 C 0.4467(3) 0.4262(6) 1.1612(3) 0.0677(16) Uani 1 1 d . . . H29A H 0.4269 0.4933 1.1796 0.101 Uiso 1 1 calc R . . H29B H 0.4266 0.4277 1.1189 0.101 Uiso 1 1 calc R . . H29C H 0.4976 0.4359 1.1691 0.101 Uiso 1 1 calc R . . C30 C 0.3219(2) 0.3529(5) 0.96840(19) 0.0439(12) Uani 1 1 d . . . C31 C 0.3082(3) 0.4873(5) 0.9767(2) 0.0631(15) Uani 1 1 d . . . H31A H 0.3338 0.5134 1.0163 0.076 Uiso 1 1 calc R . . H31B H 0.2576 0.5004 0.9729 0.076 Uiso 1 1 calc R . . C32 C 0.3323(3) 0.5651(6) 0.9305(3) 0.0729(18) Uani 1 1 d . . . H32 H 0.3228 0.6535 0.9366 0.087 Uiso 1 1 calc R . . C33 C 0.4083(4) 0.5478(7) 0.9371(3) 0.088(2) Uani 1 1 d . . . H33A H 0.4342 0.5754 0.9764 0.106 Uiso 1 1 calc R . . H33B H 0.4238 0.5983 0.9077 0.106 Uiso 1 1 calc R . . C34 C 0.4247(3) 0.4156(7) 0.9291(3) 0.0779(19) Uani 1 1 d . . . H34 H 0.4762 0.4056 0.9339 0.094 Uiso 1 1 calc R . . C35 C 0.4013(3) 0.3383(6) 0.9746(3) 0.0687(17) Uani 1 1 d . . . H35A H 0.4271 0.3642 1.0143 0.082 Uiso 1 1 calc R . . H35B H 0.4123 0.2511 0.9696 0.082 Uiso 1 1 calc R . . C36 C 0.2843(3) 0.3113(6) 0.9072(2) 0.0767(18) Uani 1 1 d . . . H36A H 0.2331 0.3208 0.9019 0.092 Uiso 1 1 calc R . . H36B H 0.2942 0.2236 0.9024 0.092 Uiso 1 1 calc R . . C37 C 0.3084(4) 0.3874(8) 0.8607(3) 0.097(2) Uani 1 1 d . . . H37 H 0.2839 0.3597 0.8205 0.117 Uiso 1 1 calc R . . C38 C 0.3873(4) 0.3742(7) 0.8705(3) 0.085(2) Uani 1 1 d . . . H38A H 0.3989 0.2872 0.8656 0.102 Uiso 1 1 calc R . . H38B H 0.4032 0.4228 0.8408 0.102 Uiso 1 1 calc R . . C39 C 0.2905(4) 0.5260(7) 0.8704(3) 0.095(2) Uani 1 1 d . . . H39A H 0.3029 0.5781 0.8401 0.114 Uiso 1 1 calc R . . H39B H 0.2398 0.5351 0.8675 0.114 Uiso 1 1 calc R . . C40 C 0.2298(2) 0.4401(5) 1.14368(19) 0.0419(12) Uani 1 1 d . . . C41 C 0.2692(3) 0.4306(5) 1.2087(2) 0.0561(14) Uani 1 1 d . . . H41A H 0.2566 0.3528 1.2251 0.067 Uiso 1 1 calc R . . H41B H 0.3203 0.4298 1.2120 0.067 Uiso 1 1 calc R . . C42 C 0.2511(3) 0.5375(6) 1.2436(2) 0.0619(16) Uani 1 1 d . . . H42 H 0.2776 0.5297 1.2854 0.074 Uiso 1 1 calc R . . C43 C 0.2718(3) 0.6573(6) 1.2181(3) 0.0717(17) Uani 1 1 d . . . H43A H 0.2604 0.7281 1.2403 0.086 Uiso 1 1 calc R . . H43B H 0.3228 0.6580 1.2212 0.086 Uiso 1 1 calc R . . C44 C 0.2322(3) 0.6672(5) 1.1547(2) 0.0660(16) Uani 1 1 d . . . H44 H 0.2456 0.7455 1.1382 0.079 Uiso 1 1 calc R . . C45 C 0.2499(3) 0.5601(5) 1.1193(2) 0.0536(13) Uani 1 1 d . . . H45A H 0.2240 0.5688 1.0779 0.064 Uiso 1 1 calc R . . H45B H 0.3006 0.5603 1.1211 0.064 Uiso 1 1 calc R . . C46 C 0.1541(3) 0.6686(6) 1.1504(3) 0.0746(18) Uani 1 1 d . . . H46A H 0.1281 0.6763 1.1090 0.090 Uiso 1 1 calc R . . H46B H 0.1423 0.7399 1.1721 0.090 Uiso 1 1 calc R . . C47 C 0.1330(3) 0.5511(6) 1.1760(2) 0.0652(16) Uani 1 1 d . . . H47 H 0.0816 0.5519 1.1733 0.078 Uiso 1 1 calc R . . C48 C 0.1737(3) 0.5403(6) 1.2399(2) 0.0690(17) Uani 1 1 d . . . H48A H 0.1626 0.6109 1.2624 0.083 Uiso 1 1 calc R . . H48B H 0.1598 0.4644 1.2571 0.083 Uiso 1 1 calc R . . C49 C 0.1514(3) 0.4417(6) 1.1409(2) 0.0622(15) Uani 1 1 d . . . H49A H 0.1380 0.3642 1.1570 0.075 Uiso 1 1 calc R . . H49B H 0.1245 0.4481 1.0996 0.075 Uiso 1 1 calc R . . N1 N 0.19402(16) 0.1087(3) 1.04128(15) 0.0338(9) Uani 1 1 d . . . N2 N 0.33919(16) 0.1126(3) 1.11896(14) 0.0334(9) Uani 1 1 d . . . N3 N 0.30067(18) 0.2783(4) 1.01175(16) 0.0436(10) Uani 1 1 d . . . N4 N 0.24608(18) 0.3350(4) 1.11160(15) 0.0423(10) Uani 1 1 d . . . V1 V 0.27171(3) 0.22949(7) 1.06837(3) 0.0359(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(2) 0.037(3) 0.042(3) -0.003(2) 0.0053(18) -0.005(2) C2 0.036(2) 0.039(3) 0.056(3) -0.004(3) 0.006(2) 0.001(2) C3 0.039(3) 0.059(4) 0.072(4) -0.011(3) -0.003(2) 0.011(3) C4 0.086(4) 0.047(4) 0.108(5) -0.006(4) -0.003(4) 0.012(3) C5 0.055(3) 0.092(5) 0.086(4) -0.015(4) 0.011(3) 0.020(3) C6 0.037(3) 0.065(4) 0.065(3) -0.003(3) -0.004(2) 0.008(3) C7 0.047(3) 0.072(4) 0.055(3) -0.003(3) -0.006(2) 0.001(3) C8 0.057(3) 0.067(4) 0.053(3) -0.020(3) 0.007(2) 0.005(3) C9 0.041(3) 0.051(3) 0.043(3) -0.002(3) 0.004(2) 0.000(2) C10 0.058(3) 0.052(4) 0.045(3) -0.009(3) 0.010(2) 0.018(3) C11 0.107(5) 0.091(6) 0.089(5) 0.031(4) 0.052(4) 0.051(4) C12 0.074(4) 0.086(5) 0.071(4) -0.001(4) 0.019(3) 0.022(4) C13 0.039(3) 0.048(3) 0.064(3) 0.003(3) 0.013(2) -0.007(2) C14 0.041(2) 0.028(3) 0.046(3) -0.007(2) 0.016(2) 0.000(2) C15 0.039(2) 0.042(3) 0.040(3) -0.003(2) 0.0142(19) -0.003(2) C16 0.045(3) 0.031(3) 0.033(2) -0.004(2) 0.0076(19) -0.002(2) C17 0.047(3) 0.060(4) 0.048(3) 0.011(3) 0.010(2) -0.002(3) C18 0.032(2) 0.045(3) 0.039(2) 0.002(2) 0.0098(18) -0.001(2) C19 0.037(2) 0.044(3) 0.044(3) 0.006(2) 0.0082(19) 0.004(2) C20 0.043(3) 0.051(4) 0.065(3) -0.013(3) 0.011(2) 0.011(2) C21 0.089(4) 0.090(5) 0.069(4) -0.023(4) 0.016(3) -0.006(4) C22 0.080(4) 0.054(4) 0.103(5) -0.010(4) 0.023(3) -0.006(3) C23 0.042(3) 0.057(4) 0.056(3) 0.002(3) 0.014(2) 0.013(3) C24 0.034(3) 0.074(4) 0.056(3) 0.007(3) 0.012(2) 0.003(3) C25 0.034(2) 0.062(4) 0.047(3) 0.003(3) 0.006(2) -0.009(2) C26 0.038(2) 0.045(3) 0.040(3) 0.009(2) 0.0080(19) -0.002(2) C27 0.037(2) 0.060(4) 0.052(3) -0.014(3) 0.011(2) -0.009(2) C28 0.084(4) 0.078(5) 0.054(3) -0.016(3) 0.016(3) -0.013(3) C29 0.071(4) 0.054(4) 0.082(4) -0.001(3) 0.028(3) -0.007(3) C30 0.054(3) 0.039(3) 0.042(3) 0.006(2) 0.017(2) 0.010(2) C31 0.085(4) 0.043(4) 0.071(4) 0.005(3) 0.039(3) 0.010(3) C32 0.098(5) 0.047(4) 0.088(5) 0.019(3) 0.051(4) 0.015(3) C33 0.106(5) 0.081(6) 0.095(5) 0.021(4) 0.059(4) 0.000(4) C34 0.087(4) 0.079(5) 0.083(5) 0.004(4) 0.050(4) -0.001(4) C35 0.064(3) 0.074(5) 0.076(4) 0.021(3) 0.033(3) 0.014(3) C36 0.099(5) 0.066(4) 0.060(4) 0.003(3) 0.009(3) -0.013(4) C37 0.138(7) 0.104(7) 0.047(4) 0.017(4) 0.018(4) -0.021(5) C38 0.115(6) 0.076(5) 0.082(5) 0.006(4) 0.059(4) 0.022(4) C39 0.118(6) 0.085(6) 0.091(5) 0.054(5) 0.043(4) 0.035(4) C40 0.046(3) 0.038(3) 0.043(3) -0.007(2) 0.014(2) 0.000(2) C41 0.064(3) 0.055(4) 0.051(3) 0.001(3) 0.018(2) 0.012(3) C42 0.062(3) 0.081(5) 0.042(3) -0.011(3) 0.012(2) 0.012(3) C43 0.076(4) 0.067(5) 0.078(4) -0.029(4) 0.028(3) -0.006(3) C44 0.096(5) 0.040(4) 0.069(4) -0.002(3) 0.033(3) 0.000(3) C45 0.074(3) 0.043(3) 0.048(3) -0.001(3) 0.022(2) 0.003(3) C46 0.098(5) 0.050(4) 0.070(4) -0.015(3) 0.011(3) 0.027(4) C47 0.050(3) 0.076(5) 0.071(4) -0.022(3) 0.017(3) 0.011(3) C48 0.086(4) 0.070(4) 0.061(4) -0.012(3) 0.036(3) 0.002(3) C49 0.054(3) 0.058(4) 0.076(4) -0.022(3) 0.018(3) -0.002(3) N1 0.0334(19) 0.030(2) 0.038(2) -0.0002(18) 0.0096(15) -0.0007(16) N2 0.0337(19) 0.030(2) 0.036(2) 0.0022(18) 0.0088(15) 0.0000(16) N3 0.043(2) 0.039(2) 0.047(2) 0.003(2) 0.0074(17) 0.0014(18) N4 0.043(2) 0.032(2) 0.049(2) 0.002(2) 0.0052(16) 0.0000(18) V1 0.0338(4) 0.0316(5) 0.0413(5) 0.0005(4) 0.0071(3) -0.0008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.398(6) . ? C1 C9 1.409(6) . ? C1 N1 1.452(5) . ? C2 C6 1.400(7) . ? C2 C3 1.503(7) . ? C3 C4 1.530(8) . ? C3 C5 1.544(7) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.367(7) . ? C6 H6 0.9500 . ? C7 C8 1.368(7) . ? C7 H7 0.9500 . ? C8 C9 1.395(6) . ? C8 H8 0.9500 . ? C9 C10 1.512(6) . ? C10 C12 1.516(7) . ? C10 C11 1.523(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 . ? C13 C14 1.518(6) . ? C13 H13A 0.9801 . ? C13 H13B 0.9801 . ? C13 H13C 0.9801 . ? C14 N1 1.330(5) . ? C14 C15 1.412(6) . ? C15 C16 1.409(6) . ? C15 H15 0.9500 . ? C16 N2 1.333(5) . ? C16 C17 1.496(6) . ? C17 H17A 0.9801 . ? C17 H17B 0.9801 . ? C17 H17C 0.9801 . ? C18 C26 1.402(6) . ? C18 C19 1.407(6) . ? C18 N2 1.441(5) . ? C19 C23 1.390(6) . ? C19 C20 1.516(7) . ? C20 C21 1.501(7) . ? C20 C22 1.548(8) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.375(7) . ? C23 H23 0.9500 . ? C24 C25 1.367(7) . ? C24 H24 0.9500 . ? C25 C26 1.396(6) . ? C25 H25 0.9500 . ? C26 C27 1.514(7) . ? C27 C29 1.508(8) . ? C27 C28 1.547(7) . ? 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 N3 1.448(6) . ? C30 C31 1.513(7) . ? C30 C36 1.522(7) . ? C30 C35 1.543(6) . ? C31 C32 1.544(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.480(8) . ? C32 C39 1.517(10) . ? C32 H32 1.0000 . ? C33 C34 1.500(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C38 1.469(9) . ? C34 C35 1.525(8) . ? C34 H34 1.0000 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.541(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.522(9) . ? C37 C39 1.582(10) . ? C37 H37 1.0000 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N4 1.453(6) . ? C40 C45 1.522(7) . ? C40 C49 1.531(6) . ? C40 C41 1.544(7) . ? C41 C42 1.521(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C48 1.507(7) . ? C42 C43 1.536(8) . ? C42 H42 1.0000 . ? C43 C44 1.514(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C46 1.518(8) . ? C44 C45 1.525(7) . ? C44 H44 1.0000 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.517(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.530(8) . ? C47 C49 1.546(7) . ? C47 H47 1.0000 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? N1 V1 2.002(3) . ? N2 V1 2.011(3) . ? N3 V1 1.664(4) . ? N4 V1 1.696(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C9 121.0(4) . . ? C2 C1 N1 120.2(4) . . ? C9 C1 N1 118.7(4) . . ? C6 C2 C1 117.5(5) . . ? C6 C2 C3 118.9(4) . . ? C1 C2 C3 123.5(4) . . ? C2 C3 C4 110.7(5) . . ? C2 C3 C5 113.3(5) . . ? C4 C3 C5 110.8(5) . . ? C2 C3 H3 107.2 . . ? C4 C3 H3 107.3 . . ? C5 C3 H3 107.3 . . ? C3 C4 H4A 109.4 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.4 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 122.4(5) . . ? C7 C6 H6 118.8 . . ? C2 C6 H6 118.8 . . ? C8 C7 C6 119.2(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 121.8(5) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C8 C9 C1 118.0(4) . . ? C8 C9 C10 120.2(5) . . ? C1 C9 C10 121.8(4) . . ? C12 C10 C9 111.5(4) . . ? C12 C10 C11 110.6(5) . . ? C9 C10 C11 110.5(4) . . ? C12 C10 H10 108.0 . . ? C9 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? 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 . . ? C14 C13 H13A 109.4 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 123.1(4) . . ? N1 C14 C13 120.4(4) . . ? C15 C14 C13 116.5(4) . . ? C16 C15 C14 130.7(4) . . ? C16 C15 H15 114.7 . . ? C14 C15 H15 114.7 . . ? N2 C16 C15 123.2(4) . . ? N2 C16 C17 120.1(4) . . ? C15 C16 C17 116.7(4) . . ? C16 C17 H17A 109.4 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C18 C19 120.9(4) . . ? C26 C18 N2 120.2(4) . . ? C19 C18 N2 118.9(4) . . ? C23 C19 C18 118.2(4) . . ? C23 C19 C20 118.7(4) . . ? C18 C19 C20 123.2(4) . . ? C21 C20 C19 110.4(5) . . ? C21 C20 C22 109.8(5) . . ? C19 C20 C22 112.5(4) . . ? C21 C20 H20 108.0 . . ? C19 C20 H20 108.0 . . ? C22 C20 H20 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.5(5) . . ? C24 C23 H23 119.3 . . ? C19 C23 H23 119.2 . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 121.9(5) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C18 117.8(5) . . ? C25 C26 C27 119.1(4) . . ? C18 C26 C27 123.1(4) . . ? C26 C27 C29 112.9(4) . . ? C26 C27 C28 110.5(4) . . ? C29 C27 C28 110.1(5) . . ? C26 C27 H27 107.7 . . ? C29 C27 H27 107.7 . . ? C28 C27 H27 107.7 . . ? 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 . . ? N3 C30 C31 111.3(4) . . ? N3 C30 C36 110.2(4) . . ? C31 C30 C36 110.5(4) . . ? N3 C30 C35 109.7(4) . . ? C31 C30 C35 107.2(5) . . ? C36 C30 C35 107.8(4) . . ? C30 C31 C32 110.3(4) . . ? C30 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? C30 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C33 C32 C39 111.4(5) . . ? C33 C32 C31 109.5(5) . . ? C39 C32 C31 108.4(5) . . ? C33 C32 H32 109.2 . . ? C39 C32 H32 109.2 . . ? C31 C32 H32 109.2 . . ? C32 C33 C34 110.6(6) . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C38 C34 C33 110.0(6) . . ? C38 C34 C35 109.0(6) . . ? C33 C34 C35 109.4(5) . . ? C38 C34 H34 109.5 . . ? C33 C34 H34 109.5 . . ? C35 C34 H34 109.5 . . ? C34 C35 C30 110.5(5) . . ? C34 C35 H35A 109.6 . . ? C30 C35 H35A 109.6 . . ? C34 C35 H35B 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C30 C36 C37 110.6(5) . . ? C30 C36 H36A 109.5 . . ? C37 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C36 108.8(6) . . ? C38 C37 C39 108.9(6) . . ? C36 C37 C39 107.1(6) . . ? C38 C37 H37 110.7 . . ? C36 C37 H37 110.7 . . ? C39 C37 H37 110.7 . . ? C34 C38 C37 111.8(5) . . ? C34 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C34 C38 H38B 109.3 . . ? C37 C38 H38B 109.3 . . ? H38A C38 H38B 107.9 . . ? C32 C39 C37 108.4(5) . . ? C32 C39 H39A 110.0 . . ? C37 C39 H39A 110.0 . . ? C32 C39 H39B 110.0 . . ? C37 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? N4 C40 C45 111.8(4) . . ? N4 C40 C49 109.6(4) . . ? C45 C40 C49 109.1(4) . . ? N4 C40 C41 110.1(4) . . ? C45 C40 C41 108.7(4) . . ? C49 C40 C41 107.5(4) . . ? C42 C41 C40 111.1(4) . . ? C42 C41 H41A 109.4 . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41B 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C48 C42 C41 110.6(5) . . ? C48 C42 C43 108.8(5) . . ? C41 C42 C43 108.7(4) . . ? C48 C42 H42 109.5 . . ? C41 C42 H42 109.5 . . ? C43 C42 H42 109.6 . . ? C44 C43 C42 109.1(5) . . ? C44 C43 H43A 109.9 . . ? C42 C43 H43A 109.9 . . ? C44 C43 H43B 109.9 . . ? C42 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? C46 C44 C43 109.5(5) . . ? C46 C44 C45 109.6(5) . . ? C43 C44 C45 110.9(5) . . ? C46 C44 H44 108.9 . . ? C43 C44 H44 109.0 . . ? C45 C44 H44 109.0 . . ? C40 C45 C44 109.7(4) . . ? C40 C45 H45A 109.7 . . ? C44 C45 H45A 109.7 . . ? C40 C45 H45B 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C44 C46 C47 109.7(5) . . ? C44 C46 H46A 109.7 . . ? C47 C46 H46A 109.7 . . ? C44 C46 H46B 109.7 . . ? C47 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? C46 C47 C48 109.2(5) . . ? C46 C47 C49 108.5(4) . . ? C48 C47 C49 109.6(5) . . ? C46 C47 H47 109.9 . . ? C48 C47 H47 109.9 . . ? C49 C47 H47 109.9 . . ? C42 C48 C47 109.6(4) . . ? C42 C48 H48A 109.8 . . ? C47 C48 H48A 109.7 . . ? C42 C48 H48B 109.7 . . ? C47 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? C40 C49 C47 110.6(4) . . ? C40 C49 H49A 109.5 . . ? C47 C49 H49A 109.5 . . ? C40 C49 H49B 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? C14 N1 C1 120.1(3) . . ? C14 N1 V1 110.5(3) . . ? C1 N1 V1 128.4(3) . . ? C16 N2 C18 120.1(3) . . ? C16 N2 V1 110.2(3) . . ? C18 N2 V1 129.1(3) . . ? C30 N3 V1 164.4(3) . . ? C40 N4 V1 170.4(3) . . ? N3 V1 N4 118.5(2) . . ? N3 V1 N1 109.87(17) . . ? N4 V1 N1 108.79(16) . . ? N3 V1 N2 111.91(16) . . ? N4 V1 N2 108.93(15) . . ? N1 V1 N2 96.57(15) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.491 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.167 # Attachment 'cpd_6_CCDC_764812.cif' data_a7258' _database_code_depnum_ccdc_archive 'CCDC 764812' #TrackingRef 'cpd_6_CCDC_764812.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H55 N4 V' _chemical_formula_sum 'C43 H55 N4 V' _chemical_formula_weight 678.85 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.4976(7) _cell_length_b 18.3271(6) _cell_length_c 11.2990(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4037.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown(dark) _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9114 _exptl_absorpt_correction_T_max 0.9595 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24352 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3686 _reflns_number_gt 2411 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1025P)^2^+2.3082P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3686 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1918 _refine_ls_wR_factor_gt 0.1529 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.010 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 0.11025(15) 0.40440(19) 0.6258(3) 0.0503(9) Uani 1 1 d . . . C2 C 0.12983(18) 0.4523(2) 0.7166(4) 0.0660(11) Uani 1 1 d . . . C3 C 0.1294(2) 0.4314(3) 0.8460(4) 0.0807(13) Uani 1 1 d . . . H3 H 0.1137 0.3796 0.8523 0.097 Uiso 1 1 calc R . . C4 C 0.2009(3) 0.4363(3) 0.8981(5) 0.130(2) Uani 1 1 d . . . H4A H 0.1996 0.4215 0.9814 0.195 Uiso 1 1 calc R . . H4B H 0.2175 0.4866 0.8924 0.195 Uiso 1 1 calc R . . H4C H 0.2318 0.4039 0.8543 0.195 Uiso 1 1 calc R . . C5 C 0.0794(3) 0.4796(4) 0.9179(5) 0.138(2) Uani 1 1 d . . . H5A H 0.0795 0.4639 1.0008 0.206 Uiso 1 1 calc R . . H5B H 0.0330 0.4747 0.8854 0.206 Uiso 1 1 calc R . . H5C H 0.0940 0.5307 0.9131 0.206 Uiso 1 1 calc R . . C6 C 0.1514(2) 0.5223(3) 0.6820(5) 0.0840(15) Uani 1 1 d . . . H6 H 0.1647 0.5564 0.7410 0.101 Uiso 1 1 calc R . . C7 C 0.1539(2) 0.5423(3) 0.5665(6) 0.0865(15) Uani 1 1 d . . . H7 H 0.1686 0.5901 0.5458 0.104 Uiso 1 1 calc R . . C8 C 0.13541(19) 0.4943(2) 0.4797(5) 0.0761(13) Uani 1 1 d . . . H8 H 0.1379 0.5091 0.3993 0.091 Uiso 1 1 calc R . . C9 C 0.11287(17) 0.4235(2) 0.5067(4) 0.0572(10) Uani 1 1 d . . . C10 C 0.0921(2) 0.3717(2) 0.4101(3) 0.0735(12) Uani 1 1 d . . . H10 H 0.0798 0.3242 0.4482 0.088 Uiso 1 1 calc R . . C11 C 0.0304(3) 0.3973(4) 0.3409(5) 0.1257(16) Uani 1 1 d . . . H11A H 0.0189 0.3611 0.2802 0.189 Uiso 1 1 calc R . . H11B H 0.0408 0.4441 0.3029 0.189 Uiso 1 1 calc R . . H11C H -0.0087 0.4034 0.3947 0.189 Uiso 1 1 calc R . . C12 C 0.1496(3) 0.3572(4) 0.3246(5) 0.1257(16) Uani 1 1 d . . . H12A H 0.1340 0.3231 0.2634 0.189 Uiso 1 1 calc R . . H12B H 0.1886 0.3359 0.3671 0.189 Uiso 1 1 calc R . . H12C H 0.1638 0.4031 0.2874 0.189 Uiso 1 1 calc R . . C13 C -0.02696(17) 0.3820(2) 0.6902(3) 0.0605(10) Uani 1 1 d . . . H13A H -0.0021 0.4281 0.6804 0.091 Uiso 1 1 calc R . . H13B H -0.0509 0.3820 0.7664 0.091 Uiso 1 1 calc R . . H13C H -0.0604 0.3766 0.6260 0.091 Uiso 1 1 calc R . . C14 C 0.02307(14) 0.31931(18) 0.6865(3) 0.0413(7) Uani 1 1 d . . . C15 C -0.0039(2) 0.2500 0.7071(4) 0.0411(11) Uani 1 2 d S . . H15 H -0.0485 0.2500 0.7410 0.049 Uiso 1 2 calc SR . . C16 C 0.2292(2) 0.2500 0.9166(4) 0.0453(11) Uani 1 2 d S . . C17 C 0.2088(2) 0.2500 1.0335(4) 0.0715(17) Uani 1 2 d S . . H17 H 0.1613 0.2500 1.0520 0.086 Uiso 1 2 calc SR . . C18 C 0.2563(3) 0.2500 1.1241(5) 0.0699(17) Uani 1 2 d S . . H18 H 0.2405 0.2500 1.2037 0.084 Uiso 1 2 calc SR . . C19 C 0.3249(2) 0.2500 1.1028(4) 0.0455(11) Uani 1 2 d S . . C20 C 0.3759(3) 0.2500 1.2030(5) 0.0698(16) Uani 1 2 d S . . H20A H 0.3864 0.3004 1.2255 0.105 Uiso 0.50 1 calc PR . . H20B H 0.4180 0.2255 1.1775 0.105 Uiso 0.50 1 calc PR . . H20C H 0.3564 0.2241 1.2710 0.105 Uiso 0.50 1 calc PR . . C21 C 0.3455(2) 0.2500 0.9855(4) 0.0483(12) Uani 1 2 d S . . H21 H 0.3931 0.2500 0.9678 0.058 Uiso 1 2 calc SR . . C22 C 0.2995(2) 0.2500 0.8946(4) 0.0454(11) Uani 1 2 d S . . H22 H 0.3156 0.2500 0.8153 0.055 Uiso 1 2 calc SR . . C23 C 0.2893(2) 0.2500 0.5604(4) 0.0406(10) Uani 1 2 d S . . C24 C 0.32513(17) 0.3148(2) 0.5461(3) 0.0539(9) Uani 1 1 d . . . H24 H 0.3021 0.3601 0.5550 0.065 Uiso 1 1 calc R . . C25 C 0.39444(19) 0.3136(2) 0.5189(3) 0.0663(11) Uani 1 1 d . . . H25 H 0.4180 0.3587 0.5096 0.080 Uiso 1 1 calc R . . C26 C 0.4302(2) 0.2500 0.5050(4) 0.0618(15) Uani 1 2 d S . . C27 C 0.5056(3) 0.2500 0.4735(5) 0.101(3) Uani 1 2 d S . . H27A H 0.5222 0.1996 0.4687 0.152 Uiso 0.50 1 calc PR . . H27B H 0.5314 0.2763 0.5345 0.152 Uiso 0.50 1 calc PR . . H27C H 0.5121 0.2741 0.3969 0.152 Uiso 0.50 1 calc PR . . N1 N 0.08854(12) 0.33147(14) 0.6570(2) 0.0425(7) Uani 1 1 d . . . N2 N 0.18174(19) 0.2500 0.8248(3) 0.0528(10) Uani 1 2 d S . . N3 N 0.22010(18) 0.2500 0.5885(3) 0.0458(9) Uani 1 2 d S . . V1 V 0.15382(3) 0.2500 0.68392(7) 0.0420(3) Uani 1 2 d S . . 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 0.0277(15) 0.049(2) 0.074(3) -0.0023(19) 0.0004(15) 0.0015(14) C2 0.0446(19) 0.062(3) 0.092(3) -0.017(2) -0.009(2) -0.0006(18) C3 0.081(3) 0.076(3) 0.084(3) -0.029(3) -0.024(2) 0.000(2) C4 0.113(4) 0.109(4) 0.168(6) -0.011(4) -0.071(4) -0.023(3) C5 0.159(6) 0.147(5) 0.107(5) -0.055(4) -0.003(4) 0.035(5) C6 0.056(2) 0.054(3) 0.142(5) -0.017(3) -0.009(3) -0.008(2) C7 0.056(2) 0.053(3) 0.150(5) 0.008(3) 0.015(3) -0.005(2) C8 0.058(2) 0.063(3) 0.107(4) 0.022(3) 0.026(2) 0.007(2) C9 0.0433(18) 0.053(2) 0.076(3) 0.006(2) 0.0123(18) 0.0056(16) C10 0.105(3) 0.060(3) 0.055(2) 0.011(2) 0.014(2) 0.013(2) C11 0.085(3) 0.177(4) 0.115(3) -0.047(3) -0.005(2) 0.034(3) C12 0.085(3) 0.177(4) 0.115(3) -0.047(3) -0.005(2) 0.034(3) C13 0.0441(19) 0.062(2) 0.075(3) -0.0023(19) 0.0064(18) 0.0106(16) C14 0.0326(15) 0.056(2) 0.0355(16) -0.0025(15) -0.0038(13) 0.0070(14) C15 0.031(2) 0.055(3) 0.037(2) 0.000 0.0014(18) 0.000 C16 0.034(2) 0.061(3) 0.040(3) 0.000 -0.0056(19) 0.000 C17 0.033(2) 0.132(5) 0.049(3) 0.000 0.007(2) 0.000 C18 0.048(3) 0.124(5) 0.038(3) 0.000 0.005(2) 0.000 C19 0.041(2) 0.052(3) 0.043(3) 0.000 -0.004(2) 0.000 C20 0.058(3) 0.101(5) 0.051(3) 0.000 -0.020(3) 0.000 C21 0.031(2) 0.070(3) 0.044(3) 0.000 0.000(2) 0.000 C22 0.039(2) 0.065(3) 0.032(2) 0.000 0.0017(19) 0.000 C23 0.030(2) 0.051(3) 0.040(2) 0.000 -0.0044(18) 0.000 C24 0.0458(18) 0.058(2) 0.058(2) 0.0064(18) -0.0024(16) -0.0053(16) C25 0.052(2) 0.091(3) 0.057(2) 0.016(2) -0.0054(18) -0.025(2) C26 0.038(3) 0.110(5) 0.038(3) 0.000 -0.006(2) 0.000 C27 0.043(3) 0.203(8) 0.058(4) 0.000 0.005(3) 0.000 N1 0.0324(13) 0.0473(16) 0.0478(16) -0.0028(13) -0.0044(12) -0.0005(11) N2 0.036(2) 0.067(3) 0.056(3) 0.000 -0.0082(18) 0.000 N3 0.037(2) 0.047(2) 0.054(2) 0.000 -0.0046(17) 0.000 V1 0.0267(4) 0.0528(5) 0.0465(5) 0.000 -0.0065(3) 0.000 _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 C9 1.392(5) . ? C1 C2 1.403(5) . ? C1 N1 1.446(4) . ? C2 C6 1.405(6) . ? C2 C3 1.511(6) . ? C3 C4 1.516(6) . ? C3 C5 1.546(6) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.357(7) . ? C6 H6 0.9500 . ? C7 C8 1.366(7) . ? C7 H7 0.9500 . ? C8 C9 1.403(5) . ? C8 H8 0.9500 . ? C9 C10 1.502(6) . ? C10 C12 1.505(6) . ? C10 C11 1.510(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 . ? C13 C14 1.507(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N1 1.338(4) . ? C14 C15 1.395(4) . ? C15 C14 1.395(4) 8_565 ? C15 H15 0.9500 . ? C16 C17 1.380(6) . ? C16 N2 1.390(5) . ? C16 C22 1.392(6) . ? C17 C18 1.380(7) . ? C17 H17 0.9500 . ? C18 C19 1.359(6) . ? C18 H18 0.9500 . ? C19 C21 1.385(6) . ? C19 C20 1.507(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.363(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 N3 1.386(5) . ? C23 C24 1.387(4) . ? C23 C24 1.387(4) 8_565 ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 C26 1.368(5) . ? C25 H25 0.9500 . ? C26 C25 1.368(5) 8_565 ? C26 C27 1.512(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? N1 V1 1.985(3) . ? N2 V1 1.682(4) . ? N3 V1 1.683(4) . ? V1 N1 1.985(3) 8_565 ? 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 C9 C1 C2 122.7(4) . . ? C9 C1 N1 118.6(3) . . ? C2 C1 N1 118.7(3) . . ? C1 C2 C6 116.7(4) . . ? C1 C2 C3 123.2(4) . . ? C6 C2 C3 120.1(4) . . ? C2 C3 C4 110.9(4) . . ? C2 C3 C5 111.5(4) . . ? C4 C3 C5 110.0(4) . . ? C2 C3 H3 108.1 . . ? C4 C3 H3 108.1 . . ? C5 C3 H3 108.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.7(5) . . ? C7 C6 H6 119.1 . . ? C2 C6 H6 119.1 . . ? C6 C7 C8 120.4(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 121.6(5) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C1 C9 C8 117.0(4) . . ? C1 C9 C10 122.3(3) . . ? C8 C9 C10 120.8(4) . . ? C9 C10 C12 112.2(4) . . ? C9 C10 C11 113.2(4) . . ? C12 C10 C11 108.5(4) . . ? C9 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? 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 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 123.6(3) . . ? N1 C14 C13 119.8(3) . . ? C15 C14 C13 116.4(3) . . ? C14 C15 C14 131.2(4) . 8_565 ? C14 C15 H15 114.4 . . ? C14 C15 H15 114.4 8_565 . ? C17 C16 N2 121.5(4) . . ? C17 C16 C22 117.0(4) . . ? N2 C16 C22 121.5(4) . . ? C16 C17 C18 121.1(4) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 121.9(5) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C21 117.1(4) . . ? C18 C19 C20 121.1(5) . . ? C21 C19 C20 121.9(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C19 122.0(4) . . ? C22 C21 H21 119.0 . . ? C19 C21 H21 119.0 . . ? C21 C22 C16 120.9(4) . . ? C21 C22 H22 119.6 . . ? C16 C22 H22 119.6 . . ? N3 C23 C24 121.1(2) . . ? N3 C23 C24 121.1(2) . 8_565 ? C24 C23 C24 117.8(4) . 8_565 ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 122.4(4) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C25 C26 C25 116.9(5) 8_565 . ? C25 C26 C27 121.5(2) 8_565 . ? C25 C26 C27 121.5(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C14 N1 C1 119.6(3) . . ? C14 N1 V1 116.6(2) . . ? C1 N1 V1 123.02(18) . . ? C16 N2 V1 157.1(3) . . ? C23 N3 V1 153.4(3) . . ? N2 V1 N3 110.95(18) . . ? N2 V1 N1 110.64(11) . 8_565 ? N3 V1 N1 113.21(10) . 8_565 ? N2 V1 N1 110.64(11) . . ? N3 V1 N1 113.21(10) . . ? N1 V1 N1 97.53(14) 8_565 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.497 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.108