Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Gibson, Vernon' 'Newton, Claire' 'Redshaw, Carl' 'Solan, Gregory A.' 'White, Andrew J. P.' 'WIlliams, David J.' _publ_contact_author_name 'Prof Vernon Gibson' _publ_contact_author_address ; Prof Vernon Gibson Chemistry Imperial College Exhibition Road London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email 'V.GIBSON@IC.AC.UK' _publ_section_title ; Chromium Complexes Bearing Pyrrolide-Imine N,N-Chelate Ligands: Synthesis, Structures and Ethylene Polymerisation Behaviour ; data_Compound 1 _database_code_CSD 185874 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H42 N4 Cr' _chemical_formula_weight 558.72 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.2491(15) _cell_length_b 10.5695(10) _cell_length_c 17.731(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.934(8) _cell_angle_gamma 90.00 _cell_volume 3075.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.75 _cell_measurement_theta_max 28.02 _exptl_crystal_description prisms _exptl_crystal_colour Orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method ? _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 3.261 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.5012 _exptl_absorpt_correction_T_max 0.7134 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4701 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 59.99 _reflns_number_total 4533 _reflns_number_observed 3427 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 279 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.2010P)^2^+2.2371P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4254 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_obs 0.0863 _refine_ls_wR_factor_all 0.2923 _refine_ls_wR_factor_obs 0.2544 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_restrained_S_all 1.107 _refine_ls_restrained_S_obs 1.112 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr -0.00138(6) 0.45368(9) 0.24367(5) 0.0344(4) Uani 1 d . . N1 N -0.0161(3) 0.2685(4) 0.2031(2) 0.0249(9) Uani 1 d . . C2 C 0.0161(3) 0.1498(5) 0.2146(3) 0.0318(12) Uani 1 d . . H2A H 0.0626(3) 0.1263(5) 0.2561(3) 0.038 Uiso 1 calc R . C3 C -0.0295(4) 0.0687(5) 0.1565(4) 0.0371(13) Uani 1 d . . H3A H -0.0201(4) -0.0181(5) 0.1519(4) 0.045 Uiso 1 calc R . C4 C -0.0916(3) 0.1398(5) 0.1066(3) 0.0335(12) Uani 1 d . . H4A H -0.1320(3) 0.1105(5) 0.0613(3) 0.040 Uiso 1 calc R . C5 C -0.0830(3) 0.2621(5) 0.1359(3) 0.0230(10) Uani 1 d . . C6 C -0.1276(3) 0.3743(5) 0.1097(3) 0.0260(11) Uani 1 d . . H6A H -0.1741(3) 0.3722(5) 0.0649(3) 0.031 Uiso 1 calc R . N7 N -0.1052(2) 0.4799(4) 0.1466(2) 0.0225(9) Uani 1 d . . C8 C -0.1523(3) 0.5919(5) 0.1203(3) 0.0224(10) Uani 1 d . . C9 C -0.2121(3) 0.6267(5) 0.1551(3) 0.0273(11) Uani 1 d . . C10 C -0.2515(3) 0.7415(6) 0.1332(3) 0.0357(12) Uani 1 d . . H10A H -0.2912(3) 0.7674(6) 0.1562(3) 0.043 Uiso 1 calc R . C11 C -0.2330(4) 0.8184(6) 0.0779(3) 0.0407(14) Uani 1 d . . H11A H -0.2602(4) 0.8960(6) 0.0639(3) 0.049 Uiso 1 calc R . C12 C -0.1762(4) 0.7830(5) 0.0438(3) 0.0354(12) Uani 1 d . . H12A H -0.1652(4) 0.8363(5) 0.0059(3) 0.042 Uiso 1 calc R . C13 C -0.1335(3) 0.6689(5) 0.0634(3) 0.0257(11) Uani 1 d . . C14 C -0.2326(3) 0.5402(6) 0.2150(3) 0.0352(13) Uani 1 d . . H14A H -0.1842(3) 0.4878(6) 0.2412(3) 0.042 Uiso 1 calc R . C15 C -0.3012(5) 0.4549(8) 0.1728(6) 0.071(2) Uani 1 d . . H15A H -0.2865(5) 0.4076(8) 0.1324(6) 0.106 Uiso 1 calc R . H15B H -0.3495(5) 0.5051(8) 0.1482(6) 0.106 Uiso 1 calc R . H15C H -0.3123(5) 0.3966(8) 0.2105(6) 0.106 Uiso 1 calc R . C16 C -0.2563(8) 0.6138(10) 0.2782(6) 0.087(3) Uani 1 d . . H16A H -0.2119(8) 0.6695(10) 0.3058(6) 0.131 Uiso 1 calc R . H16B H -0.2674(8) 0.5552(10) 0.3157(6) 0.131 Uiso 1 calc R . H16C H -0.3046(8) 0.6637(10) 0.2534(6) 0.131 Uiso 1 calc R . C17 C -0.0687(3) 0.6329(6) 0.0257(3) 0.0330(12) Uani 1 d . . H17A H -0.0585(3) 0.5411(6) 0.0346(3) 0.040 Uiso 1 calc R . C18 C -0.0937(4) 0.6545(8) -0.0628(4) 0.050(2) Uani 1 d . . H18A H -0.1446(4) 0.6109(8) -0.0879(4) 0.074 Uiso 1 calc R . H18B H -0.0517(4) 0.6221(8) -0.0836(4) 0.074 Uiso 1 calc R . H18C H -0.1008(4) 0.7445(8) -0.0737(4) 0.074 Uiso 1 calc R . C19 C 0.0108(4) 0.7001(10) 0.0666(4) 0.065(2) Uani 1 d . . H19A H 0.0258(4) 0.6852(10) 0.1232(4) 0.098 Uiso 1 calc R . H19B H 0.0042(4) 0.7902(10) 0.0563(4) 0.098 Uiso 1 calc R . H19C H 0.0532(4) 0.6679(10) 0.0464(4) 0.098 Uiso 1 calc R . N21 N 0.0124(2) 0.6397(4) 0.2836(2) 0.0248(9) Uani 1 d . . C22 C -0.0179(3) 0.7561(5) 0.2717(3) 0.0323(12) Uani 1 d . . H22A H -0.0645(3) 0.7791(5) 0.2301(3) 0.039 Uiso 1 calc R . C23 C 0.0285(3) 0.8407(5) 0.3292(3) 0.0298(11) Uani 1 d . . H23A H 0.0195(3) 0.9279(5) 0.3328(3) 0.036 Uiso 1 calc R . C24 C 0.0903(3) 0.7688(5) 0.3796(3) 0.0263(11) Uani 1 d . . H24A H 0.1314(3) 0.7978(5) 0.4246(3) 0.032 Uiso 1 calc R . C25 C 0.0800(3) 0.6461(5) 0.3509(3) 0.0208(10) Uani 1 d . . C26 C 0.1237(3) 0.5322(5) 0.3778(3) 0.0226(10) Uani 1 d . . H26A H 0.1690(3) 0.5331(5) 0.4239(3) 0.027 Uiso 1 calc R . N27 N 0.1018(2) 0.4285(4) 0.3399(2) 0.0205(8) Uani 1 d . . C28 C 0.1434(3) 0.3129(4) 0.3702(3) 0.0184(9) Uani 1 d . . C29 C 0.1123(3) 0.2359(5) 0.4187(3) 0.0250(10) Uani 1 d . . C30 C 0.1482(3) 0.1202(5) 0.4423(3) 0.0300(11) Uani 1 d . . H30A H 0.1278(3) 0.0674(5) 0.4745(3) 0.036 Uiso 1 calc R . C31 C 0.2143(3) 0.0806(5) 0.4189(3) 0.0299(11) Uani 1 d . . H31A H 0.2383(3) 0.0013(5) 0.4353(3) 0.036 Uiso 1 calc R . C32 C 0.2446(3) 0.1565(5) 0.3721(3) 0.0304(11) Uani 1 d . . H32A H 0.2892(3) 0.1285(5) 0.3567(3) 0.037 Uiso 1 calc R . C33 C 0.2104(3) 0.2748(5) 0.3470(3) 0.0229(10) Uani 1 d . . C34 C 0.0411(3) 0.2804(6) 0.4451(4) 0.0371(13) Uani 1 d . . H34A H 0.0116(3) 0.3454(6) 0.4067(4) 0.045 Uiso 1 calc R . C35 C 0.0711(5) 0.3438(8) 0.5264(5) 0.060(2) Uani 1 d . . H35A H 0.0248(5) 0.3715(8) 0.5421(5) 0.091 Uiso 1 calc R . H35B H 0.1047(5) 0.4163(8) 0.5237(5) 0.091 Uiso 1 calc R . H35C H 0.1031(5) 0.2839(8) 0.5650(5) 0.091 Uiso 1 calc R . C36 C -0.0192(5) 0.1753(9) 0.4446(5) 0.066(2) Uani 1 d . . H36A H -0.0633(5) 0.2088(9) 0.4619(5) 0.099 Uiso 1 calc R . H36B H 0.0083(5) 0.1084(9) 0.4803(5) 0.099 Uiso 1 calc R . H36C H -0.0411(5) 0.1417(9) 0.3913(5) 0.099 Uiso 1 calc R . C37 C 0.2447(3) 0.3616(6) 0.2962(3) 0.0329(12) Uani 1 d . . H37A H 0.1997(3) 0.4154(6) 0.2641(3) 0.040 Uiso 1 calc R . C38 C 0.3098(4) 0.4481(6) 0.3489(5) 0.050(2) Uani 1 d . . H38A H 0.3311(4) 0.5028(6) 0.3161(5) 0.075 Uiso 1 calc R . H38B H 0.3536(4) 0.3973(6) 0.3828(5) 0.075 Uiso 1 calc R . H38C H 0.2859(4) 0.4993(6) 0.3815(5) 0.075 Uiso 1 calc R . C39 C 0.2797(4) 0.2884(8) 0.2391(4) 0.051(2) Uani 1 d . . H39A H 0.2380(4) 0.2336(8) 0.2058(4) 0.077 Uiso 1 calc R . H39B H 0.3257(4) 0.2377(8) 0.2693(4) 0.077 Uiso 1 calc R . H39C H 0.2976(4) 0.3478(8) 0.2061(4) 0.077 Uiso 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 Cr 0.0325(6) 0.0305(6) 0.0358(6) 0.0004(4) 0.0038(4) 0.0023(4) N1 0.026(2) 0.022(2) 0.025(2) -0.001(2) 0.006(2) -0.001(2) C2 0.035(3) 0.024(3) 0.032(3) 0.002(2) 0.005(2) 0.005(2) C3 0.046(3) 0.018(2) 0.047(3) -0.001(2) 0.014(3) 0.004(2) C4 0.039(3) 0.027(3) 0.032(3) -0.006(2) 0.006(2) -0.007(2) C5 0.024(2) 0.018(2) 0.027(2) 0.000(2) 0.008(2) -0.002(2) C6 0.021(2) 0.027(3) 0.026(2) 0.001(2) 0.003(2) -0.002(2) N7 0.017(2) 0.022(2) 0.024(2) 0.006(2) -0.001(2) 0.001(2) C8 0.019(2) 0.021(2) 0.021(2) 0.002(2) -0.004(2) 0.000(2) C9 0.019(2) 0.031(3) 0.027(2) 0.002(2) 0.000(2) 0.004(2) C10 0.025(3) 0.038(3) 0.040(3) -0.003(2) 0.004(2) 0.009(2) C11 0.044(3) 0.031(3) 0.039(3) 0.009(2) 0.000(3) 0.019(3) C12 0.044(3) 0.024(3) 0.031(3) 0.010(2) 0.001(2) 0.005(2) C13 0.024(2) 0.025(2) 0.023(2) 0.004(2) 0.000(2) 0.002(2) C14 0.030(3) 0.040(3) 0.037(3) 0.007(2) 0.012(2) 0.004(2) C15 0.063(5) 0.058(5) 0.085(6) 0.018(4) 0.014(4) -0.025(4) C16 0.142(10) 0.070(6) 0.069(5) 0.000(4) 0.060(6) -0.007(6) C17 0.032(3) 0.035(3) 0.033(3) 0.007(2) 0.012(2) 0.000(2) C18 0.044(3) 0.074(5) 0.033(3) 0.000(3) 0.014(3) -0.013(3) C19 0.026(3) 0.113(7) 0.053(4) -0.024(4) 0.007(3) -0.013(4) N21 0.023(2) 0.022(2) 0.027(2) -0.002(2) 0.005(2) -0.001(2) C22 0.027(3) 0.031(3) 0.034(3) 0.002(2) 0.002(2) 0.001(2) C23 0.036(3) 0.016(2) 0.039(3) -0.003(2) 0.014(2) 0.003(2) C24 0.023(2) 0.028(3) 0.030(2) -0.004(2) 0.012(2) -0.003(2) C25 0.018(2) 0.022(2) 0.024(2) -0.003(2) 0.009(2) -0.001(2) C26 0.017(2) 0.027(3) 0.025(2) 0.003(2) 0.008(2) 0.003(2) N27 0.014(2) 0.023(2) 0.022(2) 0.003(2) 0.002(2) 0.005(2) C28 0.014(2) 0.018(2) 0.019(2) 0.001(2) -0.002(2) 0.004(2) C29 0.019(2) 0.028(3) 0.025(2) 0.001(2) 0.003(2) 0.000(2) C30 0.030(3) 0.027(3) 0.026(2) 0.006(2) -0.001(2) -0.002(2) C31 0.025(3) 0.020(2) 0.037(3) 0.002(2) -0.002(2) 0.007(2) C32 0.019(2) 0.031(3) 0.037(3) -0.001(2) 0.001(2) 0.008(2) C33 0.014(2) 0.026(2) 0.026(2) 0.002(2) 0.002(2) 0.004(2) C34 0.033(3) 0.042(3) 0.044(3) 0.010(3) 0.022(3) 0.009(2) C35 0.068(5) 0.061(5) 0.069(5) -0.016(4) 0.047(4) -0.010(4) C36 0.046(4) 0.079(6) 0.084(5) -0.020(5) 0.035(4) -0.014(4) C37 0.024(3) 0.036(3) 0.042(3) 0.011(2) 0.015(2) 0.009(2) C38 0.033(3) 0.042(4) 0.081(5) -0.003(3) 0.028(3) -0.004(3) C39 0.050(4) 0.067(4) 0.048(3) 0.013(3) 0.032(3) 0.017(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 Cr N27 2.069(4) . ? Cr N1 2.073(4) . ? Cr N21 2.078(4) . ? Cr N7 2.085(4) . ? N1 C2 1.361(7) . ? N1 C5 1.382(7) . ? C2 C3 1.384(8) . ? C3 C4 1.382(9) . ? C4 C5 1.384(8) . ? C5 C6 1.413(7) . ? C6 N7 1.291(7) . ? N7 C8 1.430(6) . ? C8 C9 1.405(7) . ? C8 C13 1.409(7) . ? C9 C10 1.386(8) . ? C9 C14 1.523(8) . ? C10 C11 1.384(9) . ? C11 C12 1.353(9) . ? C12 C13 1.401(7) . ? C13 C17 1.517(7) . ? C14 C15 1.493(10) . ? C14 C16 1.520(10) . ? C17 C18 1.512(8) . ? C17 C19 1.515(8) . ? N21 C22 1.328(7) . ? N21 C25 1.389(6) . ? C22 C23 1.407(8) . ? C23 C24 1.388(8) . ? C24 C25 1.384(7) . ? C25 C26 1.423(7) . ? C26 N27 1.281(7) . ? N27 C28 1.435(6) . ? C28 C33 1.401(7) . ? C28 C29 1.403(7) . ? C29 C30 1.377(8) . ? C29 C34 1.518(7) . ? C30 C31 1.393(8) . ? C31 C32 1.368(8) . ? C32 C33 1.396(7) . ? C33 C37 1.527(7) . ? C34 C36 1.520(10) . ? C34 C35 1.529(10) . ? C37 C38 1.524(9) . ? C37 C39 1.538(8) . ? 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 N27 Cr N1 98.4(2) . . ? N27 Cr N21 82.1(2) . . ? N1 Cr N21 179.50(15) . . ? N27 Cr N7 179.7(2) . . ? N1 Cr N7 81.8(2) . . ? N21 Cr N7 97.7(2) . . ? C2 N1 C5 106.1(4) . . ? C2 N1 Cr 144.8(4) . . ? C5 N1 Cr 109.0(3) . . ? N1 C2 C3 110.4(5) . . ? C4 C3 C2 106.8(5) . . ? C3 C4 C5 107.2(5) . . ? N1 C5 C4 109.5(4) . . ? N1 C5 C6 117.9(4) . . ? C4 C5 C6 132.6(5) . . ? N7 C6 C5 120.8(4) . . ? C6 N7 C8 119.9(4) . . ? C6 N7 Cr 110.5(3) . . ? C8 N7 Cr 129.5(3) . . ? C9 C8 C13 121.6(5) . . ? C9 C8 N7 119.6(4) . . ? C13 C8 N7 118.6(4) . . ? C10 C9 C8 118.0(5) . . ? C10 C9 C14 121.5(5) . . ? C8 C9 C14 120.6(5) . . ? C11 C10 C9 120.8(5) . . ? C12 C11 C10 120.7(5) . . ? C11 C12 C13 121.6(5) . . ? C12 C13 C8 117.2(5) . . ? C12 C13 C17 120.5(5) . . ? C8 C13 C17 122.3(5) . . ? C15 C14 C16 109.1(7) . . ? C15 C14 C9 109.3(5) . . ? C16 C14 C9 112.3(6) . . ? C18 C17 C19 110.6(5) . . ? C18 C17 C13 114.0(5) . . ? C19 C17 C13 110.7(5) . . ? C22 N21 C25 106.1(4) . . ? C22 N21 Cr 145.5(4) . . ? C25 N21 Cr 108.4(3) . . ? N21 C22 C23 111.4(5) . . ? C24 C23 C22 105.7(5) . . ? C25 C24 C23 106.9(4) . . ? C24 C25 N21 109.9(4) . . ? C24 C25 C26 132.4(4) . . ? N21 C25 C26 117.7(4) . . ? N27 C26 C25 120.5(4) . . ? C26 N27 C28 120.0(4) . . ? C26 N27 Cr 111.3(3) . . ? C28 N27 Cr 128.5(3) . . ? C33 C28 C29 121.2(4) . . ? C33 C28 N27 119.8(4) . . ? C29 C28 N27 118.8(4) . . ? C30 C29 C28 118.8(5) . . ? C30 C29 C34 120.8(5) . . ? C28 C29 C34 120.4(5) . . ? C29 C30 C31 120.6(5) . . ? C32 C31 C30 120.3(5) . . ? C31 C32 C33 121.1(5) . . ? C32 C33 C28 118.0(5) . . ? C32 C33 C37 121.6(4) . . ? C28 C33 C37 120.4(4) . . ? C29 C34 C36 112.9(5) . . ? C29 C34 C35 110.8(5) . . ? C36 C34 C35 111.0(6) . . ? C38 C37 C33 110.2(5) . . ? C38 C37 C39 110.0(5) . . ? C33 C37 C39 112.8(5) . . ? _refine_diff_density_max 0.844 _refine_diff_density_min -1.583 _refine_diff_density_rms 0.122 data_Compound 2 _database_code_CSD 185875 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44.50 H64 N4 O2 Cl2 Li Cr' _chemical_formula_weight 816.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.598(4) _cell_length_b 17.638(4) _cell_length_c 15.151(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.061(14) _cell_angle_gamma 90.00 _cell_volume 4599.1(20) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 4.74 _cell_measurement_theta_max 10.50 _exptl_crystal_description prisms _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method ? _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.403 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6217 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.1852 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5949 _reflns_number_observed 2736 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1051 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0584P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4898 _refine_ls_number_parameters 526 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.1926 _refine_ls_R_factor_obs 0.0741 _refine_ls_wR_factor_all 0.5432 _refine_ls_wR_factor_obs 0.1331 _refine_ls_goodness_of_fit_all 0.986 _refine_ls_goodness_of_fit_obs 1.149 _refine_ls_restrained_S_all 3.501 _refine_ls_restrained_S_obs 1.157 _refine_ls_shift/esd_max -0.056 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr -0.19211(7) 0.03121(8) 0.10395(9) 0.0341(4) Uani 1 d . . Li Li -0.0730(9) -0.1121(9) 0.1451(12) 0.056(5) Uani 1 d . . Cl1 Cl -0.12932(12) -0.04471(13) 0.01365(14) 0.0447(6) Uani 1 d . . Cl2 Cl -0.15855(13) -0.05649(12) 0.22284(15) 0.0446(6) Uani 1 d . . N1 N -0.0963(4) 0.0964(4) 0.1318(4) 0.035(2) Uani 1 d . . C2 C -0.0295(5) 0.1037(6) 0.1032(6) 0.048(2) Uani 1 d . . H2A H -0.0091(5) 0.0667(6) 0.0701(6) 0.057 Uiso 1 calc R . C3 C 0.0053(5) 0.1727(6) 0.1288(6) 0.052(3) Uani 1 d . . H3A H 0.0526(5) 0.1903(6) 0.1168(6) 0.063 Uiso 1 calc R . C4 C -0.0426(5) 0.2109(6) 0.1754(6) 0.054(3) Uani 1 d . . H4A H -0.0345(5) 0.2594(6) 0.2014(6) 0.065 Uiso 1 calc R . C5 C -0.1059(5) 0.1624(5) 0.1759(6) 0.040(2) Uani 1 d . . C6 C -0.1729(5) 0.1671(5) 0.2112(5) 0.037(2) Uani 1 d . . H6A H -0.1806(5) 0.2096(5) 0.2457(5) 0.045 Uiso 1 calc R . N7 N -0.2242(4) 0.1142(4) 0.1971(4) 0.031(2) Uani 1 d . . C8 C -0.2855(5) 0.1198(5) 0.2476(6) 0.036(2) Uani 1 d . . C9 C -0.2708(5) 0.0973(5) 0.3370(6) 0.044(2) Uani 1 d . . C10 C -0.3328(7) 0.1074(5) 0.3840(6) 0.059(3) Uani 1 d . . H10A H -0.3257(7) 0.0920(5) 0.4446(6) 0.071 Uiso 1 calc R . C11 C -0.4017(6) 0.1387(6) 0.3427(8) 0.064(3) Uani 1 d . . H11A H -0.4419(6) 0.1436(6) 0.3745(8) 0.076 Uiso 1 calc R . C12 C -0.4128(5) 0.1624(5) 0.2575(7) 0.053(3) Uani 1 d . . H12A H -0.4604(5) 0.1856(5) 0.2318(7) 0.064 Uiso 1 calc R . C13 C -0.3561(5) 0.1544(5) 0.2036(6) 0.037(2) Uani 1 d . . C14 C -0.1913(6) 0.0708(5) 0.3876(6) 0.057(3) Uani 1 d . . H14A H -0.1597(6) 0.0604(5) 0.3420(6) 0.068 Uiso 1 calc R . C15 C -0.1506(6) 0.1327(6) 0.4489(7) 0.068(3) Uani 1 d . . H15A H -0.1497(6) 0.1789(6) 0.4143(7) 0.102 Uiso 1 calc R . H15B H -0.0978(6) 0.1171(6) 0.4747(7) 0.102 Uiso 1 calc R . H15C H -0.1782(6) 0.1418(6) 0.4970(7) 0.102 Uiso 1 calc R . C16 C -0.1925(7) -0.0009(6) 0.4417(7) 0.083(4) Uani 1 d . . H16A H -0.2186(7) -0.0407(6) 0.4027(7) 0.124 Uiso 1 calc R . H16B H -0.2201(7) 0.0084(6) 0.4898(7) 0.124 Uiso 1 calc R . H16C H -0.1397(7) -0.0163(6) 0.4675(7) 0.124 Uiso 1 calc R . C17 C -0.3678(5) 0.1893(6) 0.1119(6) 0.051(3) Uani 1 d . . H17A H -0.3309(5) 0.1641(6) 0.0801(6) 0.061 Uiso 1 calc R . C18 C -0.3473(7) 0.2733(6) 0.1175(8) 0.089(4) Uani 1 d . . H18A H -0.3555(7) 0.2944(6) 0.0571(8) 0.133 Uiso 1 calc R . H18B H -0.2933(7) 0.2795(6) 0.1473(8) 0.133 Uiso 1 calc R . H18C H -0.3802(7) 0.2995(6) 0.1516(8) 0.133 Uiso 1 calc R . C19 C -0.4498(5) 0.1766(7) 0.0543(7) 0.094(4) Uani 1 d . . H19A H -0.4537(5) 0.2005(7) -0.0041(7) 0.140 Uiso 1 calc R . H19B H -0.4879(5) 0.1986(7) 0.0845(7) 0.140 Uiso 1 calc R . H19C H -0.4595(5) 0.1226(7) 0.0462(7) 0.140 Uiso 1 calc R . N21 N -0.2357(4) 0.1016(4) 0.0020(4) 0.034(2) Uani 1 d . . C22 C -0.2193(5) 0.1694(5) -0.0308(6) 0.041(2) Uani 1 d . . H22A H -0.1740(5) 0.1974(5) -0.0085(6) 0.049 Uiso 1 calc R . C23 C -0.2784(5) 0.1924(5) -0.1020(6) 0.042(2) Uani 1 d . . H23A H -0.2804(5) 0.2377(5) -0.1353(6) 0.051 Uiso 1 calc R . C24 C -0.3330(5) 0.1357(5) -0.1138(6) 0.044(2) Uani 1 d . . H24A H -0.3795(5) 0.1343(5) -0.1577(6) 0.053 Uiso 1 calc R . C25 C -0.3070(5) 0.0808(5) -0.0493(6) 0.037(2) Uani 1 d . . C26 C -0.3365(5) 0.0104(5) -0.0249(5) 0.037(2) Uani 1 d . . H26A H -0.3832(5) -0.0093(5) -0.0586(5) 0.044 Uiso 1 calc R . N27 N -0.2982(3) -0.0259(4) 0.0439(4) 0.033(2) Uani 1 d . . C28 C -0.3231(5) -0.1043(5) 0.0532(6) 0.037(2) Uani 1 d . . C29 C -0.3521(4) -0.1262(4) 0.1291(6) 0.033(2) Uani 1 d . . C30 C -0.3739(5) -0.2014(5) 0.1345(7) 0.052(3) Uani 1 d . . H30A H -0.3939(5) -0.2173(5) 0.1843(7) 0.063 Uiso 1 calc R . C31 C -0.3670(5) -0.2531(5) 0.0692(7) 0.057(3) Uani 1 d . . H31A H -0.3808(5) -0.3040(5) 0.0754(7) 0.068 Uiso 1 calc R . C32 C -0.3400(5) -0.2307(6) -0.0048(7) 0.059(3) Uani 1 d . . H32A H -0.3365(5) -0.2667(6) -0.0495(7) 0.070 Uiso 1 calc R . C33 C -0.3175(5) -0.1561(5) -0.0165(6) 0.044(2) Uani 1 d . . C34 C -0.3678(5) -0.0688(5) 0.1964(6) 0.046(2) Uani 1 d . . H34A H -0.3292(5) -0.0275(5) 0.1994(6) 0.055 Uiso 1 calc R . C35 C -0.4484(5) -0.0348(6) 0.1614(7) 0.071(3) Uani 1 d . . H35A H -0.4515(5) -0.0148(6) 0.1011(7) 0.107 Uiso 1 calc R . H35B H -0.4573(5) 0.0058(6) 0.2013(7) 0.107 Uiso 1 calc R . H35C H -0.4875(5) -0.0738(6) 0.1598(7) 0.107 Uiso 1 calc R . C36 C -0.3603(7) -0.1004(6) 0.2895(6) 0.075(4) Uani 1 d . . H36A H -0.3711(7) -0.0609(6) 0.3297(6) 0.113 Uiso 1 calc R . H36B H -0.3079(7) -0.1193(6) 0.3109(6) 0.113 Uiso 1 calc R . H36C H -0.3971(7) -0.1416(6) 0.2883(6) 0.113 Uiso 1 calc R . C37 C -0.2919(5) -0.1367(5) -0.1038(6) 0.048(3) Uani 1 d . . H37A H -0.2712(5) -0.0844(5) -0.0986(6) 0.058 Uiso 1 calc R . C38 C -0.3607(5) -0.1391(6) -0.1822(6) 0.059(3) Uani 1 d . . H38A H -0.4009(5) -0.1054(6) -0.1703(6) 0.089 Uiso 1 calc R . H38B H -0.3808(5) -0.1904(6) -0.1900(6) 0.089 Uiso 1 calc R . H38C H -0.3446(5) -0.1230(6) -0.2367(6) 0.089 Uiso 1 calc R . C39 C -0.2284(6) -0.1892(6) -0.1215(7) 0.074(3) Uani 1 d . . H39A H -0.1845(6) -0.1873(6) -0.0708(7) 0.111 Uiso 1 calc R . H39B H -0.2120(6) -0.1732(6) -0.1759(7) 0.111 Uiso 1 calc R . H39C H -0.2481(6) -0.2406(6) -0.1291(7) 0.111 Uiso 1 calc R . O40 O 0.0331(3) -0.0927(4) 0.2011(4) 0.057(2) Uani 1 d D . C41 C 0.0571(5) -0.0462(7) 0.2788(6) 0.082(4) Uani 1 d D . H41A H 0.0344(5) -0.0646(7) 0.3286(6) 0.098 Uiso 0.60 calc PR 1 H41B H 0.0405(5) 0.0063(7) 0.2654(6) 0.098 Uiso 0.60 calc PR 1 H41C H 0.0651(5) -0.0762(7) 0.3328(6) 0.098 Uiso 0.40 d PR 2 H41D H 0.0181(5) -0.0088(7) 0.2815(6) 0.098 Uiso 0.40 d PR 2 C42 C 0.1446(6) -0.0509(11) 0.3038(8) 0.081(6) Uani 0.60 d PD 1 H42A H 0.1672(6) -0.0040(11) 0.3326(8) 0.097 Uiso 0.60 calc PR 1 H42B H 0.1617(6) -0.0937(11) 0.3442(8) 0.097 Uiso 0.60 calc PR 1 C42' C 0.1303(10) -0.0056(10) 0.2664(16) 0.072(9) Uiso 0.40 d PD 2 H42C H 0.1178(10) 0.0417(10) 0.2326(16) 0.087 Uiso 0.40 calc PR 2 H42D H 0.1647(10) 0.0055(10) 0.3246(16) 0.087 Uiso 0.40 calc PR 2 C43 C 0.1657(5) -0.0622(8) 0.2140(7) 0.114(5) Uani 1 d D . H43A H 0.2139(5) -0.0915(8) 0.2201(7) 0.136 Uiso 0.60 calc PR 1 H43B H 0.1723(5) -0.0134(8) 0.1855(7) 0.136 Uiso 0.60 calc PR 1 H43C H 0.2002(5) -0.0964(8) 0.2522(7) 0.136 Uiso 0.40 d PR 2 H43D H 0.1940(5) -0.0365(8) 0.1752(7) 0.136 Uiso 0.40 d PR 2 C44 C 0.0975(5) -0.1054(6) 0.1600(6) 0.069(3) Uani 1 d D . H44A H 0.0857(5) -0.0875(6) 0.0974(6) 0.083 Uiso 1 calc R . H44B H 0.1095(5) -0.1597(6) 0.1601(6) 0.083 Uiso 1 calc R . O50 O -0.0864(4) -0.2193(3) 0.1267(5) 0.070(2) Uani 1 d D . C51 C -0.0408(5) -0.2713(5) 0.0890(7) 0.077(3) Uani 1 d D . H51A H 0.0140(5) -0.2671(5) 0.1193(7) 0.093 Uiso 0.60 calc PR 1 H51B H -0.0451(5) -0.2608(5) 0.0246(7) 0.093 Uiso 0.60 calc PR 1 H51C H 0.0019(5) -0.2908(5) 0.1332(7) 0.093 Uiso 0.40 d PR 2 H51D H -0.0206(5) -0.2463(5) 0.0425(7) 0.093 Uiso 0.40 d PR 2 C52 C -0.0710(10) -0.3498(6) 0.1019(17) 0.101(8) Uani 0.60 d PDU 1 H52A H -0.0747(10) -0.3801(6) 0.0470(17) 0.121 Uiso 0.60 calc PR 1 H52B H -0.0368(10) -0.3758(6) 0.1520(17) 0.121 Uiso 0.60 calc PR 1 C53 C -0.1498(11) -0.3373(8) 0.1222(22) 0.107(10) Uani 0.60 d PDU 1 H53A H -0.1906(11) -0.3465(8) 0.0684(22) 0.128 Uiso 0.60 calc PR 1 H53B H -0.1581(11) -0.3713(8) 0.1705(22) 0.128 Uiso 0.60 calc PR 1 C52' C -0.0964(14) -0.3324(17) 0.0451(24) 0.143(19) Uiso 0.40 d PD 2 H52C H -0.1128(14) -0.3235(17) -0.0200(24) 0.172 Uiso 0.40 calc PR 2 H52D H -0.0722(14) -0.3826(17) 0.0549(24) 0.172 Uiso 0.40 calc PR 2 C53' C -0.1643(16) -0.3262(16) 0.0909(26) 0.104(19) Uiso 0.40 d PD 2 H53C H -0.1678(16) -0.3716(16) 0.1271(26) 0.125 Uiso 0.40 calc PR 2 H53D H -0.2129(16) -0.3208(16) 0.0460(26) 0.125 Uiso 0.40 calc PR 2 C54 C -0.1500(5) -0.2563(5) 0.1511(8) 0.078(4) Uani 1 d D . H54A H -0.1987(5) -0.2319(5) 0.1216(8) 0.094 Uiso 0.60 calc PR 1 H54B H -0.1456(5) -0.2534(5) 0.2166(8) 0.094 Uiso 0.60 calc PR 1 H54C H -0.1946(5) -0.2236(5) 0.1399(8) 0.094 Uiso 0.40 d PR 2 H54D H -0.1388(5) -0.2704(5) 0.2137(8) 0.094 Uiso 0.40 d PR 2 C60 C -0.6428(18) -0.0079(24) 0.3774(33) 0.187(14) Uani 0.50 d PDU -1 H60A H -0.6724(18) 0.0153(24) 0.3229(33) 0.281 Uiso 0.50 calc PR -1 H60B H -0.6510(18) 0.0203(24) 0.4297(33) 0.281 Uiso 0.50 calc PR -1 H60C H -0.6598(18) -0.0599(24) 0.3813(33) 0.281 Uiso 0.50 calc PR -1 C61 C -0.5589(18) -0.0069(22) 0.3749(24) 0.180(13) Uani 0.50 d PDU -1 H61A H -0.5419(18) 0.0456(22) 0.3701(24) 0.216 Uiso 0.50 calc PR -1 H61B H -0.5508(18) -0.0345(22) 0.3214(24) 0.216 Uiso 0.50 calc PR -1 C62 C -0.5112(26) -0.0425(20) 0.4577(29) 0.186(13) Uani 0.50 d PDU -1 H62A H -0.5406(26) -0.0842(20) 0.4773(29) 0.224 Uiso 0.50 calc PR -1 H62B H -0.4637(26) -0.0638(20) 0.4434(29) 0.224 Uiso 0.50 calc PR -1 C63 C -0.4900(29) 0.0136(23) 0.5324(29) 0.183(13) Uani 0.50 d PDU -1 H63A H -0.5302(29) 0.0146(23) 0.5684(29) 0.219 Uiso 0.50 calc PR -1 H63B H -0.4862(29) 0.0644(23) 0.5074(29) 0.219 Uiso 0.50 calc PR -1 C64 C -0.4132(20) -0.0085(25) 0.5911(31) 0.185(14) Uani 0.50 d PDU -1 H64A H -0.3992(20) 0.0279(25) 0.6398(31) 0.278 Uiso 0.50 calc PR -1 H64B H -0.3736(20) -0.0090(25) 0.5552(31) 0.278 Uiso 0.50 calc PR -1 H64C H -0.4175(20) -0.0586(25) 0.6161(31) 0.278 Uiso 0.50 calc PR -1 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 Cr 0.0317(7) 0.0341(8) 0.0385(8) 0.0009(7) 0.0118(6) 0.0026(7) Li 0.046(10) 0.051(10) 0.069(12) -0.008(9) 0.004(9) 0.006(8) Cl1 0.0427(13) 0.0466(15) 0.0481(14) -0.0062(12) 0.0171(11) 0.0071(11) Cl2 0.0472(13) 0.0434(14) 0.0447(14) 0.0075(11) 0.0132(11) 0.0108(11) N1 0.027(4) 0.047(5) 0.035(4) 0.002(4) 0.014(3) 0.002(3) C2 0.033(5) 0.066(7) 0.045(6) 0.002(5) 0.010(5) -0.003(5) C3 0.038(6) 0.070(7) 0.048(6) 0.000(5) 0.006(5) -0.023(5) C4 0.052(6) 0.059(7) 0.051(7) -0.007(5) 0.010(5) -0.013(5) C5 0.035(5) 0.050(6) 0.032(5) -0.002(5) -0.002(4) 0.005(5) C6 0.044(6) 0.035(5) 0.032(5) 0.000(4) 0.003(4) 0.002(5) N7 0.028(4) 0.032(4) 0.032(4) 0.004(3) 0.005(3) 0.004(3) C8 0.032(5) 0.039(5) 0.038(6) -0.002(4) 0.012(4) 0.000(4) C9 0.062(7) 0.038(6) 0.034(6) -0.006(5) 0.015(5) -0.004(5) C10 0.107(10) 0.040(6) 0.042(6) 0.001(5) 0.041(7) -0.006(6) C11 0.044(7) 0.072(8) 0.085(9) -0.012(7) 0.037(6) 0.001(6) C12 0.046(6) 0.063(7) 0.054(7) -0.011(6) 0.017(5) -0.001(5) C13 0.028(5) 0.040(5) 0.046(6) -0.013(5) 0.011(4) -0.004(4) C14 0.078(7) 0.048(6) 0.044(6) 0.005(5) 0.010(5) 0.010(5) C15 0.075(8) 0.070(7) 0.056(7) 0.001(6) 0.005(6) 0.009(6) C16 0.120(11) 0.071(8) 0.055(7) 0.021(6) 0.012(7) 0.011(7) C17 0.030(5) 0.082(8) 0.041(6) -0.013(6) 0.007(5) 0.011(5) C18 0.129(11) 0.063(8) 0.075(9) 0.021(7) 0.023(8) 0.013(8) C19 0.043(7) 0.155(13) 0.073(8) -0.001(8) -0.012(6) 0.032(7) N21 0.032(4) 0.039(5) 0.033(4) -0.004(4) 0.011(3) -0.002(3) C22 0.049(6) 0.032(5) 0.043(6) -0.004(5) 0.014(5) -0.003(5) C23 0.038(5) 0.040(6) 0.048(6) 0.024(5) 0.006(5) 0.015(5) C24 0.035(5) 0.055(6) 0.044(6) 0.005(5) 0.011(5) -0.001(5) C25 0.042(6) 0.035(5) 0.036(5) 0.000(4) 0.012(5) 0.003(4) C26 0.033(5) 0.046(6) 0.030(5) -0.002(4) 0.006(4) 0.002(4) N27 0.028(4) 0.034(4) 0.035(4) 0.001(4) 0.004(3) 0.002(3) C28 0.036(5) 0.027(5) 0.046(6) -0.006(5) 0.003(4) 0.001(4) C29 0.033(5) 0.025(5) 0.039(5) 0.000(4) 0.000(4) -0.019(4) C30 0.042(6) 0.053(7) 0.064(7) 0.005(6) 0.015(5) 0.002(5) C31 0.065(7) 0.027(5) 0.080(8) -0.001(6) 0.020(6) 0.000(5) C32 0.049(6) 0.065(8) 0.059(7) -0.021(6) 0.001(6) 0.015(6) C33 0.032(5) 0.036(6) 0.062(7) -0.008(5) 0.006(5) 0.008(4) C34 0.052(6) 0.030(5) 0.060(7) 0.000(5) 0.025(5) -0.005(4) C35 0.063(7) 0.070(7) 0.087(8) -0.023(7) 0.029(6) -0.006(6) C36 0.129(11) 0.056(7) 0.051(7) -0.005(6) 0.042(7) -0.019(7) C37 0.050(6) 0.054(6) 0.034(6) -0.016(5) -0.007(5) -0.005(5) C38 0.059(7) 0.078(8) 0.046(6) 0.005(6) 0.023(5) -0.003(6) C39 0.069(8) 0.072(8) 0.085(9) -0.029(7) 0.022(7) 0.002(6) O40 0.040(4) 0.076(5) 0.058(4) -0.009(4) 0.015(3) 0.003(3) C41 0.080(8) 0.108(10) 0.057(7) -0.040(7) 0.012(6) -0.015(8) C42 0.073(14) 0.071(14) 0.085(15) -0.005(12) -0.013(11) -0.018(11) C43 0.073(9) 0.200(17) 0.070(9) -0.037(10) 0.021(7) -0.038(10) C44 0.049(7) 0.102(9) 0.060(7) -0.026(7) 0.021(6) -0.007(6) O50 0.067(5) 0.041(4) 0.105(6) 0.000(4) 0.023(4) 0.007(4) C51 0.085(9) 0.065(8) 0.081(9) -0.005(7) 0.018(7) 0.018(7) C52 0.100(14) 0.057(12) 0.133(16) -0.026(12) -0.004(13) -0.001(11) C53 0.103(16) 0.050(12) 0.153(19) 0.007(13) -0.005(14) -0.008(11) C54 0.063(7) 0.063(8) 0.107(10) 0.002(7) 0.016(7) -0.003(6) C60 0.244(30) 0.120(19) 0.248(28) 0.102(20) 0.169(29) 0.009(24) C61 0.253(27) 0.109(18) 0.238(29) 0.085(20) 0.188(25) 0.046(20) C62 0.261(26) 0.106(21) 0.251(28) 0.082(20) 0.188(24) 0.053(21) C63 0.267(26) 0.089(19) 0.246(29) 0.103(21) 0.176(25) 0.041(20) C64 0.231(32) 0.122(21) 0.261(30) 0.115(21) 0.184(28) 0.053(23) _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 Cr N21 2.005(7) . ? Cr N1 2.011(7) . ? Cr N27 2.149(6) . ? Cr N7 2.188(6) . ? Cr Cl1 2.349(2) . ? Cr Cl2 2.354(3) . ? Cr Li 3.26(2) . ? Li O40 1.91(2) . ? Li O50 1.92(2) . ? Li Cl2 2.31(2) . ? Li Cl1 2.35(2) . ? N1 C2 1.341(10) . ? N1 C5 1.371(10) . ? C2 C3 1.381(12) . ? C3 C4 1.384(12) . ? C4 C5 1.405(12) . ? C5 C6 1.394(11) . ? C6 N7 1.286(9) . ? N7 C8 1.451(9) . ? C8 C9 1.384(11) . ? C8 C13 1.418(11) . ? C9 C10 1.433(12) . ? C9 C14 1.520(12) . ? C10 C11 1.361(13) . ? C11 C12 1.331(13) . ? C12 C13 1.423(11) . ? C13 C17 1.494(12) . ? C14 C16 1.510(12) . ? C14 C15 1.514(12) . ? C17 C18 1.524(14) . ? C17 C19 1.539(12) . ? N21 C22 1.348(10) . ? N21 C25 1.380(10) . ? C22 C23 1.394(11) . ? C23 C24 1.374(11) . ? C24 C25 1.384(11) . ? C25 C26 1.425(11) . ? C26 N27 1.287(9) . ? N27 C28 1.467(10) . ? C28 C29 1.406(11) . ? C28 C33 1.415(11) . ? C29 C30 1.387(12) . ? C29 C34 1.504(11) . ? C30 C31 1.368(12) . ? C31 C32 1.365(13) . ? C32 C33 1.396(13) . ? C33 C37 1.522(12) . ? C34 C36 1.498(12) . ? C34 C35 1.529(12) . ? C37 C38 1.509(11) . ? C37 C39 1.517(12) . ? O40 C44 1.420(7) . ? O40 C41 1.424(7) . ? C41 C42 1.509(9) . ? C41 C42' 1.519(10) . ? C42 C43 1.497(9) . ? C42' C43 1.490(10) . ? C43 C44 1.511(8) . ? O50 C54 1.411(7) . ? O50 C51 1.415(7) . ? C51 C52 1.510(9) . ? C51 C52' 1.513(10) . ? C52 C53 1.498(9) . ? C53 C54 1.495(9) . ? C52' C53' 1.506(10) . ? C53' C54 1.522(10) . ? C60 C61 1.486(10) . ? C61 C62 1.494(10) . ? C62 C63 1.491(10) . ? C63 C64 1.505(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Cr N1 88.7(3) . . ? N21 Cr N27 78.8(3) . . ? N1 Cr N27 166.6(3) . . ? N21 Cr N7 88.5(2) . . ? N1 Cr N7 78.5(3) . . ? N27 Cr N7 105.5(2) . . ? N21 Cr Cl1 93.2(2) . . ? N1 Cr Cl1 88.4(2) . . ? N27 Cr Cl1 87.7(2) . . ? N7 Cr Cl1 166.7(2) . . ? N21 Cr Cl2 172.2(2) . . ? N1 Cr Cl2 98.6(2) . . ? N27 Cr Cl2 94.2(2) . . ? N7 Cr Cl2 90.2(2) . . ? Cl1 Cr Cl2 89.87(9) . . ? N21 Cr Li 139.0(4) . . ? N1 Cr Li 85.7(4) . . ? N27 Cr Li 100.7(3) . . ? N7 Cr Li 129.6(3) . . ? Cl1 Cr Li 46.2(3) . . ? Cl2 Cr Li 45.2(3) . . ? O40 Li O50 108.6(8) . . ? O40 Li Cl2 112.2(8) . . ? O50 Li Cl2 114.7(8) . . ? O40 Li Cl1 119.0(8) . . ? O50 Li Cl1 110.9(8) . . ? Cl2 Li Cl1 90.7(6) . . ? O40 Li Cr 118.4(7) . . ? O50 Li Cr 133.0(7) . . ? Cl2 Li Cr 46.2(3) . . ? Cl1 Li Cr 46.1(3) . . ? Cr Cl1 Li 87.8(4) . . ? Li Cl2 Cr 88.6(4) . . ? C2 N1 C5 106.3(7) . . ? C2 N1 Cr 137.8(6) . . ? C5 N1 Cr 113.9(5) . . ? N1 C2 C3 111.3(8) . . ? C2 C3 C4 106.8(8) . . ? C3 C4 C5 106.0(8) . . ? N1 C5 C6 116.0(8) . . ? N1 C5 C4 109.6(8) . . ? C6 C5 C4 134.4(9) . . ? N7 C6 C5 120.9(8) . . ? C6 N7 C8 116.0(7) . . ? C6 N7 Cr 109.0(5) . . ? C8 N7 Cr 134.9(5) . . ? C9 C8 C13 123.4(8) . . ? C9 C8 N7 119.2(7) . . ? C13 C8 N7 117.2(7) . . ? C8 C9 C10 116.4(8) . . ? C8 C9 C14 123.1(8) . . ? C10 C9 C14 120.2(8) . . ? C11 C10 C9 121.3(9) . . ? C12 C11 C10 120.6(9) . . ? C11 C12 C13 123.1(9) . . ? C8 C13 C12 115.1(8) . . ? C8 C13 C17 123.4(7) . . ? C12 C13 C17 121.0(8) . . ? C16 C14 C15 109.2(8) . . ? C16 C14 C9 114.5(9) . . ? C15 C14 C9 110.8(8) . . ? C13 C17 C18 111.3(8) . . ? C13 C17 C19 113.5(8) . . ? C18 C17 C19 110.8(9) . . ? C22 N21 C25 105.5(7) . . ? C22 N21 Cr 139.1(6) . . ? C25 N21 Cr 115.2(5) . . ? N21 C22 C23 111.2(8) . . ? C24 C23 C22 106.0(8) . . ? C23 C24 C25 107.3(8) . . ? N21 C25 C24 109.9(7) . . ? N21 C25 C26 115.0(8) . . ? C24 C25 C26 135.1(9) . . ? N27 C26 C25 119.1(8) . . ? C26 N27 C28 115.5(7) . . ? C26 N27 Cr 111.8(5) . . ? C28 N27 Cr 130.7(5) . . ? C29 C28 C33 121.8(8) . . ? C29 C28 N27 120.3(7) . . ? C33 C28 N27 117.9(8) . . ? C30 C29 C28 117.6(8) . . ? C30 C29 C34 120.8(8) . . ? C28 C29 C34 121.2(7) . . ? C31 C30 C29 121.8(9) . . ? C32 C31 C30 120.0(9) . . ? C31 C32 C33 122.3(9) . . ? C32 C33 C28 116.5(9) . . ? C32 C33 C37 117.7(8) . . ? C28 C33 C37 125.7(8) . . ? C36 C34 C29 113.3(7) . . ? C36 C34 C35 111.4(8) . . ? C29 C34 C35 108.6(8) . . ? C38 C37 C39 110.1(8) . . ? C38 C37 C33 110.1(7) . . ? C39 C37 C33 112.3(8) . . ? C44 O40 C41 109.1(5) . . ? C44 O40 Li 124.9(7) . . ? C41 O40 Li 124.3(7) . . ? O40 C41 C42 106.7(7) . . ? O40 C41 C42' 106.4(8) . . ? C43 C42 C41 102.3(7) . . ? C43 C42' C41 102.2(8) . . ? C42' C43 C44 104.6(8) . . ? C42 C43 C44 103.8(7) . . ? O40 C44 C43 107.4(6) . . ? C54 O50 C51 110.8(6) . . ? C54 O50 Li 119.8(7) . . ? C51 O50 Li 129.4(7) . . ? O50 C51 C52 107.2(7) . . ? O50 C51 C52' 105.6(9) . . ? C53 C52 C51 105.0(8) . . ? C54 C53 C52 105.0(8) . . ? C53' C52' C51 104.4(9) . . ? C52' C53' C54 106.7(9) . . ? O50 C54 C53 108.3(7) . . ? O50 C54 C53' 104.9(8) . . ? C60 C61 C62 111.1(15) . . ? C63 C62 C61 111.5(15) . . ? C62 C63 C64 109.2(15) . . ? _refine_diff_density_max 0.329 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.065 data_Compound 3a _database_code_CSD 185876 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H45 N4 Cr' _chemical_formula_weight 573.75 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 20.280(2) _cell_length_b 34.103(4) _cell_length_c 9.4200(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6515.1(15) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 4.78 _cell_measurement_theta_max 12.47 _exptl_crystal_description blocks _exptl_crystal_colour Green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method ? _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10.03 _diffrn_reflns_number 1530 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1530 _reflns_number_observed 1193 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0362P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(6) _refine_ls_number_reflns 1530 _refine_ls_number_parameters 182 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_obs 0.0488 _refine_ls_wR_factor_all 0.1068 _refine_ls_wR_factor_obs 0.0938 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.048 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.0000 0.0000 0.41105(12) 0.0307(3) Uani 1 d S . C C 0.0000 0.0000 0.1948(10) 0.064(3) Uani 1 d S . H0A H 0.0085 -0.0263 0.1605(10) 0.096 Uiso 0.50 d PR . H0B H 0.0341 0.0176 0.1605(10) 0.096 Uiso 0.50 d PR . H0C H -0.0426 0.0088 0.1605(10) 0.096 Uiso 0.50 d PR . N1 N -0.0735(2) 0.04011(13) 0.4238(7) 0.0383(12) Uani 1 d . . C2 C -0.1396(3) 0.0439(2) 0.4124(9) 0.0450(14) Uani 1 d . . H2A H -0.1690(3) 0.0229(2) 0.4009(9) 0.054 Uiso 1 calc R . C3 C -0.1582(3) 0.0829(2) 0.4198(11) 0.053(2) Uani 1 d . . H3A H -0.2014(3) 0.0927(2) 0.4142(11) 0.064 Uiso 1 calc R . C4 C -0.1008(3) 0.1050(2) 0.4372(8) 0.048(2) Uani 1 d . . H4A H -0.0975(3) 0.1324(2) 0.4467(8) 0.058 Uiso 1 calc R . C5 C -0.0491(3) 0.0778(2) 0.4376(8) 0.0377(13) Uani 1 d . . C6 C 0.0195(3) 0.0816(2) 0.4563(7) 0.0392(14) Uani 1 d . . H6A H 0.0388(3) 0.1063(2) 0.4722(7) 0.047 Uiso 1 calc R . N7 N 0.0560(2) 0.04964(13) 0.4507(5) 0.0308(11) Uani 1 d . . C8 C 0.1244(3) 0.0524(2) 0.4904(7) 0.0329(12) Uani 1 d . . C9 C 0.1702(3) 0.0692(2) 0.3983(8) 0.0414(15) Uani 1 d . . C10 C 0.2356(3) 0.0707(2) 0.4438(8) 0.049(2) Uani 1 d . . H10A H 0.2673(3) 0.0824(2) 0.3846(8) 0.058 Uiso 1 calc R . C11 C 0.2553(3) 0.0555(2) 0.5724(8) 0.054(2) Uani 1 d . . H11A H 0.2998(3) 0.0566(2) 0.5996(8) 0.065 Uiso 1 calc R . C12 C 0.2090(3) 0.0388(2) 0.6613(9) 0.0456(13) Uani 1 d . . H12A H 0.2222(3) 0.0289(2) 0.7499(9) 0.055 Uiso 1 calc R . C13 C 0.1430(3) 0.0363(2) 0.6213(6) 0.0376(14) Uani 1 d . . C14 C 0.1523(3) 0.0852(2) 0.2522(9) 0.059(2) Uani 1 d . . H14A H 0.1043(3) 0.0816(2) 0.2380(9) 0.070 Uiso 1 calc R . C15 C 0.1677(5) 0.1294(3) 0.2440(15) 0.109(4) Uani 1 d . . H15A H 0.1441(5) 0.1431(3) 0.3185(15) 0.163 Uiso 1 calc R . H15B H 0.1540(5) 0.1395(3) 0.1523(15) 0.163 Uiso 1 calc R . H15C H 0.2147(5) 0.1335(3) 0.2559(15) 0.163 Uiso 1 calc R . C16 C 0.1883(5) 0.0625(4) 0.1373(10) 0.101(4) Uani 1 d . . H16A H 0.1764(5) 0.0730(4) 0.0450(10) 0.152 Uiso 1 calc R . H16B H 0.1760(5) 0.0351(4) 0.1421(10) 0.152 Uiso 1 calc R . H16C H 0.2355(5) 0.0651(4) 0.1512(10) 0.152 Uiso 1 calc R . C17 C 0.0920(3) 0.0192(2) 0.7222(7) 0.0427(14) Uani 1 d . . H17A H 0.0554(3) 0.0088(2) 0.6637(7) 0.051 Uiso 1 calc R . C18 C 0.0635(4) 0.0516(2) 0.8168(9) 0.064(2) Uani 1 d . . H18A H 0.0468(4) 0.0727(2) 0.7577(9) 0.096 Uiso 1 calc R . H18B H 0.0977(4) 0.0616(2) 0.8788(9) 0.096 Uiso 1 calc R . H18C H 0.0278(4) 0.0410(2) 0.8736(9) 0.096 Uiso 1 calc R . C19 C 0.1186(4) -0.0144(2) 0.8099(11) 0.074(2) Uani 1 d . . H19A H 0.0841(4) -0.0241(2) 0.8721(11) 0.111 Uiso 1 calc R . H19B H 0.1555(4) -0.0053(2) 0.8665(11) 0.111 Uiso 1 calc R . H19C H 0.1331(4) -0.0353(2) 0.7475(11) 0.111 Uiso 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 Cr 0.0248(5) 0.0287(5) 0.0386(6) 0.000 0.000 -0.0013(6) C 0.064(6) 0.086(7) 0.041(5) 0.000 0.000 -0.011(6) N1 0.027(2) 0.034(2) 0.054(3) 0.010(3) -0.003(3) -0.002(2) C2 0.025(2) 0.040(3) 0.070(4) 0.014(4) -0.007(3) -0.002(2) C3 0.026(3) 0.046(3) 0.088(5) 0.030(4) -0.003(4) 0.010(3) C4 0.041(3) 0.032(3) 0.072(5) 0.016(3) -0.003(3) 0.007(2) C5 0.037(3) 0.030(3) 0.046(4) 0.007(3) -0.004(3) 0.000(2) C6 0.039(3) 0.028(2) 0.051(4) 0.004(3) -0.009(3) -0.001(2) N7 0.023(2) 0.028(2) 0.041(3) -0.001(2) -0.003(2) -0.002(2) C8 0.028(3) 0.029(2) 0.042(3) -0.006(2) -0.003(2) 0.001(2) C9 0.035(3) 0.036(3) 0.053(4) 0.006(3) -0.001(3) 0.002(2) C10 0.030(3) 0.047(3) 0.068(5) -0.003(3) 0.002(3) -0.005(2) C11 0.031(3) 0.060(4) 0.071(5) -0.007(4) -0.017(3) 0.001(3) C12 0.036(3) 0.051(3) 0.050(3) 0.002(4) -0.011(3) 0.004(2) C13 0.036(3) 0.031(3) 0.046(4) -0.004(2) -0.006(2) 0.002(2) C14 0.033(3) 0.078(5) 0.065(5) 0.029(4) 0.005(3) 0.002(3) C15 0.092(7) 0.085(6) 0.149(11) 0.077(7) -0.001(7) -0.005(6) C16 0.072(6) 0.179(12) 0.052(6) 0.000(7) -0.004(5) 0.008(7) C17 0.042(3) 0.044(3) 0.042(3) 0.010(3) -0.008(3) -0.002(3) C18 0.072(5) 0.071(5) 0.049(4) 0.008(4) 0.006(4) 0.003(4) C19 0.068(5) 0.073(5) 0.082(6) 0.035(5) -0.005(5) 0.000(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 Cr N1 2.026(5) 2 ? Cr N1 2.026(5) . ? Cr C 2.037(9) . ? Cr N7 2.073(4) 2 ? Cr N7 2.073(4) . ? N1 C2 1.351(7) . ? N1 C5 1.382(7) . ? C2 C3 1.384(9) . ? C3 C4 1.396(9) . ? C4 C5 1.399(8) . ? C5 C6 1.410(8) . ? C6 N7 1.318(7) . ? N7 C8 1.440(7) . ? C8 C9 1.394(9) . ? C8 C13 1.401(8) . ? C9 C10 1.395(8) . ? C9 C14 1.523(11) . ? C10 C11 1.376(11) . ? C11 C12 1.382(10) . ? C12 C13 1.393(8) . ? C13 C17 1.521(9) . ? C14 C16 1.517(13) . ? C14 C15 1.544(12) . ? C17 C19 1.511(9) . ? C17 C18 1.534(11) . ? 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 Cr N1 173.2(4) 2 . ? N1 Cr C 93.4(2) 2 . ? N1 Cr C 93.4(2) . . ? N1 Cr N7 80.9(2) 2 2 ? N1 Cr N7 97.9(2) . 2 ? C Cr N7 100.39(14) . 2 ? N1 Cr N7 97.9(2) 2 . ? N1 Cr N7 80.9(2) . . ? C Cr N7 100.39(14) . . ? N7 Cr N7 159.2(3) 2 . ? C2 N1 C5 105.8(5) . . ? C2 N1 Cr 142.2(4) . . ? C5 N1 Cr 111.7(4) . . ? N1 C2 C3 111.0(5) . . ? C2 C3 C4 107.2(5) . . ? C3 C4 C5 105.5(5) . . ? N1 C5 C4 110.4(5) . . ? N1 C5 C6 116.8(5) . . ? C4 C5 C6 132.7(6) . . ? N7 C6 C5 118.3(5) . . ? C6 N7 C8 118.5(5) . . ? C6 N7 Cr 112.0(4) . . ? C8 N7 Cr 128.9(4) . . ? C9 C8 C13 122.0(5) . . ? C9 C8 N7 120.4(6) . . ? C13 C8 N7 117.5(5) . . ? C8 C9 C10 117.2(6) . . ? C8 C9 C14 123.4(6) . . ? C10 C9 C14 119.5(6) . . ? C11 C10 C9 122.2(6) . . ? C10 C11 C12 119.5(6) . . ? C11 C12 C13 120.9(7) . . ? C12 C13 C8 118.2(6) . . ? C12 C13 C17 120.5(6) . . ? C8 C13 C17 121.2(5) . . ? C16 C14 C9 110.4(6) . . ? C16 C14 C15 111.3(8) . . ? C9 C14 C15 110.3(8) . . ? C19 C17 C13 113.0(6) . . ? C19 C17 C18 111.3(6) . . ? C13 C17 C18 110.0(5) . . ? _refine_diff_density_max 0.231 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.055 data_Compound 3b _database_code_CSD 185877 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H47 N4 Cr' _chemical_formula_weight 587.78 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 19.820(4) _cell_length_b 34.304(9) _cell_length_c 9.969(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6778.0(28) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 4.75 _cell_measurement_theta_max 12.52 _exptl_crystal_description prisms _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method ? _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 11.20 _diffrn_reflns_number 1576 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1122 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1576 _reflns_number_observed 1064 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 70 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.2140P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(13) _refine_ls_number_reflns 1506 _refine_ls_number_parameters 183 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1557 _refine_ls_R_factor_obs 0.0989 _refine_ls_wR_factor_all 0.3273 _refine_ls_wR_factor_obs 0.2562 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.048 _refine_ls_restrained_S_all 1.084 _refine_ls_restrained_S_obs 1.047 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr -0.2500 0.2500 0.4925(2) 0.0290(7) Uani 1 d S . N1 N -0.3284(5) 0.2109(3) 0.5031(15) 0.039(2) Uani 1 d . . C2 C -0.3933(7) 0.2074(4) 0.4876(20) 0.050(4) Uani 1 d . . H2A H -0.4228(7) 0.2286(4) 0.4756(20) 0.060 Uiso 1 calc R . C3 C -0.4136(6) 0.1690(4) 0.4910(25) 0.054(4) Uani 1 d . . H3A H -0.4580(6) 0.1597(4) 0.4841(25) 0.065 Uiso 1 calc R . C4 C -0.3556(7) 0.1467(4) 0.5067(22) 0.052(4) Uani 1 d . . H4A H -0.3533(7) 0.1193(4) 0.5105(22) 0.062 Uiso 1 calc R . C5 C -0.3017(6) 0.1726(4) 0.5157(16) 0.039(3) Uani 1 d . . C6 C -0.2306(7) 0.1691(4) 0.5318(17) 0.043(3) Uani 1 d . . H6A H -0.2103(7) 0.1446(4) 0.5454(17) 0.051 Uiso 1 calc R . N7 N -0.1955(6) 0.1999(3) 0.5273(11) 0.034(2) Uani 1 d . . C8 C -0.1256(6) 0.1967(4) 0.5632(15) 0.035(3) Uani 1 d . . C9 C -0.0762(7) 0.1799(4) 0.4768(19) 0.047(4) Uani 1 d . . C10 C -0.0112(7) 0.1778(5) 0.5126(22) 0.057(4) Uani 1 d . . H10A H 0.0202(7) 0.1661(5) 0.4547(22) 0.068 Uiso 1 calc R . C11 C 0.0103(8) 0.1930(5) 0.6366(23) 0.063(5) Uani 1 d . . H11A H 0.0559(8) 0.1924(5) 0.6619(23) 0.075 Uiso 1 calc R . C12 C -0.0375(7) 0.2087(5) 0.7185(18) 0.051(4) Uani 1 d . . H12A H -0.0231(7) 0.2180(5) 0.8024(18) 0.062 Uiso 1 calc R . C13 C -0.1051(7) 0.2121(4) 0.6889(15) 0.039(3) Uani 1 d . . C14 C -0.0962(9) 0.1646(7) 0.3384(22) 0.070(6) Uani 1 d . . H14A H -0.1458(9) 0.1672(7) 0.3339(22) 0.085 Uiso 1 calc R . C15 C -0.0822(13) 0.1219(9) 0.3180(40) 0.128(14) Uani 1 d . . H15A H -0.1006(13) 0.1072(9) 0.3926(40) 0.192 Uiso 1 calc R . H15B H -0.0338(13) 0.1176(9) 0.3131(40) 0.192 Uiso 1 calc R . H15C H -0.1031(13) 0.1132(9) 0.2352(40) 0.192 Uiso 1 calc R . C16 C -0.0689(17) 0.1900(11) 0.2256(31) 0.132(13) Uani 1 d . . H16A H -0.0794(17) 0.2171(11) 0.2440(31) 0.198 Uiso 1 calc R . H16B H -0.0896(17) 0.1824(11) 0.1414(31) 0.198 Uiso 1 calc R . H16C H -0.0204(17) 0.1868(11) 0.2193(31) 0.198 Uiso 1 calc R . C17 C -0.1548(9) 0.2295(5) 0.7863(18) 0.057(4) Uani 1 d . . H17A H -0.1937(9) 0.2387(5) 0.7324(18) 0.069 Uiso 1 calc R . C18 C -0.1817(11) 0.1978(7) 0.8792(24) 0.078(6) Uani 1 d . . H18A H -0.2136(11) 0.2091(7) 0.9418(24) 0.117 Uiso 1 calc R . H18B H -0.1445(11) 0.1863(7) 0.9284(24) 0.117 Uiso 1 calc R . H18C H -0.2040(11) 0.1779(7) 0.8264(24) 0.117 Uiso 1 calc R . C19 C -0.1271(13) 0.2657(8) 0.8611(29) 0.097(8) Uani 1 d . . H19A H -0.1612(13) 0.2755(8) 0.9220(29) 0.146 Uiso 1 calc R . H19B H -0.1155(13) 0.2857(8) 0.7966(29) 0.146 Uiso 1 calc R . H19C H -0.0872(13) 0.2584(8) 0.9116(29) 0.146 Uiso 1 calc R . C20 C -0.2500 0.2500 0.2903(24) 0.054(5) Uiso 1 d S . H20A H -0.2751 0.2725 0.2627(24) 0.064 Uiso 0.50 d PR . H20B H -0.2042 0.2543 0.2627(24) 0.064 Uiso 0.50 d PR . C21 C -0.2741(23) 0.2208(14) 0.2120(49) 0.082(12) Uiso 0.50 d P . H21A H -0.2696(23) 0.2267(14) 0.1183(49) 0.122 Uiso 0.50 d PR . H21B H -0.3208(23) 0.2165(14) 0.2329(49) 0.122 Uiso 0.50 d PR . H21C H -0.2486(23) 0.1979(14) 0.2329(49) 0.122 Uiso 0.50 d PR . 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 Cr 0.0214(10) 0.0311(12) 0.0344(13) 0.000 0.000 0.0020(13) N1 0.028(5) 0.040(5) 0.049(7) -0.012(6) -0.004(6) -0.007(4) C2 0.038(7) 0.044(7) 0.067(10) -0.025(9) 0.004(8) 0.004(6) C3 0.009(5) 0.052(8) 0.100(13) -0.022(10) -0.002(8) 0.002(5) C4 0.034(7) 0.035(6) 0.086(12) -0.008(9) 0.000(9) -0.013(5) C5 0.026(6) 0.046(7) 0.046(8) -0.013(7) 0.001(6) -0.008(5) C6 0.031(6) 0.037(6) 0.061(10) -0.017(6) 0.003(6) 0.002(5) N7 0.039(6) 0.030(5) 0.034(6) -0.007(5) -0.002(5) 0.006(5) C8 0.028(6) 0.029(6) 0.047(8) 0.013(6) 0.000(6) -0.013(5) C9 0.030(7) 0.052(8) 0.059(10) -0.011(8) 0.007(7) 0.005(6) C10 0.030(7) 0.055(8) 0.084(12) 0.003(9) 0.011(8) 0.013(6) C11 0.041(8) 0.064(10) 0.083(12) 0.015(10) -0.015(9) 0.003(8) C12 0.027(7) 0.068(9) 0.059(11) 0.008(8) -0.006(6) -0.003(6) C13 0.036(7) 0.036(6) 0.045(7) 0.009(6) 0.001(6) 0.004(5) C14 0.039(8) 0.090(14) 0.082(14) -0.038(12) 0.003(8) 0.009(9) C15 0.081(15) 0.116(20) 0.187(33) -0.112(23) 0.002(18) -0.011(15) C16 0.134(25) 0.194(35) 0.067(17) -0.007(20) -0.002(17) -0.067(24) C17 0.063(9) 0.053(9) 0.056(10) -0.017(8) -0.013(8) 0.006(7) C18 0.076(13) 0.091(14) 0.068(13) 0.031(12) 0.026(11) 0.022(11) C19 0.085(15) 0.112(19) 0.095(17) -0.053(16) 0.015(14) -0.016(14) _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 Cr C20 2.02(2) . ? Cr N1 2.054(10) . ? Cr N1 2.054(10) 14_455 ? Cr N7 2.059(10) 14_455 ? Cr N7 2.058(10) . ? N1 C2 1.30(2) . ? N1 C5 1.42(2) . ? C2 C3 1.38(2) . ? C3 C4 1.39(2) . ? C4 C5 1.39(2) . ? C5 C6 1.42(2) . ? C6 N7 1.27(2) . ? N7 C8 1.44(2) . ? C8 C13 1.42(2) . ? C8 C9 1.43(2) . ? C9 C10 1.34(2) . ? C9 C14 1.53(3) . ? C10 C11 1.41(3) . ? C11 C12 1.36(3) . ? C12 C13 1.38(2) . ? C13 C17 1.51(2) . ? C14 C15 1.51(4) . ? C14 C16 1.52(4) . ? C17 C18 1.52(3) . ? C17 C19 1.55(3) . ? C20 C21 1.36(5) . ? C20 C21 1.36(5) 14_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Cr N1 92.9(4) . . ? C20 Cr N1 92.9(4) . 14_455 ? N1 Cr N1 174.1(8) . 14_455 ? C20 Cr N7 99.7(3) . 14_455 ? N1 Cr N7 98.0(5) . 14_455 ? N1 Cr N7 81.0(5) 14_455 14_455 ? C20 Cr N7 99.7(3) . . ? N1 Cr N7 81.0(5) . . ? N1 Cr N7 98.0(5) 14_455 . ? N7 Cr N7 160.6(6) 14_455 . ? C2 N1 C5 107.0(11) . . ? C2 N1 Cr 143.3(11) . . ? C5 N1 Cr 109.1(8) . . ? N1 C2 C3 111.9(13) . . ? C2 C3 C4 106.8(11) . . ? C3 C4 C5 106.9(12) . . ? C4 C5 C6 135.5(13) . . ? C4 C5 N1 107.4(11) . . ? C6 C5 N1 117.1(11) . . ? N7 C6 C5 118.0(13) . . ? C6 N7 C8 117.1(11) . . ? C6 N7 Cr 114.5(9) . . ? C8 N7 Cr 127.8(8) . . ? C13 C8 C9 119.2(12) . . ? C13 C8 N7 117.9(12) . . ? C9 C8 N7 122.9(13) . . ? C10 C9 C8 121.4(17) . . ? C10 C9 C14 118.1(15) . . ? C8 C9 C14 120.5(13) . . ? C9 C10 C11 120.3(16) . . ? C12 C11 C10 117.6(15) . . ? C11 C12 C13 125.6(17) . . ? C12 C13 C8 115.8(14) . . ? C12 C13 C17 122.1(15) . . ? C8 C13 C17 122.0(13) . . ? C15 C14 C16 113.2(24) . . ? C15 C14 C9 114.1(23) . . ? C16 C14 C9 112.2(19) . . ? C13 C17 C18 109.6(14) . . ? C13 C17 C19 113.4(17) . . ? C18 C17 C19 113.8(20) . . ? C21 C20 C21 109.8(45) . 14_455 ? C21 C20 Cr 125.1(22) . . ? C21 C20 Cr 125.1(22) 14_455 . ? _refine_diff_density_max 0.949 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.137