# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_klat354s _database_code_depnum_ccdc_archive 'CCDC 698322' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 Cr N3, 0.375(C5 H12)' _chemical_formula_sum 'C31.88 H42.50 Cr N3' _chemical_formula_weight 519.69 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 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 11.960(6) _cell_length_b 14.191(7) _cell_length_c 16.977(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.191(5) _cell_angle_gamma 90.00 _cell_volume 2859(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 922 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 28.15 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1115 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9010 _exptl_absorpt_correction_T_max 0.9729 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 24123 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4952 _reflns_number_gt 3710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+12.5870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4952 _refine_ls_number_parameters 337 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.1978 _refine_ls_wR_factor_gt 0.1815 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.078 _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 Cr Cr 0.20164(6) 0.17499(6) 0.17980(5) 0.0257(2) Uani 1 1 d . . . N1 N 0.0320(3) 0.1563(3) 0.1492(2) 0.0257(9) Uani 1 1 d . . . N2 N 0.2134(3) 0.2218(3) 0.0622(2) 0.0259(9) Uani 1 1 d . . . N3 N 0.3751(3) 0.1347(3) 0.1911(2) 0.0288(10) Uani 1 1 d . . . C1 C 0.2201(4) 0.2998(4) 0.2439(3) 0.0277(11) Uani 1 1 d D . . H1A H 0.165(3) 0.346(3) 0.221(3) 0.033 Uiso 1 1 d D . . H1B H 0.293(3) 0.322(4) 0.232(3) 0.033 Uiso 1 1 d D . . C2 C 0.2162(5) 0.2806(4) 0.3311(3) 0.0319(12) Uani 1 1 d D . . H2A H 0.138(2) 0.278(4) 0.342(3) 0.038 Uiso 1 1 d D . . H2B H 0.251(4) 0.332(3) 0.364(3) 0.038 Uiso 1 1 d D . . C3 C 0.2682(5) 0.1869(4) 0.3517(3) 0.0325(12) Uani 1 1 d D . . H3A H 0.262(5) 0.167(4) 0.4065(17) 0.039 Uiso 1 1 d D . . H3B H 0.347(2) 0.195(4) 0.343(3) 0.039 Uiso 1 1 d D . . C4 C 0.2099(5) 0.1134(4) 0.2942(3) 0.0328(12) Uani 1 1 d D . . H4A H 0.132(2) 0.104(4) 0.304(3) 0.039 Uiso 1 1 d D . . H4B H 0.242(4) 0.050(2) 0.300(3) 0.039 Uiso 1 1 d D . . C5 C -0.0227(5) 0.0006(4) 0.1894(3) 0.0379(14) Uani 1 1 d . . . C6 C -0.0754(5) -0.0575(5) 0.2385(4) 0.0479(16) Uani 1 1 d . . . H6A H -0.0757 -0.1223 0.2302 0.058 Uiso 1 1 calc R . . C7 C -0.1277(5) -0.0211(5) 0.2995(4) 0.0496(17) Uani 1 1 d . . . H7A H -0.1603 -0.0610 0.3337 0.059 Uiso 1 1 calc R . . C8 C -0.1312(4) 0.0760(5) 0.3095(3) 0.0419(15) Uani 1 1 d . . . H8A H -0.1670 0.1008 0.3504 0.050 Uiso 1 1 calc R . . C9 C -0.0827(4) 0.1365(4) 0.2598(3) 0.0329(12) Uani 1 1 d . . . C10 C -0.0264(4) 0.0982(4) 0.2004(3) 0.0279(11) Uani 1 1 d . . . C11 C 0.0376(6) -0.0407(5) 0.1252(4) 0.0561(18) Uani 1 1 d . . . H11A H 0.0269 -0.1077 0.1236 0.084 Uiso 1 1 calc R . . H11B H 0.1166 -0.0268 0.1360 0.084 Uiso 1 1 calc R . . H11C H 0.0080 -0.0139 0.0750 0.084 Uiso 1 1 calc R . . C12 C -0.0906(4) 0.2415(4) 0.2705(3) 0.0368(13) Uani 1 1 d . . . H12A H -0.0285 0.2716 0.2499 0.055 Uiso 1 1 calc R . . H12B H -0.0883 0.2558 0.3259 0.055 Uiso 1 1 calc R . . H12C H -0.1601 0.2640 0.2424 0.055 Uiso 1 1 calc R . . C13 C -0.1550(4) 0.1670(5) 0.0701(3) 0.0421(15) Uani 1 1 d . . . H13A H -0.1894 0.1954 0.1124 0.063 Uiso 1 1 calc R . . H13B H -0.1680 0.1002 0.0698 0.063 Uiso 1 1 calc R . . H13C H -0.1872 0.1934 0.0203 0.063 Uiso 1 1 calc R . . C14 C -0.0296(4) 0.1860(4) 0.0823(3) 0.0289(12) Uani 1 1 d . . . C15 C 0.0139(4) 0.2310(4) 0.0210(3) 0.0297(12) Uani 1 1 d . . . H15A H -0.0393 0.2567 -0.0177 0.036 Uiso 1 1 calc R . . C16 C 0.1262(4) 0.2438(4) 0.0084(3) 0.0278(11) Uani 1 1 d . . . C17 C 0.1466(4) 0.2806(4) -0.0717(3) 0.0341(13) Uani 1 1 d . . . H17A H 0.1960 0.3341 -0.0649 0.051 Uiso 1 1 calc R . . H17B H 0.0761 0.2990 -0.1010 0.051 Uiso 1 1 calc R . . H17C H 0.1806 0.2321 -0.1002 0.051 Uiso 1 1 calc R . . C18 C 0.3815(4) 0.3177(5) 0.0467(3) 0.0375(14) Uani 1 1 d . . . C19 C 0.4905(5) 0.3215(6) 0.0252(3) 0.055(2) Uani 1 1 d . . . H19A H 0.5305 0.3777 0.0312 0.067 Uiso 1 1 calc R . . C20 C 0.5391(6) 0.2448(8) -0.0042(4) 0.069(3) Uani 1 1 d . . . H20A H 0.6125 0.2485 -0.0167 0.082 Uiso 1 1 calc R . . C21 C 0.4817(6) 0.1637(7) -0.0151(3) 0.064(2) Uani 1 1 d . . . H21A H 0.5160 0.1123 -0.0362 0.077 Uiso 1 1 calc R . . C22 C 0.3712(5) 0.1537(5) 0.0041(3) 0.0462(17) Uani 1 1 d . . . C23 C 0.3233(4) 0.2326(4) 0.0369(3) 0.0330(13) Uani 1 1 d . . . C24 C 0.3327(5) 0.4049(5) 0.0794(3) 0.0416(14) Uani 1 1 d . . . H24A H 0.2596 0.3909 0.0942 0.062 Uiso 1 1 calc R . . H24B H 0.3259 0.4534 0.0396 0.062 Uiso 1 1 calc R . . H24C H 0.3814 0.4262 0.1252 0.062 Uiso 1 1 calc R . . C25 C 0.3059(6) 0.0655(5) -0.0123(3) 0.0552(19) Uani 1 1 d . . . H25A H 0.2727 0.0474 0.0340 0.083 Uiso 1 1 calc R . . H25B H 0.3552 0.0164 -0.0260 0.083 Uiso 1 1 calc R . . H25C H 0.2475 0.0756 -0.0557 0.083 Uiso 1 1 calc R . . C26 C 0.4643(4) 0.1931(4) 0.1992(3) 0.0280(12) Uani 1 1 d . . . H26A H 0.4523 0.2576 0.2030 0.034 Uiso 1 1 calc R . . C27 C 0.5730(5) 0.1599(4) 0.2020(3) 0.0368(14) Uani 1 1 d . . . H27A H 0.6336 0.2015 0.2084 0.044 Uiso 1 1 calc R . . C28 C 0.5909(5) 0.0647(5) 0.1952(3) 0.0413(15) Uani 1 1 d . . . H28A H 0.6636 0.0412 0.1959 0.050 Uiso 1 1 calc R . . C29 C 0.5012(5) 0.0054(4) 0.1874(3) 0.0397(14) Uani 1 1 d . . . H29A H 0.5116 -0.0592 0.1827 0.048 Uiso 1 1 calc R . . C30 C 0.3951(5) 0.0420(4) 0.1867(3) 0.0341(13) Uani 1 1 d . . . H30A H 0.3343 0.0007 0.1830 0.041 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 Cr 0.0211(4) 0.0349(5) 0.0199(4) -0.0033(4) -0.0025(3) 0.0057(4) N1 0.024(2) 0.033(2) 0.020(2) -0.0067(18) -0.0004(17) 0.0100(18) N2 0.020(2) 0.039(3) 0.019(2) -0.0064(18) 0.0014(16) 0.0060(18) N3 0.025(2) 0.040(3) 0.019(2) -0.0026(19) -0.0034(17) 0.008(2) C1 0.024(3) 0.036(3) 0.024(3) -0.001(2) 0.007(2) 0.004(2) C2 0.033(3) 0.039(3) 0.023(3) -0.009(2) 0.000(2) -0.007(3) C3 0.033(3) 0.044(3) 0.020(2) -0.001(2) 0.000(2) -0.004(3) C4 0.027(3) 0.044(3) 0.026(3) 0.008(2) -0.003(2) 0.002(2) C5 0.030(3) 0.040(3) 0.041(3) -0.003(3) -0.008(2) 0.007(3) C6 0.034(3) 0.047(4) 0.058(4) 0.003(3) -0.015(3) 0.004(3) C7 0.029(3) 0.057(4) 0.059(4) 0.024(3) -0.010(3) 0.000(3) C8 0.024(3) 0.068(4) 0.033(3) 0.002(3) 0.000(2) 0.004(3) C9 0.022(3) 0.048(3) 0.028(3) 0.003(3) 0.003(2) 0.005(2) C10 0.025(3) 0.031(3) 0.026(3) -0.003(2) -0.003(2) 0.001(2) C11 0.051(4) 0.052(4) 0.061(4) -0.017(3) -0.010(3) 0.014(3) C12 0.025(3) 0.051(4) 0.035(3) -0.011(3) 0.004(2) 0.007(3) C13 0.027(3) 0.073(4) 0.025(3) -0.001(3) -0.002(2) 0.004(3) C14 0.022(2) 0.037(3) 0.026(3) -0.004(2) -0.004(2) 0.009(2) C15 0.025(3) 0.040(3) 0.023(3) -0.003(2) -0.004(2) 0.010(2) C16 0.031(3) 0.035(3) 0.017(2) -0.007(2) 0.000(2) 0.010(2) C17 0.029(3) 0.047(3) 0.025(3) 0.000(2) -0.002(2) 0.009(3) C18 0.019(2) 0.073(4) 0.020(3) 0.000(3) 0.000(2) 0.004(3) C19 0.028(3) 0.117(6) 0.022(3) 0.006(4) 0.006(2) -0.002(4) C20 0.028(3) 0.150(9) 0.029(3) 0.000(5) 0.006(3) 0.023(5) C21 0.048(4) 0.121(7) 0.023(3) -0.008(4) 0.006(3) 0.049(5) C22 0.040(3) 0.075(5) 0.022(3) -0.008(3) -0.002(2) 0.032(3) C23 0.023(3) 0.060(4) 0.016(2) -0.003(2) 0.000(2) 0.013(3) C24 0.033(3) 0.058(4) 0.034(3) 0.002(3) 0.005(2) -0.008(3) C25 0.067(4) 0.069(5) 0.027(3) -0.016(3) -0.008(3) 0.036(4) C26 0.024(3) 0.038(3) 0.020(2) -0.005(2) -0.004(2) 0.002(2) C27 0.030(3) 0.055(4) 0.025(3) -0.008(3) 0.001(2) 0.007(3) C28 0.029(3) 0.062(4) 0.032(3) -0.009(3) -0.003(2) 0.021(3) C29 0.039(3) 0.040(3) 0.037(3) -0.009(3) -0.009(3) 0.020(3) C30 0.035(3) 0.035(3) 0.031(3) -0.006(2) -0.004(2) 0.011(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 Cr N1 2.048(4) . ? Cr C1 2.076(5) . ? Cr C4 2.120(5) . ? Cr N2 2.126(4) . ? Cr N3 2.138(4) . ? N1 C14 1.342(6) . ? N1 C10 1.440(7) . ? N2 C16 1.334(6) . ? N2 C23 1.441(6) . ? N3 C30 1.341(7) . ? N3 C26 1.344(6) . ? C1 C2 1.512(7) . ? C2 C3 1.492(8) . ? C3 C4 1.534(8) . ? C5 C6 1.381(9) . ? C5 C10 1.399(8) . ? C5 C11 1.499(8) . ? C6 C7 1.376(9) . ? C7 C8 1.390(9) . ? C8 C9 1.381(8) . ? C9 C10 1.391(7) . ? C9 C12 1.505(8) . ? C13 C14 1.512(7) . ? C14 C15 1.377(7) . ? C15 C16 1.398(7) . ? C16 C17 1.504(7) . ? C18 C23 1.393(8) . ? C18 C19 1.398(7) . ? C18 C24 1.503(8) . ? C19 C20 1.358(11) . ? C20 C21 1.341(12) . ? C21 C22 1.407(9) . ? C22 C23 1.405(8) . ? C22 C25 1.483(10) . ? C26 C27 1.378(7) . ? C27 C28 1.376(8) . ? C28 C29 1.357(8) . ? C29 C30 1.369(7) . ? 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 C1 106.27(18) . . ? N1 Cr C4 96.30(19) . . ? C1 Cr C4 83.2(2) . . ? N1 Cr N2 88.99(16) . . ? C1 Cr N2 102.16(19) . . ? C4 Cr N2 171.14(19) . . ? N1 Cr N3 155.22(17) . . ? C1 Cr N3 98.23(18) . . ? C4 Cr N3 82.79(19) . . ? N2 Cr N3 89.43(15) . . ? C14 N1 C10 115.7(4) . . ? C14 N1 Cr 126.5(4) . . ? C10 N1 Cr 117.5(3) . . ? C16 N2 C23 115.8(4) . . ? C16 N2 Cr 125.3(3) . . ? C23 N2 Cr 118.9(3) . . ? C30 N3 C26 117.8(5) . . ? C30 N3 Cr 115.8(4) . . ? C26 N3 Cr 126.4(4) . . ? C2 C1 Cr 110.2(4) . . ? C3 C2 C1 109.1(4) . . ? C2 C3 C4 108.3(4) . . ? C3 C4 Cr 105.5(4) . . ? C6 C5 C10 119.1(6) . . ? C6 C5 C11 120.2(6) . . ? C10 C5 C11 120.7(6) . . ? C7 C6 C5 121.0(6) . . ? C6 C7 C8 119.2(6) . . ? C9 C8 C7 121.4(6) . . ? C8 C9 C10 118.6(6) . . ? C8 C9 C12 120.3(5) . . ? C10 C9 C12 121.1(5) . . ? C9 C10 C5 120.7(5) . . ? C9 C10 N1 121.9(5) . . ? C5 C10 N1 117.4(5) . . ? N1 C14 C15 124.5(5) . . ? N1 C14 C13 119.3(5) . . ? C15 C14 C13 116.1(4) . . ? C14 C15 C16 129.6(5) . . ? N2 C16 C15 123.3(5) . . ? N2 C16 C17 119.9(4) . . ? C15 C16 C17 116.8(4) . . ? C23 C18 C19 118.0(6) . . ? C23 C18 C24 123.2(5) . . ? C19 C18 C24 118.9(6) . . ? C20 C19 C18 121.5(8) . . ? C21 C20 C19 120.2(6) . . ? C20 C21 C22 122.3(7) . . ? C23 C22 C21 116.9(7) . . ? C23 C22 C25 121.1(5) . . ? C21 C22 C25 122.0(6) . . ? C18 C23 C22 121.1(5) . . ? C18 C23 N2 121.1(5) . . ? C22 C23 N2 117.7(6) . . ? N3 C26 C27 121.7(5) . . ? C28 C27 C26 119.2(6) . . ? C29 C28 C27 119.2(5) . . ? C28 C29 C30 119.1(6) . . ? N3 C30 C29 122.8(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Cr N1 C14 91.5(4) . . . . ? C4 Cr N1 C14 176.2(4) . . . . ? N2 Cr N1 C14 -10.9(4) . . . . ? N3 Cr N1 C14 -97.3(5) . . . . ? C1 Cr N1 C10 -94.8(4) . . . . ? C4 Cr N1 C10 -10.0(4) . . . . ? N2 Cr N1 C10 162.9(3) . . . . ? N3 Cr N1 C10 76.4(5) . . . . ? N1 Cr N2 C16 12.1(4) . . . . ? C1 Cr N2 C16 -94.3(4) . . . . ? C4 Cr N2 C16 139.0(12) . . . . ? N3 Cr N2 C16 167.4(4) . . . . ? N1 Cr N2 C23 -168.8(4) . . . . ? C1 Cr N2 C23 84.8(4) . . . . ? C4 Cr N2 C23 -41.9(14) . . . . ? N3 Cr N2 C23 -13.5(4) . . . . ? N1 Cr N3 C30 -18.2(6) . . . . ? C1 Cr N3 C30 153.3(4) . . . . ? C4 Cr N3 C30 71.2(4) . . . . ? N2 Cr N3 C30 -104.5(4) . . . . ? N1 Cr N3 C26 159.4(4) . . . . ? C1 Cr N3 C26 -29.2(4) . . . . ? C4 Cr N3 C26 -111.2(4) . . . . ? N2 Cr N3 C26 73.0(4) . . . . ? N1 Cr C1 C2 88.6(4) . . . . ? C4 Cr C1 C2 -6.0(4) . . . . ? N2 Cr C1 C2 -178.9(3) . . . . ? N3 Cr C1 C2 -87.7(4) . . . . ? Cr C1 C2 C3 33.7(5) . . . . ? C1 C2 C3 C4 -53.3(6) . . . . ? C2 C3 C4 Cr 46.0(5) . . . . ? N1 Cr C4 C3 -127.1(4) . . . . ? C1 Cr C4 C3 -21.3(4) . . . . ? N2 Cr C4 C3 106.5(13) . . . . ? N3 Cr C4 C3 77.9(4) . . . . ? C10 C5 C6 C7 -2.4(8) . . . . ? C11 C5 C6 C7 177.6(5) . . . . ? C5 C6 C7 C8 2.7(8) . . . . ? C6 C7 C8 C9 -0.5(8) . . . . ? C7 C8 C9 C10 -2.0(8) . . . . ? C7 C8 C9 C12 178.3(5) . . . . ? C8 C9 C10 C5 2.3(8) . . . . ? C12 C9 C10 C5 -177.9(5) . . . . ? C8 C9 C10 N1 -176.3(4) . . . . ? C12 C9 C10 N1 3.5(7) . . . . ? C6 C5 C10 C9 -0.2(8) . . . . ? C11 C5 C10 C9 179.8(5) . . . . ? C6 C5 C10 N1 178.5(4) . . . . ? C11 C5 C10 N1 -1.5(7) . . . . ? C14 N1 C10 C9 -89.8(6) . . . . ? Cr N1 C10 C9 95.8(5) . . . . ? C14 N1 C10 C5 91.5(6) . . . . ? Cr N1 C10 C5 -82.9(5) . . . . ? C10 N1 C14 C15 -170.8(5) . . . . ? Cr N1 C14 C15 3.0(7) . . . . ? C10 N1 C14 C13 7.0(7) . . . . ? Cr N1 C14 C13 -179.1(4) . . . . ? N1 C14 C15 C16 10.0(9) . . . . ? C13 C14 C15 C16 -167.9(5) . . . . ? C23 N2 C16 C15 175.3(5) . . . . ? Cr N2 C16 C15 -5.6(7) . . . . ? C23 N2 C16 C17 -2.1(7) . . . . ? Cr N2 C16 C17 177.0(4) . . . . ? C14 C15 C16 N2 -8.3(9) . . . . ? C14 C15 C16 C17 169.1(5) . . . . ? C23 C18 C19 C20 -0.2(8) . . . . ? C24 C18 C19 C20 179.6(6) . . . . ? C18 C19 C20 C21 1.7(10) . . . . ? C19 C20 C21 C22 -1.1(10) . . . . ? C20 C21 C22 C23 -1.0(9) . . . . ? C20 C21 C22 C25 176.5(6) . . . . ? C19 C18 C23 C22 -1.9(8) . . . . ? C24 C18 C23 C22 178.2(5) . . . . ? C19 C18 C23 N2 176.2(5) . . . . ? C24 C18 C23 N2 -3.6(8) . . . . ? C21 C22 C23 C18 2.5(8) . . . . ? C25 C22 C23 C18 -175.0(5) . . . . ? C21 C22 C23 N2 -175.7(5) . . . . ? C25 C22 C23 N2 6.8(8) . . . . ? C16 N2 C23 C18 89.2(6) . . . . ? Cr N2 C23 C18 -89.9(5) . . . . ? C16 N2 C23 C22 -92.6(6) . . . . ? Cr N2 C23 C22 88.3(5) . . . . ? C30 N3 C26 C27 0.8(7) . . . . ? Cr N3 C26 C27 -176.6(4) . . . . ? N3 C26 C27 C28 0.9(8) . . . . ? C26 C27 C28 C29 -1.2(8) . . . . ? C27 C28 C29 C30 -0.1(8) . . . . ? C26 N3 C30 C29 -2.3(8) . . . . ? Cr N3 C30 C29 175.4(4) . . . . ? C28 C29 C30 N3 2.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.467 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.087 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 198.2 36.6 2 0.500 0.000 0.500 198.2 36.4 _platon_squeeze_details ; PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 Void Space Analysis consistent with 1.5 molecules of co-crystallized pentane molecules per unit cell. ; _vrf_CHEMW03_klat354s ; PROBLEM: WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: 1.5 molecules of co-crystallized pentane molecules per unit cell were treated as bulk solvent. See _platon_squeeze_details. ; data_klat309a _database_code_depnum_ccdc_archive 'CCDC 918023' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H51 Cr N2' _chemical_formula_weight 647.86 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 21.020(4) _cell_length_b 18.707(3) _cell_length_c 19.091(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7507(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 839 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 18.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9269 _exptl_absorpt_correction_T_max 0.9421 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 42444 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6835 _reflns_number_gt 4533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Phenyl ring C36-C41 was disorded near a mirror plane and refined as rigid group. ; _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^)+(0.1000P)^2^+0.3046P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6835 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1765 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.44866(3) 0.2500 0.74508(3) 0.0407(2) Uani 1 2 d S . . Cr2 Cr 0.23907(3) 0.2500 0.28007(3) 0.0439(2) Uani 1 2 d S . . N1 N 0.51466(11) 0.17466(13) 0.74970(12) 0.0457(6) Uani 1 1 d . . . N2 N 0.30439(10) 0.32441(13) 0.29505(12) 0.0445(6) Uani 1 1 d . . . C1 C 0.2600(2) 0.2500 0.6425(3) 0.0730(15) Uani 1 2 d S . . H1A H 0.2407 0.2500 0.6875 0.088 Uiso 1 2 calc SR . . C2 C 0.2215(3) 0.2500 0.5827(3) 0.0943(19) Uani 1 2 d S . . H2A H 0.1765 0.2500 0.5868 0.113 Uiso 1 2 calc SR . . C3 C 0.2500(3) 0.2500 0.5181(3) 0.0806(17) Uani 1 2 d S . . H3A H 0.2243 0.2500 0.4771 0.097 Uiso 1 2 calc SR . . C4 C 0.3141(3) 0.2500 0.5115(3) 0.0738(15) Uani 1 2 d S . . H4A H 0.3331 0.2500 0.4664 0.089 Uiso 1 2 calc SR . . C5 C 0.3517(2) 0.2500 0.5710(2) 0.0568(12) Uani 1 2 d S . . H5A H 0.3967 0.2500 0.5662 0.068 Uiso 1 2 calc SR . . C6 C 0.32512(19) 0.2500 0.6373(2) 0.0469(10) Uani 1 2 d S . . C7 C 0.36549(17) 0.2500 0.7005(2) 0.0407(9) Uani 1 2 d S . . C8 C 0.35738(17) 0.2500 0.7684(2) 0.0366(9) Uani 1 2 d S . . C9 C 0.30570(17) 0.2500 0.82009(19) 0.0398(9) Uani 1 2 d S . . C10 C 0.28123(18) 0.1881(2) 0.8459(2) 0.0828(12) Uani 1 1 d . . . H10A H 0.2965 0.1436 0.8290 0.099 Uiso 1 1 calc R . . C11 C 0.2340(2) 0.1895(4) 0.8971(3) 0.126(2) Uani 1 1 d . . . H11A H 0.2176 0.1456 0.9145 0.151 Uiso 1 1 calc R . . C12 C 0.2116(4) 0.2500 0.9219(4) 0.151(5) Uani 1 2 d S . . H12A H 0.1797 0.2500 0.9572 0.181 Uiso 1 2 calc SR . . C13 C 0.49002(14) 0.10299(16) 0.75824(15) 0.0457(7) Uani 1 1 d . . . C14 C 0.47430(15) 0.06213(16) 0.69898(16) 0.0519(8) Uani 1 1 d . . . C15 C 0.45253(15) -0.00744(18) 0.70959(18) 0.0612(9) Uani 1 1 d . . . H15A H 0.4412 -0.0358 0.6703 0.073 Uiso 1 1 calc R . . C16 C 0.44704(16) -0.03595(18) 0.7760(2) 0.0641(9) Uani 1 1 d . . . H16A H 0.4341 -0.0842 0.7822 0.077 Uiso 1 1 calc R . . C17 C 0.46041(14) 0.00609(18) 0.83302(18) 0.0568(8) Uani 1 1 d . . . H17A H 0.4549 -0.0133 0.8786 0.068 Uiso 1 1 calc R . . C18 C 0.48164(13) 0.07581(17) 0.82629(15) 0.0483(7) Uani 1 1 d . . . C19 C 0.49399(15) 0.12070(18) 0.89098(16) 0.0600(9) Uani 1 1 d . . . H19A H 0.5118 0.1675 0.8750 0.072 Uiso 1 1 calc R . . C20 C 0.4326(2) 0.1359(3) 0.9285(2) 0.0987(14) Uani 1 1 d . . . H20A H 0.4028 0.1591 0.8962 0.148 Uiso 1 1 calc R . . H20B H 0.4408 0.1675 0.9684 0.148 Uiso 1 1 calc R . . H20C H 0.4141 0.0909 0.9453 0.148 Uiso 1 1 calc R . . C21 C 0.5416(3) 0.0876(3) 0.9406(3) 0.179(3) Uani 1 1 d . . . H21A H 0.5473 0.1188 0.9813 0.269 Uiso 1 1 calc R . . H21B H 0.5825 0.0817 0.9165 0.269 Uiso 1 1 calc R . . H21C H 0.5261 0.0408 0.9561 0.269 Uiso 1 1 calc R . . C22 C 0.48045(19) 0.0910(2) 0.62534(17) 0.0736(11) Uani 1 1 d . . . H22A H 0.4889 0.1435 0.6283 0.088 Uiso 1 1 calc R . . C23 C 0.5371(3) 0.0555(3) 0.5879(2) 0.131(2) Uani 1 1 d . . . H23A H 0.5765 0.0668 0.6130 0.197 Uiso 1 1 calc R . . H23B H 0.5399 0.0736 0.5398 0.197 Uiso 1 1 calc R . . H23C H 0.5309 0.0036 0.5870 0.197 Uiso 1 1 calc R . . C24 C 0.4199(2) 0.0798(2) 0.5823(2) 0.1030(15) Uani 1 1 d . . . H24A H 0.3839 0.1027 0.6061 0.154 Uiso 1 1 calc R . . H24B H 0.4116 0.0285 0.5775 0.154 Uiso 1 1 calc R . . H24C H 0.4254 0.1011 0.5358 0.154 Uiso 1 1 calc R . . C25 C 0.62187(17) 0.1195(2) 0.7522(2) 0.0897(13) Uani 1 1 d . . . H25A H 0.6107 0.0851 0.7156 0.134 Uiso 1 1 calc R . . H25B H 0.6176 0.0968 0.7983 0.134 Uiso 1 1 calc R . . H25C H 0.6659 0.1354 0.7456 0.134 Uiso 1 1 calc R . . C26 C 0.57786(15) 0.18310(18) 0.74806(18) 0.0598(9) Uani 1 1 d . . . C27 C 0.6067(2) 0.2500 0.7444(3) 0.0671(14) Uani 1 2 d S . . H27A H 0.6516 0.2500 0.7387 0.081 Uiso 1 2 calc SR . . C28 C 0.0278(2) 0.2500 0.2972(2) 0.0620(13) Uani 1 2 d S . . H28A H 0.0265 0.2500 0.2474 0.074 Uiso 1 2 calc SR . . C29 C -0.0275(2) 0.2500 0.3343(3) 0.0798(17) Uani 1 2 d S . . H29A H -0.0669 0.2500 0.3099 0.096 Uiso 1 2 calc SR . . C30 C -0.0274(2) 0.2500 0.4061(3) 0.0719(15) Uani 1 2 d S . . H30A H -0.0665 0.2500 0.4312 0.086 Uiso 1 2 calc SR . . C31 C 0.0292(2) 0.2500 0.4414(2) 0.0661(13) Uani 1 2 d S . . H31A H 0.0299 0.2500 0.4912 0.079 Uiso 1 2 calc SR . . C32 C 0.0852(2) 0.2500 0.4039(2) 0.0545(11) Uani 1 2 d S . . H32A H 0.1244 0.2500 0.4286 0.065 Uiso 1 2 calc SR . . C33 C 0.08630(18) 0.2500 0.3313(2) 0.0427(10) Uani 1 2 d S . . C34 C 0.14661(18) 0.2500 0.2917(2) 0.0413(9) Uani 1 2 d S . . C35 C 0.16076(18) 0.2500 0.2241(2) 0.0419(9) Uani 1 2 d S . . C42 C 0.27954(14) 0.39414(16) 0.27706(15) 0.0477(7) Uani 1 1 d . . . C43 C 0.28425(17) 0.41780(19) 0.20716(17) 0.0611(9) Uani 1 1 d . . . C44 C 0.25359(19) 0.4815(2) 0.1898(2) 0.0744(11) Uani 1 1 d . . . H44A H 0.2559 0.4983 0.1429 0.089 Uiso 1 1 calc R . . C45 C 0.22029(19) 0.5205(2) 0.2381(2) 0.0739(11) Uani 1 1 d . . . H45A H 0.1992 0.5633 0.2247 0.089 Uiso 1 1 calc R . . C46 C 0.21763(16) 0.49705(19) 0.3068(2) 0.0671(9) Uani 1 1 d . . . H46A H 0.1951 0.5246 0.3404 0.081 Uiso 1 1 calc R . . C47 C 0.24700(14) 0.43439(18) 0.32760(17) 0.0537(8) Uani 1 1 d . . . C48 C 0.24304(16) 0.4119(2) 0.40360(17) 0.0669(10) Uani 1 1 d . . . H48A H 0.2587 0.3615 0.4067 0.080 Uiso 1 1 calc R . . C49 C 0.17655(16) 0.4133(2) 0.43262(18) 0.0737(10) Uani 1 1 d . . . H49A H 0.1486 0.3845 0.4028 0.110 Uiso 1 1 calc R . . H49B H 0.1611 0.4627 0.4338 0.110 Uiso 1 1 calc R . . H49C H 0.1766 0.3936 0.4802 0.110 Uiso 1 1 calc R . . C50 C 0.2856(2) 0.4575(3) 0.4503(2) 0.139(2) Uani 1 1 d . . . H50A H 0.2891 0.4351 0.4966 0.208 Uiso 1 1 calc R . . H50B H 0.2670 0.5053 0.4553 0.208 Uiso 1 1 calc R . . H50C H 0.3279 0.4614 0.4292 0.208 Uiso 1 1 calc R . . C51 C 0.32204(19) 0.37729(19) 0.15221(17) 0.0751(11) Uani 1 1 d . . . H51A H 0.3411 0.3344 0.1753 0.090 Uiso 1 1 calc R . . C52 C 0.2802(3) 0.3510(3) 0.0910(2) 0.1230(19) Uani 1 1 d . . . H52A H 0.2476 0.3184 0.1089 0.185 Uiso 1 1 calc R . . H52B H 0.3068 0.3258 0.0568 0.185 Uiso 1 1 calc R . . H52C H 0.2598 0.3920 0.0684 0.185 Uiso 1 1 calc R . . C53 C 0.3766(2) 0.4230(2) 0.1235(2) 0.0952(13) Uani 1 1 d . . . H53A H 0.4010 0.4432 0.1626 0.143 Uiso 1 1 calc R . . H53B H 0.3592 0.4619 0.0949 0.143 Uiso 1 1 calc R . . H53C H 0.4046 0.3933 0.0946 0.143 Uiso 1 1 calc R . . C54 C 0.40675(17) 0.3811(2) 0.3243(2) 0.0812(12) Uani 1 1 d . . . H54A H 0.3805 0.4243 0.3275 0.122 Uiso 1 1 calc R . . H54B H 0.4350 0.3847 0.2837 0.122 Uiso 1 1 calc R . . H54C H 0.4323 0.3763 0.3670 0.122 Uiso 1 1 calc R . . C55 C 0.36445(14) 0.31657(18) 0.31635(15) 0.0519(8) Uani 1 1 d . . . C56 C 0.39122(19) 0.2500 0.3293(2) 0.0546(12) Uani 1 2 d S . . H56A H 0.4326 0.2500 0.3494 0.066 Uiso 1 2 calc SR . . C41 C 0.1228(3) 0.1696(3) 0.1281(2) 0.067(2) Uani 0.50 1 d PG A -1 H41A H 0.1437 0.1303 0.1496 0.081 Uiso 0.50 1 calc PR A -1 C40 C 0.0886(3) 0.1596(3) 0.0665(3) 0.098(3) Uani 0.50 1 d PG A -1 H40A H 0.0861 0.1135 0.0460 0.118 Uiso 0.50 1 calc PR A -1 C39 C 0.0581(2) 0.2172(4) 0.0350(2) 0.081(3) Uani 0.50 1 d PG A -1 H39A H 0.0347 0.2103 -0.0070 0.097 Uiso 0.50 1 calc PR A -1 C38 C 0.0617(3) 0.2847(3) 0.0651(3) 0.088(4) Uani 0.50 1 d PG A -1 H38A H 0.0409 0.3241 0.0436 0.106 Uiso 0.50 1 calc PR A -1 C37 C 0.0959(3) 0.2947(2) 0.1266(3) 0.067(2) Uani 0.50 1 d PG A -1 H37A H 0.0984 0.3409 0.1472 0.080 Uiso 0.50 1 calc PR A -1 C36 C 0.12645(19) 0.2372(3) 0.15812(17) 0.0444(19) Uani 0.50 1 d PG A -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 Cr1 0.0281(4) 0.0511(4) 0.0428(4) 0.000 -0.0029(3) 0.000 Cr2 0.0301(4) 0.0542(4) 0.0473(4) 0.000 -0.0028(3) 0.000 N1 0.0340(14) 0.0533(16) 0.0498(15) -0.0034(11) -0.0013(11) 0.0018(11) N2 0.0336(14) 0.0612(16) 0.0388(13) 0.0010(11) 0.0021(11) -0.0055(11) C1 0.043(3) 0.131(5) 0.044(3) 0.000 -0.008(2) 0.000 C2 0.052(3) 0.148(6) 0.082(5) 0.000 -0.023(3) 0.000 C3 0.082(4) 0.103(4) 0.057(4) 0.000 -0.035(3) 0.000 C4 0.087(4) 0.092(4) 0.043(3) 0.000 -0.007(3) 0.000 C5 0.052(3) 0.078(3) 0.041(3) 0.000 -0.004(2) 0.000 C6 0.041(2) 0.059(3) 0.041(2) 0.000 -0.0035(19) 0.000 C7 0.035(2) 0.047(2) 0.041(2) 0.000 -0.0032(18) 0.000 C8 0.031(2) 0.037(2) 0.042(2) 0.000 -0.0010(17) 0.000 C9 0.034(2) 0.051(2) 0.034(2) 0.000 -0.0036(17) 0.000 C10 0.076(3) 0.081(3) 0.092(3) 0.011(2) 0.016(2) -0.021(2) C11 0.099(4) 0.197(7) 0.083(4) 0.045(4) 0.026(3) -0.057(4) C12 0.067(5) 0.324(18) 0.062(5) 0.000 0.027(4) 0.000 C13 0.0346(17) 0.0481(17) 0.0545(19) -0.0029(14) -0.0018(13) 0.0054(13) C14 0.0540(19) 0.0548(19) 0.0470(18) -0.0034(15) -0.0041(15) 0.0095(16) C15 0.061(2) 0.060(2) 0.062(2) -0.0136(18) -0.0079(17) 0.0067(17) C16 0.056(2) 0.052(2) 0.085(3) 0.0034(19) -0.0002(19) 0.0001(16) C17 0.0462(19) 0.066(2) 0.058(2) 0.0087(18) 0.0033(16) 0.0021(16) C18 0.0352(16) 0.064(2) 0.0460(18) -0.0026(15) -0.0009(13) 0.0066(15) C19 0.055(2) 0.078(2) 0.0477(18) -0.0083(16) -0.0061(16) 0.0085(17) C20 0.081(3) 0.138(4) 0.077(3) -0.041(3) 0.015(2) 0.007(3) C21 0.188(6) 0.204(6) 0.146(5) -0.100(5) -0.121(5) 0.127(5) C22 0.106(3) 0.067(2) 0.048(2) -0.0008(17) -0.004(2) 0.008(2) C23 0.154(5) 0.171(5) 0.069(3) 0.037(3) 0.041(3) 0.053(4) C24 0.151(4) 0.094(3) 0.064(3) -0.010(2) -0.042(3) 0.025(3) C25 0.049(2) 0.072(3) 0.148(4) -0.002(2) 0.006(2) 0.0172(19) C26 0.0335(18) 0.068(2) 0.078(2) -0.0031(18) -0.0022(16) 0.0081(17) C27 0.028(2) 0.069(3) 0.104(4) 0.000 -0.003(2) 0.000 C28 0.037(2) 0.098(4) 0.051(3) 0.000 -0.006(2) 0.000 C29 0.031(3) 0.152(5) 0.057(3) 0.000 0.001(2) 0.000 C30 0.041(3) 0.113(4) 0.062(3) 0.000 0.001(2) 0.000 C31 0.063(3) 0.093(4) 0.043(3) 0.000 -0.003(2) 0.000 C32 0.039(3) 0.074(3) 0.051(3) 0.000 -0.009(2) 0.000 C33 0.031(2) 0.045(2) 0.053(3) 0.000 -0.0060(19) 0.000 C34 0.034(2) 0.035(2) 0.054(3) 0.000 -0.0073(19) 0.000 C35 0.035(2) 0.036(2) 0.055(3) 0.000 -0.0043(19) 0.000 C42 0.0373(17) 0.0565(19) 0.0494(18) 0.0013(15) -0.0046(14) -0.0128(14) C43 0.066(2) 0.068(2) 0.049(2) 0.0040(17) -0.0023(16) -0.0302(19) C44 0.086(3) 0.071(3) 0.065(2) 0.025(2) -0.016(2) -0.027(2) C45 0.068(3) 0.071(2) 0.083(3) 0.020(2) -0.009(2) -0.002(2) C46 0.056(2) 0.074(2) 0.072(2) 0.010(2) 0.0044(18) -0.0009(19) C47 0.0387(17) 0.067(2) 0.056(2) 0.0067(17) 0.0014(14) -0.0030(15) C48 0.060(2) 0.085(3) 0.056(2) 0.0063(18) 0.0124(17) 0.0233(19) C49 0.067(2) 0.087(3) 0.067(2) 0.009(2) 0.0083(19) 0.000(2) C50 0.084(3) 0.271(8) 0.061(3) 0.007(4) -0.012(2) -0.052(4) C51 0.105(3) 0.073(2) 0.047(2) 0.0005(17) 0.011(2) -0.029(2) C52 0.162(5) 0.141(4) 0.067(3) -0.020(3) 0.007(3) -0.071(4) C53 0.107(3) 0.097(3) 0.081(3) -0.009(2) 0.025(2) -0.032(3) C54 0.053(2) 0.109(3) 0.081(3) 0.004(2) -0.0115(19) -0.028(2) C55 0.0350(17) 0.084(2) 0.0370(16) -0.0034(15) 0.0011(13) -0.0126(16) C56 0.029(2) 0.091(4) 0.044(2) 0.000 -0.0019(19) 0.000 C41 0.089(7) 0.061(5) 0.052(4) -0.005(4) -0.011(4) -0.018(4) C40 0.109(8) 0.105(7) 0.080(6) 0.004(6) -0.039(6) -0.037(6) C39 0.073(6) 0.141(9) 0.029(5) 0.016(5) -0.018(4) -0.016(5) C38 0.074(6) 0.157(11) 0.034(5) 0.022(5) -0.012(4) 0.021(6) C37 0.062(6) 0.069(6) 0.068(5) 0.016(4) -0.001(4) 0.019(4) C36 0.037(3) 0.043(6) 0.053(3) 0.009(3) 0.003(2) -0.006(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 C7 1.944(4) . ? Cr1 C8 1.970(4) . ? Cr1 N1 1.980(2) . ? Cr1 N1 1.980(2) 7_565 ? Cr2 C34 1.956(4) . ? Cr2 C35 1.962(4) . ? Cr2 N2 1.976(2) . ? Cr2 N2 1.976(2) 7_565 ? N1 C26 1.338(4) . ? N1 C13 1.447(4) . ? N2 C55 1.335(4) . ? N2 C42 1.446(4) . ? C1 C6 1.373(6) . ? C1 C2 1.399(7) . ? C2 C3 1.372(8) . ? C3 C4 1.352(7) . ? C4 C5 1.384(6) . ? C5 C6 1.384(6) . ? C6 C7 1.476(5) . ? C7 C8 1.307(5) . ? C8 C9 1.468(5) . ? C9 C10 1.359(4) 7_565 ? C9 C10 1.359(4) . ? C10 C11 1.393(6) . ? C11 C12 1.314(6) . ? C12 C11 1.314(6) 7_565 ? C13 C14 1.405(4) . ? C13 C18 1.406(4) . ? C14 C15 1.394(5) . ? C14 C22 1.512(4) . ? C15 C16 1.380(5) . ? C16 C17 1.372(5) . ? C17 C18 1.384(4) . ? C18 C19 1.516(4) . ? C19 C20 1.503(5) . ? C19 C21 1.511(5) . ? C22 C24 1.529(5) . ? C22 C23 1.540(5) . ? C25 C26 1.509(5) . ? C26 C27 1.392(4) . ? C27 C26 1.392(4) 7_565 ? C28 C29 1.362(6) . ? C28 C33 1.390(6) . ? C29 C30 1.371(7) . ? C30 C31 1.369(6) . ? C31 C32 1.378(6) . ? C32 C33 1.387(6) . ? C33 C34 1.476(5) . ? C34 C35 1.324(6) . ? C35 C36 1.472(5) 7_565 ? C35 C36 1.472(5) . ? C42 C47 1.402(4) . ? C42 C43 1.409(4) . ? C43 C44 1.394(5) . ? C43 C51 1.519(5) . ? C44 C45 1.370(5) . ? C45 C46 1.384(5) . ? C46 C47 1.383(4) . ? C47 C48 1.513(4) . ? C48 C49 1.504(4) . ? C48 C50 1.524(6) . ? C51 C53 1.533(5) . ? C51 C52 1.543(5) . ? C54 C55 1.507(4) . ? C55 C56 1.389(4) . ? C56 C55 1.389(4) 7_565 ? C41 C40 1.3900 . ? C41 C36 1.3900 . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? 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 C7 Cr1 C8 39.00(15) . . ? C7 Cr1 N1 130.52(8) . . ? C8 Cr1 N1 132.27(8) . . ? C7 Cr1 N1 130.52(8) . 7_565 ? C8 Cr1 N1 132.27(8) . 7_565 ? N1 Cr1 N1 90.78(14) . 7_565 ? C34 Cr2 C35 39.50(16) . . ? C34 Cr2 N2 132.37(8) . . ? C35 Cr2 N2 131.43(8) . . ? C34 Cr2 N2 132.37(8) . 7_565 ? C35 Cr2 N2 131.43(8) . 7_565 ? N2 Cr2 N2 89.57(14) . 7_565 ? C26 N1 C13 117.9(2) . . ? C26 N1 Cr1 127.6(2) . . ? C13 N1 Cr1 114.45(17) . . ? C55 N2 C42 120.9(2) . . ? C55 N2 Cr2 128.6(2) . . ? C42 N2 Cr2 110.48(17) . . ? C6 C1 C2 121.2(5) . . ? C3 C2 C1 118.8(5) . . ? C4 C3 C2 121.2(5) . . ? C3 C4 C5 119.6(5) . . ? C4 C5 C6 121.3(4) . . ? C1 C6 C5 118.0(4) . . ? C1 C6 C7 120.9(4) . . ? C5 C6 C7 121.1(4) . . ? C8 C7 C6 137.4(4) . . ? C8 C7 Cr1 71.5(2) . . ? C6 C7 Cr1 151.0(3) . . ? C7 C8 C9 139.8(4) . . ? C7 C8 Cr1 69.5(2) . . ? C9 C8 Cr1 150.8(3) . . ? C10 C9 C10 116.7(5) 7_565 . ? C10 C9 C8 121.6(2) 7_565 . ? C10 C9 C8 121.6(2) . . ? C9 C10 C11 120.6(4) . . ? C12 C11 C10 121.6(6) . . ? C11 C12 C11 118.8(8) 7_565 . ? C14 C13 C18 121.2(3) . . ? C14 C13 N1 119.8(3) . . ? C18 C13 N1 119.0(3) . . ? C15 C14 C13 117.9(3) . . ? C15 C14 C22 119.8(3) . . ? C13 C14 C22 122.3(3) . . ? C16 C15 C14 121.4(3) . . ? C15 C16 C17 119.4(3) . . ? C16 C17 C18 122.2(3) . . ? C17 C18 C13 117.8(3) . . ? C17 C18 C19 120.1(3) . . ? C13 C18 C19 122.1(3) . . ? C20 C19 C21 110.4(4) . . ? C20 C19 C18 110.2(3) . . ? C21 C19 C18 113.4(3) . . ? C14 C22 C24 112.3(3) . . ? C14 C22 C23 110.1(3) . . ? C24 C22 C23 109.6(3) . . ? N1 C26 C27 122.7(3) . . ? N1 C26 C25 121.0(3) . . ? C27 C26 C25 116.4(3) . . ? C26 C27 C26 128.0(4) . 7_565 ? C29 C28 C33 120.8(4) . . ? C28 C29 C30 121.3(5) . . ? C31 C30 C29 119.6(5) . . ? C30 C31 C32 119.1(4) . . ? C31 C32 C33 122.3(4) . . ? C32 C33 C28 116.9(4) . . ? C32 C33 C34 121.7(4) . . ? C28 C33 C34 121.3(4) . . ? C35 C34 C33 133.8(4) . . ? C35 C34 Cr2 70.5(2) . . ? C33 C34 Cr2 155.8(3) . . ? C34 C35 C36 136.4(4) . 7_565 ? C34 C35 C36 136.4(4) . . ? C36 C35 C36 18.7(4) 7_565 . ? C34 C35 Cr2 70.0(2) . . ? C36 C35 Cr2 151.3(3) 7_565 . ? C36 C35 Cr2 151.3(3) . . ? C47 C42 C43 121.1(3) . . ? C47 C42 N2 119.8(3) . . ? C43 C42 N2 118.9(3) . . ? C44 C43 C42 117.5(3) . . ? C44 C43 C51 120.2(3) . . ? C42 C43 C51 122.3(3) . . ? C45 C44 C43 122.1(3) . . ? C44 C45 C46 119.3(4) . . ? C47 C46 C45 121.5(4) . . ? C46 C47 C42 118.4(3) . . ? C46 C47 C48 119.1(3) . . ? C42 C47 C48 122.5(3) . . ? C49 C48 C47 113.5(3) . . ? C49 C48 C50 108.6(3) . . ? C47 C48 C50 111.9(3) . . ? C43 C51 C53 111.1(3) . . ? C43 C51 C52 112.6(4) . . ? C53 C51 C52 109.5(3) . . ? N2 C55 C56 122.4(3) . . ? N2 C55 C54 120.0(3) . . ? C56 C55 C54 117.5(3) . . ? C55 C56 C55 127.4(4) 7_565 . ? C40 C41 C36 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C36 C41 120.0 . . ? C37 C36 C35 118.1(4) . . ? C41 C36 C35 121.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 Cr1 N1 C26 143.8(3) . . . . ? C8 Cr1 N1 C26 -163.4(3) . . . . ? N1 Cr1 N1 C26 -6.3(3) 7_565 . . . ? C7 Cr1 N1 C13 -38.5(3) . . . . ? C8 Cr1 N1 C13 14.3(3) . . . . ? N1 Cr1 N1 C13 171.45(14) 7_565 . . . ? C34 Cr2 N2 C55 147.1(3) . . . . ? C35 Cr2 N2 C55 -158.9(3) . . . . ? N2 Cr2 N2 C55 -7.8(3) 7_565 . . . ? C34 Cr2 N2 C42 -34.9(3) . . . . ? C35 Cr2 N2 C42 19.1(3) . . . . ? N2 Cr2 N2 C42 170.24(14) 7_565 . . . ? C6 C1 C2 C3 0.000(1) . . . . ? C1 C2 C3 C4 0.000(1) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C2 C1 C6 C5 0.0 . . . . ? C2 C1 C6 C7 180.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C4 C5 C6 C7 180.0 . . . . ? C1 C6 C7 C8 0.000(1) . . . . ? C5 C6 C7 C8 180.0 . . . . ? C1 C6 C7 Cr1 180.0 . . . . ? C5 C6 C7 Cr1 0.000(1) . . . . ? N1 Cr1 C7 C8 110.53(13) . . . . ? N1 Cr1 C7 C8 -110.53(13) 7_565 . . . ? C8 Cr1 C7 C6 180.000(1) . . . . ? N1 Cr1 C7 C6 -69.47(13) . . . . ? N1 Cr1 C7 C6 69.47(13) 7_565 . . . ? C6 C7 C8 C9 0.000(2) . . . . ? Cr1 C7 C8 C9 180.000(1) . . . . ? C6 C7 C8 Cr1 180.000(1) . . . . ? N1 Cr1 C8 C7 -105.81(13) . . . . ? N1 Cr1 C8 C7 105.82(13) 7_565 . . . ? C7 Cr1 C8 C9 180.000(2) . . . . ? N1 Cr1 C8 C9 74.19(14) . . . . ? N1 Cr1 C8 C9 -74.18(14) 7_565 . . . ? C7 C8 C9 C10 -91.0(4) . . . 7_565 ? Cr1 C8 C9 C10 89.0(4) . . . 7_565 ? C7 C8 C9 C10 91.0(4) . . . . ? Cr1 C8 C9 C10 -89.0(4) . . . . ? C10 C9 C10 C11 -0.8(8) 7_565 . . . ? C8 C9 C10 C11 177.3(4) . . . . ? C9 C10 C11 C12 0.1(10) . . . . ? C10 C11 C12 C11 0.7(14) . . . 7_565 ? C26 N1 C13 C14 -93.4(3) . . . . ? Cr1 N1 C13 C14 88.6(3) . . . . ? C26 N1 C13 C18 87.2(3) . . . . ? Cr1 N1 C13 C18 -90.8(3) . . . . ? C18 C13 C14 C15 -2.6(4) . . . . ? N1 C13 C14 C15 178.1(3) . . . . ? C18 C13 C14 C22 177.6(3) . . . . ? N1 C13 C14 C22 -1.7(4) . . . . ? C13 C14 C15 C16 -0.6(5) . . . . ? C22 C14 C15 C16 179.2(3) . . . . ? C14 C15 C16 C17 3.1(5) . . . . ? C15 C16 C17 C18 -2.5(5) . . . . ? C16 C17 C18 C13 -0.6(4) . . . . ? C16 C17 C18 C19 178.3(3) . . . . ? C14 C13 C18 C17 3.2(4) . . . . ? N1 C13 C18 C17 -177.5(2) . . . . ? C14 C13 C18 C19 -175.7(3) . . . . ? N1 C13 C18 C19 3.6(4) . . . . ? C17 C18 C19 C20 -67.1(4) . . . . ? C13 C18 C19 C20 111.8(4) . . . . ? C17 C18 C19 C21 57.2(5) . . . . ? C13 C18 C19 C21 -123.9(4) . . . . ? C15 C14 C22 C24 50.4(4) . . . . ? C13 C14 C22 C24 -129.8(3) . . . . ? C15 C14 C22 C23 -72.0(5) . . . . ? C13 C14 C22 C23 107.8(4) . . . . ? C13 N1 C26 C27 -175.9(4) . . . . ? Cr1 N1 C26 C27 1.7(5) . . . . ? C13 N1 C26 C25 2.3(5) . . . . ? Cr1 N1 C26 C25 179.9(3) . . . . ? N1 C26 C27 C26 6.1(9) . . . 7_565 ? C25 C26 C27 C26 -172.1(4) . . . 7_565 ? C33 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C28 0.0 . . . . ? C31 C32 C33 C34 180.0 . . . . ? C29 C28 C33 C32 0.0 . . . . ? C29 C28 C33 C34 180.0 . . . . ? C32 C33 C34 C35 180.0 . . . . ? C28 C33 C34 C35 0.0 . . . . ? C32 C33 C34 Cr2 0.0 . . . . ? C28 C33 C34 Cr2 180.0 . . . . ? N2 Cr2 C34 C35 107.55(14) . . . . ? N2 Cr2 C34 C35 -107.55(14) 7_565 . . . ? C35 Cr2 C34 C33 180.0 . . . . ? N2 Cr2 C34 C33 -72.45(15) . . . . ? N2 Cr2 C34 C33 72.45(14) 7_565 . . . ? C33 C34 C35 C36 13.7(3) . . . 7_565 ? Cr2 C34 C35 C36 -166.3(3) . . . 7_565 ? C33 C34 C35 C36 -13.7(3) . . . . ? Cr2 C34 C35 C36 166.3(3) . . . . ? C33 C34 C35 Cr2 180.0 . . . . ? N2 Cr2 C35 C34 -110.03(14) . . . . ? N2 Cr2 C35 C34 110.02(14) 7_565 . . . ? C34 Cr2 C35 C36 160.2(5) . . . 7_565 ? N2 Cr2 C35 C36 50.2(5) . . . 7_565 ? N2 Cr2 C35 C36 -89.8(5) 7_565 . . 7_565 ? C34 Cr2 C35 C36 -160.2(5) . . . . ? N2 Cr2 C35 C36 89.8(4) . . . . ? N2 Cr2 C35 C36 -50.2(5) 7_565 . . . ? C55 N2 C42 C47 -94.3(3) . . . . ? Cr2 N2 C42 C47 87.5(3) . . . . ? C55 N2 C42 C43 90.7(3) . . . . ? Cr2 N2 C42 C43 -87.5(3) . . . . ? C47 C42 C43 C44 -2.1(4) . . . . ? N2 C42 C43 C44 172.9(3) . . . . ? C47 C42 C43 C51 176.8(3) . . . . ? N2 C42 C43 C51 -8.3(4) . . . . ? C42 C43 C44 C45 0.4(5) . . . . ? C51 C43 C44 C45 -178.4(3) . . . . ? C43 C44 C45 C46 1.1(6) . . . . ? C44 C45 C46 C47 -1.0(6) . . . . ? C45 C46 C47 C42 -0.6(5) . . . . ? C45 C46 C47 C48 179.4(3) . . . . ? C43 C42 C47 C46 2.1(4) . . . . ? N2 C42 C47 C46 -172.8(3) . . . . ? C43 C42 C47 C48 -177.8(3) . . . . ? N2 C42 C47 C48 7.3(4) . . . . ? C46 C47 C48 C49 49.6(5) . . . . ? C42 C47 C48 C49 -130.5(3) . . . . ? C46 C47 C48 C50 -73.8(4) . . . . ? C42 C47 C48 C50 106.1(4) . . . . ? C44 C43 C51 C53 60.5(4) . . . . ? C42 C43 C51 C53 -118.3(4) . . . . ? C44 C43 C51 C52 -62.8(4) . . . . ? C42 C43 C51 C52 118.4(4) . . . . ? C42 N2 C55 C56 -175.4(3) . . . . ? Cr2 N2 C55 C56 2.4(4) . . . . ? C42 N2 C55 C54 2.1(4) . . . . ? Cr2 N2 C55 C54 179.9(2) . . . . ? N2 C55 C56 C55 7.0(7) . . . 7_565 ? C54 C55 C56 C55 -170.6(3) . . . 7_565 ? C36 C41 C40 C39 0.0 . . . . ? C41 C40 C39 C38 0.0 . . . . ? C40 C39 C38 C37 0.0 . . . . ? C39 C38 C37 C36 0.0 . . . . ? C38 C37 C36 C41 0.0 . . . . ? C38 C37 C36 C35 -178.5(4) . . . . ? C40 C41 C36 C37 0.0 . . . . ? C40 C41 C36 C35 178.5(4) . . . . ? C34 C35 C36 C37 87.8(4) . . . . ? C36 C35 C36 C37 -12.2(2) 7_565 . . . ? Cr2 C35 C36 C37 -119.7(4) . . . . ? C34 C35 C36 C41 -90.7(4) . . . . ? C36 C35 C36 C41 169.33(15) 7_565 . . . ? Cr2 C35 C36 C41 61.8(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.276 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.050 _vrf_PLAT413_klat309a ; PROBLEM: Short Inter XH3 .. XHn H23B .. H40A RESPONSE: H-atom positions on isopropyl groups are less precise because of the thermal motion. ; _vrf_PLAT220_klat309a ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) RESPONSE: The isoproyl groups have slight yet significant apparent thermal motion making their Ueq larger than most other C-atom Ueq. ; data_klat610 _database_code_depnum_ccdc_archive 'CCDC 918024' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H61 Cr N2 O' _chemical_formula_weight 649.92 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' 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 8.924(3) _cell_length_b 11.555(4) _cell_length_c 19.287(7) _cell_angle_alpha 106.796(6) _cell_angle_beta 96.988(6) _cell_angle_gamma 100.378(7) _cell_volume 1840.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9360 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 17000 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6485 _reflns_number_gt 5254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0852P)^2^+0.1073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6485 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Cr Cr 0.16407(5) -0.00167(4) 0.26750(2) 0.01893(15) Uani 1 1 d . . . N1 N 0.0686(2) -0.10391(19) 0.16222(11) 0.0186(5) Uani 1 1 d . . . N2 N 0.1560(2) 0.1638(2) 0.24113(11) 0.0193(5) Uani 1 1 d . . . O1 O 0.3206(2) 0.11096(18) 0.36461(9) 0.0247(4) Uani 1 1 d . . . C1 C 0.2196(3) -0.1472(3) 0.30076(15) 0.0269(6) Uani 1 1 d . . . C2 C 0.1255(4) -0.1744(3) 0.34699(16) 0.0322(7) Uani 1 1 d . . . C3 C -0.0080(3) -0.1141(3) 0.35346(15) 0.0304(7) Uani 1 1 d . . . C4 C -0.0203(3) -0.0350(3) 0.31478(15) 0.0271(6) Uani 1 1 d . . . C5 C 0.3577(4) -0.2042(3) 0.28774(17) 0.0368(7) Uani 1 1 d . . . H5A H 0.3216 -0.2929 0.2604 0.055 Uiso 1 1 calc R . . H5B H 0.4216 -0.1933 0.3352 0.055 Uiso 1 1 calc R . . H5C H 0.4193 -0.1632 0.2592 0.055 Uiso 1 1 calc R . . C6 C 0.1444(4) -0.2637(3) 0.39004(19) 0.0486(9) Uani 1 1 d . . . H6A H 0.2330 -0.3000 0.3783 0.073 Uiso 1 1 calc R . . H6B H 0.0501 -0.3298 0.3767 0.073 Uiso 1 1 calc R . . H6C H 0.1624 -0.2188 0.4430 0.073 Uiso 1 1 calc R . . C7 C -0.1227(4) -0.1456(4) 0.40057(18) 0.0480(9) Uani 1 1 d . . . H7A H -0.2064 -0.1019 0.3968 0.072 Uiso 1 1 calc R . . H7B H -0.0698 -0.1198 0.4520 0.072 Uiso 1 1 calc R . . H7C H -0.1661 -0.2353 0.3834 0.072 Uiso 1 1 calc R . . C8 C -0.1612(3) 0.0181(3) 0.30495(17) 0.0333(7) Uani 1 1 d . . . H8A H -0.2552 -0.0475 0.2944 0.050 Uiso 1 1 calc R . . H8B H -0.1591 0.0519 0.2639 0.050 Uiso 1 1 calc R . . H8C H -0.1608 0.0844 0.3502 0.050 Uiso 1 1 calc R . . C9 C 0.0965(3) -0.2270(2) 0.13409(13) 0.0213(6) Uani 1 1 d . . . C10 C 0.2359(3) -0.2371(3) 0.10769(14) 0.0221(6) Uani 1 1 d . . . C11 C 0.2641(3) -0.3549(3) 0.07936(15) 0.0280(6) Uani 1 1 d . . . H11A H 0.3565 -0.3631 0.0605 0.034 Uiso 1 1 calc R . . C12 C 0.1606(3) -0.4597(3) 0.07819(16) 0.0310(7) Uani 1 1 d . . . H12A H 0.1820 -0.5393 0.0590 0.037 Uiso 1 1 calc R . . C13 C 0.0259(3) -0.4488(3) 0.10501(16) 0.0300(7) Uani 1 1 d . . . H13A H -0.0446 -0.5214 0.1044 0.036 Uiso 1 1 calc R . . C14 C -0.0092(3) -0.3330(3) 0.13314(14) 0.0235(6) Uani 1 1 d . . . C15 C -0.1628(3) -0.3301(3) 0.15982(16) 0.0304(7) Uani 1 1 d . . . H15A H -0.1707 -0.2417 0.1792 0.036 Uiso 1 1 calc R . . C16 C -0.3021(3) -0.4009(3) 0.09795(18) 0.0357(7) Uani 1 1 d . . . H16A H -0.3016 -0.3632 0.0585 0.053 Uiso 1 1 calc R . . H16B H -0.3981 -0.3970 0.1175 0.053 Uiso 1 1 calc R . . H16C H -0.2957 -0.4878 0.0783 0.053 Uiso 1 1 calc R . . C17 C -0.1720(4) -0.3875(3) 0.22169(17) 0.0438(8) Uani 1 1 d . . . H17A H -0.0794 -0.3485 0.2602 0.066 Uiso 1 1 calc R . . H17B H -0.1779 -0.4768 0.2019 0.066 Uiso 1 1 calc R . . H17C H -0.2645 -0.3741 0.2427 0.066 Uiso 1 1 calc R . . C18 C 0.3531(3) -0.1224(3) 0.10828(15) 0.0244(6) Uani 1 1 d . . . H18A H 0.3500 -0.0525 0.1526 0.029 Uiso 1 1 calc R . . C19 C 0.5200(3) -0.1401(3) 0.11333(17) 0.0341(7) Uani 1 1 d . . . H19A H 0.5454 -0.1708 0.1546 0.051 Uiso 1 1 calc R . . H19B H 0.5914 -0.0605 0.1212 0.051 Uiso 1 1 calc R . . H19C H 0.5297 -0.2003 0.0674 0.051 Uiso 1 1 calc R . . C20 C 0.3097(3) -0.0844(3) 0.03991(16) 0.0335(7) Uani 1 1 d . . . H20A H 0.3914 -0.0158 0.0392 0.050 Uiso 1 1 calc R . . H20B H 0.2116 -0.0578 0.0414 0.050 Uiso 1 1 calc R . . H20C H 0.2984 -0.1553 -0.0046 0.050 Uiso 1 1 calc R . . C21 C -0.1028(3) -0.1531(3) 0.04103(14) 0.0238(6) Uani 1 1 d . . . H21A H -0.0496 -0.2209 0.0256 0.036 Uiso 1 1 calc R . . H21B H -0.1029 -0.1079 0.0052 0.036 Uiso 1 1 calc R . . H21C H -0.2098 -0.1874 0.0438 0.036 Uiso 1 1 calc R . . C22 C -0.0189(3) -0.0651(2) 0.11633(13) 0.0191(5) Uani 1 1 d . . . C23 C -0.0378(3) 0.0567(2) 0.13141(14) 0.0206(6) Uani 1 1 d . . . H23A H -0.1237 0.0679 0.1019 0.025 Uiso 1 1 calc R . . C24 C 0.0540(3) 0.1640(2) 0.18457(13) 0.0200(5) Uani 1 1 d . . . C25 C 0.0360(3) 0.2839(3) 0.17053(15) 0.0256(6) Uani 1 1 d . . . H25A H 0.0750 0.3535 0.2162 0.038 Uiso 1 1 calc R . . H25B H -0.0738 0.2788 0.1536 0.038 Uiso 1 1 calc R . . H25C H 0.0951 0.2966 0.1327 0.038 Uiso 1 1 calc R . . C26 C 0.2645(3) 0.2801(2) 0.28138(14) 0.0209(6) Uani 1 1 d . . . C27 C 0.3953(3) 0.3166(2) 0.25216(14) 0.0239(6) Uani 1 1 d . . . C28 C 0.5019(3) 0.4271(3) 0.29205(17) 0.0331(7) Uani 1 1 d . . . H28A H 0.5904 0.4527 0.2727 0.040 Uiso 1 1 calc R . . C29 C 0.4809(4) 0.5003(3) 0.35936(17) 0.0390(8) Uani 1 1 d . . . H29A H 0.5542 0.5756 0.3858 0.047 Uiso 1 1 calc R . . C30 C 0.3522(4) 0.4631(3) 0.38790(16) 0.0348(7) Uani 1 1 d . . . H30A H 0.3388 0.5133 0.4343 0.042 Uiso 1 1 calc R . . C31 C 0.2423(3) 0.3538(3) 0.35020(15) 0.0266(6) Uani 1 1 d . . . C32 C 0.1002(3) 0.3164(3) 0.38204(15) 0.0289(6) Uani 1 1 d . . . H32A H 0.0764 0.2240 0.3694 0.035 Uiso 1 1 calc R . . C33 C -0.0432(4) 0.3519(3) 0.34894(18) 0.0367(7) Uani 1 1 d . . . H33A H -0.0720 0.3058 0.2961 0.055 Uiso 1 1 calc R . . H33B H -0.0198 0.4412 0.3561 0.055 Uiso 1 1 calc R . . H33C H -0.1294 0.3313 0.3735 0.055 Uiso 1 1 calc R . . C34 C 0.1268(4) 0.3718(3) 0.46658(17) 0.0413(8) Uani 1 1 d . . . H34A H 0.2241 0.3572 0.4882 0.062 Uiso 1 1 calc R . . H34B H 0.0407 0.3320 0.4850 0.062 Uiso 1 1 calc R . . H34C H 0.1326 0.4612 0.4804 0.062 Uiso 1 1 calc R . . C35 C 0.4276(3) 0.2408(3) 0.17854(15) 0.0266(6) Uani 1 1 d . . . H35A H 0.3427 0.1641 0.1573 0.032 Uiso 1 1 calc R . . C36 C 0.5809(3) 0.2024(3) 0.18764(16) 0.0350(7) Uani 1 1 d . . . H36A H 0.5784 0.1507 0.2200 0.053 Uiso 1 1 calc R . . H36B H 0.6653 0.2766 0.2095 0.053 Uiso 1 1 calc R . . H36C H 0.5981 0.1551 0.1394 0.053 Uiso 1 1 calc R . . C37 C 0.4302(4) 0.3146(3) 0.12362(17) 0.0383(8) Uani 1 1 d . . . H37A H 0.4391 0.2610 0.0753 0.058 Uiso 1 1 calc R . . H37B H 0.5190 0.3860 0.1414 0.058 Uiso 1 1 calc R . . H37C H 0.3341 0.3439 0.1192 0.058 Uiso 1 1 calc R . . C38 C 0.4844(3) 0.1331(3) 0.35965(15) 0.0313(7) Uani 1 1 d . . . H38A H 0.5164 0.2110 0.3481 0.038 Uiso 1 1 calc R . . H38B H 0.5044 0.0638 0.3204 0.038 Uiso 1 1 calc R . . C39 C 0.5721(4) 0.1424(4) 0.43277(18) 0.0563(11) Uani 1 1 d . . . H39A H 0.6715 0.2048 0.4459 0.068 Uiso 1 1 calc R . . H39B H 0.5932 0.0614 0.4331 0.068 Uiso 1 1 calc R . . C40 C 0.4641(4) 0.1824(4) 0.48474(17) 0.0434(8) Uani 1 1 d . . . H40A H 0.4722 0.2730 0.4987 0.052 Uiso 1 1 calc R . . H40B H 0.4855 0.1591 0.5299 0.052 Uiso 1 1 calc R . . C41 C 0.3074(3) 0.1110(3) 0.43912(14) 0.0305(7) Uani 1 1 d . . . H41A H 0.2841 0.0252 0.4414 0.037 Uiso 1 1 calc R . . H41B H 0.2247 0.1524 0.4565 0.037 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 Cr 0.0217(3) 0.0156(3) 0.0200(2) 0.00571(17) 0.00481(17) 0.00493(17) N1 0.0199(11) 0.0128(12) 0.0226(11) 0.0047(9) 0.0047(9) 0.0031(9) N2 0.0206(11) 0.0136(12) 0.0224(11) 0.0035(9) 0.0061(9) 0.0028(9) O1 0.0277(10) 0.0246(11) 0.0208(9) 0.0064(8) 0.0048(8) 0.0045(8) C1 0.0316(16) 0.0180(15) 0.0263(14) 0.0032(11) -0.0040(12) 0.0063(12) C2 0.0408(18) 0.0242(17) 0.0288(15) 0.0109(12) -0.0009(13) 0.0013(13) C3 0.0341(17) 0.0255(17) 0.0272(14) 0.0075(12) 0.0063(12) -0.0031(13) C4 0.0256(15) 0.0242(16) 0.0282(14) 0.0048(12) 0.0080(11) 0.0014(12) C5 0.0417(18) 0.0337(19) 0.0386(17) 0.0137(14) 0.0004(14) 0.0183(15) C6 0.053(2) 0.046(2) 0.049(2) 0.0291(18) -0.0035(17) 0.0029(17) C7 0.059(2) 0.046(2) 0.0421(19) 0.0192(16) 0.0223(17) 0.0013(18) C8 0.0271(16) 0.0320(18) 0.0394(17) 0.0078(14) 0.0132(13) 0.0044(13) C9 0.0268(14) 0.0151(14) 0.0219(13) 0.0053(10) 0.0012(11) 0.0076(11) C10 0.0228(14) 0.0204(15) 0.0219(13) 0.0046(11) 0.0006(10) 0.0076(11) C11 0.0292(16) 0.0241(16) 0.0284(14) 0.0019(12) 0.0042(12) 0.0119(12) C12 0.0363(17) 0.0146(15) 0.0370(16) 0.0008(12) -0.0005(13) 0.0102(12) C13 0.0313(16) 0.0198(16) 0.0376(16) 0.0090(12) 0.0016(12) 0.0058(12) C14 0.0277(15) 0.0169(15) 0.0256(13) 0.0068(11) 0.0027(11) 0.0060(11) C15 0.0344(17) 0.0171(15) 0.0403(16) 0.0081(12) 0.0150(13) 0.0033(12) C16 0.0293(17) 0.0268(17) 0.0555(19) 0.0169(15) 0.0118(14) 0.0088(13) C17 0.049(2) 0.034(2) 0.0397(18) 0.0077(15) 0.0108(15) -0.0093(16) C18 0.0237(14) 0.0206(15) 0.0280(14) 0.0046(11) 0.0067(11) 0.0065(11) C19 0.0258(16) 0.0307(18) 0.0446(17) 0.0081(14) 0.0092(13) 0.0083(13) C20 0.0330(17) 0.0342(19) 0.0385(16) 0.0179(14) 0.0112(13) 0.0069(13) C21 0.0255(14) 0.0195(15) 0.0245(13) 0.0050(11) 0.0018(11) 0.0054(11) C22 0.0147(13) 0.0183(14) 0.0241(13) 0.0073(11) 0.0044(10) 0.0016(10) C23 0.0190(13) 0.0195(15) 0.0243(13) 0.0079(11) 0.0037(10) 0.0059(11) C24 0.0231(14) 0.0155(14) 0.0229(13) 0.0054(10) 0.0080(10) 0.0067(11) C25 0.0297(15) 0.0164(15) 0.0307(14) 0.0072(11) 0.0034(11) 0.0072(12) C26 0.0241(14) 0.0125(14) 0.0261(13) 0.0049(10) 0.0054(11) 0.0056(11) C27 0.0261(15) 0.0156(15) 0.0284(14) 0.0055(11) 0.0041(11) 0.0037(11) C28 0.0290(16) 0.0241(17) 0.0400(17) 0.0057(13) 0.0084(13) -0.0031(13) C29 0.0404(19) 0.0210(17) 0.0429(18) -0.0019(13) 0.0061(14) -0.0043(14) C30 0.0429(19) 0.0205(17) 0.0325(16) -0.0030(12) 0.0066(13) 0.0048(13) C31 0.0307(15) 0.0179(15) 0.0287(14) 0.0031(11) 0.0053(12) 0.0064(12) C32 0.0336(16) 0.0208(16) 0.0309(15) 0.0027(12) 0.0109(12) 0.0084(12) C33 0.0361(18) 0.0312(19) 0.0478(18) 0.0138(15) 0.0154(14) 0.0135(14) C34 0.049(2) 0.039(2) 0.0337(17) 0.0042(14) 0.0171(14) 0.0116(16) C35 0.0248(15) 0.0219(16) 0.0298(14) 0.0049(12) 0.0086(11) 0.0006(12) C36 0.0372(18) 0.0375(19) 0.0347(16) 0.0110(14) 0.0157(13) 0.0137(14) C37 0.0380(18) 0.045(2) 0.0353(16) 0.0184(15) 0.0078(14) 0.0081(15) C38 0.0245(15) 0.0365(19) 0.0305(15) 0.0091(13) 0.0039(12) 0.0043(13) C39 0.042(2) 0.088(3) 0.0378(19) 0.0189(19) 0.0058(16) 0.015(2) C40 0.0402(19) 0.054(2) 0.0268(15) 0.0059(15) 0.0008(13) 0.0044(16) C41 0.0368(17) 0.0298(17) 0.0233(14) 0.0060(12) 0.0075(12) 0.0059(13) _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 C4 2.007(3) . ? Cr N1 2.019(2) . ? Cr C1 2.081(3) . ? Cr O1 2.1102(19) . ? Cr N2 2.126(2) . ? N1 C22 1.335(3) . ? N1 C9 1.447(3) . ? N2 C24 1.334(3) . ? N2 C26 1.446(3) . ? O1 C41 1.456(3) . ? O1 C38 1.458(3) . ? C1 C2 1.359(4) . ? C1 C5 1.512(4) . ? C2 C3 1.485(4) . ? C2 C6 1.518(4) . ? C3 C4 1.347(4) . ? C3 C7 1.513(4) . ? C4 C8 1.511(4) . ? C9 C14 1.399(4) . ? C9 C10 1.411(4) . ? C10 C11 1.393(4) . ? C10 C18 1.530(4) . ? C11 C12 1.377(4) . ? C12 C13 1.377(4) . ? C13 C14 1.399(4) . ? C14 C15 1.524(4) . ? C15 C17 1.527(4) . ? C15 C16 1.532(4) . ? C18 C19 1.535(4) . ? C18 C20 1.535(4) . ? C21 C22 1.520(3) . ? C22 C23 1.397(4) . ? C23 C24 1.398(4) . ? C24 C25 1.519(4) . ? C26 C27 1.407(4) . ? C26 C31 1.414(4) . ? C27 C28 1.394(4) . ? C27 C35 1.529(4) . ? C28 C29 1.385(4) . ? C29 C30 1.385(4) . ? C30 C31 1.391(4) . ? C31 C32 1.522(4) . ? C32 C33 1.535(4) . ? C32 C34 1.540(4) . ? C35 C36 1.519(4) . ? C35 C37 1.540(4) . ? C38 C39 1.492(4) . ? C39 C40 1.508(5) . ? C40 C41 1.509(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 C4 Cr N1 98.97(10) . . ? C4 Cr C1 82.56(12) . . ? N1 Cr C1 96.42(10) . . ? C4 Cr O1 97.10(10) . . ? N1 Cr O1 163.85(8) . . ? C1 Cr O1 84.00(9) . . ? C4 Cr N2 105.98(10) . . ? N1 Cr N2 90.12(8) . . ? C1 Cr N2 168.37(10) . . ? O1 Cr N2 87.05(8) . . ? C22 N1 C9 117.5(2) . . ? C22 N1 Cr 124.11(18) . . ? C9 N1 Cr 118.41(15) . . ? C24 N2 C26 116.7(2) . . ? C24 N2 Cr 121.32(17) . . ? C26 N2 Cr 121.89(16) . . ? C41 O1 C38 108.33(19) . . ? C41 O1 Cr 125.80(16) . . ? C38 O1 Cr 116.42(15) . . ? C2 C1 C5 122.1(3) . . ? C2 C1 Cr 109.9(2) . . ? C5 C1 Cr 127.3(2) . . ? C1 C2 C3 116.6(3) . . ? C1 C2 C6 125.0(3) . . ? C3 C2 C6 118.3(3) . . ? C4 C3 C2 116.6(3) . . ? C4 C3 C7 123.8(3) . . ? C2 C3 C7 119.6(3) . . ? C3 C4 C8 123.6(3) . . ? C3 C4 Cr 112.8(2) . . ? C8 C4 Cr 123.5(2) . . ? C14 C9 C10 120.6(2) . . ? C14 C9 N1 121.9(2) . . ? C10 C9 N1 117.6(2) . . ? C11 C10 C9 118.5(3) . . ? C11 C10 C18 120.1(2) . . ? C9 C10 C18 121.4(2) . . ? C12 C11 C10 121.3(3) . . ? C13 C12 C11 119.7(3) . . ? C12 C13 C14 121.4(3) . . ? C13 C14 C9 118.5(3) . . ? C13 C14 C15 117.7(2) . . ? C9 C14 C15 123.8(2) . . ? C14 C15 C17 111.0(3) . . ? C14 C15 C16 112.1(2) . . ? C17 C15 C16 107.9(2) . . ? C10 C18 C19 113.1(2) . . ? C10 C18 C20 111.1(2) . . ? C19 C18 C20 109.2(2) . . ? N1 C22 C23 124.2(2) . . ? N1 C22 C21 120.8(2) . . ? C23 C22 C21 115.0(2) . . ? C22 C23 C24 128.1(2) . . ? N2 C24 C23 124.1(2) . . ? N2 C24 C25 121.5(2) . . ? C23 C24 C25 114.3(2) . . ? C27 C26 C31 120.5(2) . . ? C27 C26 N2 118.9(2) . . ? C31 C26 N2 120.5(2) . . ? C28 C27 C26 118.8(3) . . ? C28 C27 C35 117.9(2) . . ? C26 C27 C35 123.3(2) . . ? C29 C28 C27 121.2(3) . . ? C28 C29 C30 119.6(3) . . ? C29 C30 C31 121.5(3) . . ? C30 C31 C26 118.4(3) . . ? C30 C31 C32 120.5(2) . . ? C26 C31 C32 121.1(2) . . ? C31 C32 C33 112.4(2) . . ? C31 C32 C34 112.9(2) . . ? C33 C32 C34 108.6(2) . . ? C36 C35 C27 111.9(2) . . ? C36 C35 C37 108.6(2) . . ? C27 C35 C37 111.1(2) . . ? O1 C38 C39 106.8(2) . . ? C38 C39 C40 103.2(3) . . ? C39 C40 C41 102.2(3) . . ? O1 C41 C40 104.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Cr N1 C22 81.8(2) . . . . ? C1 Cr N1 C22 165.3(2) . . . . ? O1 Cr N1 C22 -104.1(3) . . . . ? N2 Cr N1 C22 -24.4(2) . . . . ? C4 Cr N1 C9 -98.4(2) . . . . ? C1 Cr N1 C9 -14.9(2) . . . . ? O1 Cr N1 C9 75.7(4) . . . . ? N2 Cr N1 C9 155.43(18) . . . . ? C4 Cr N2 C24 -74.6(2) . . . . ? N1 Cr N2 C24 24.8(2) . . . . ? C1 Cr N2 C24 149.1(4) . . . . ? O1 Cr N2 C24 -171.15(19) . . . . ? C4 Cr N2 C26 108.1(2) . . . . ? N1 Cr N2 C26 -152.57(19) . . . . ? C1 Cr N2 C26 -28.2(6) . . . . ? O1 Cr N2 C26 11.52(18) . . . . ? C4 Cr O1 C41 22.8(2) . . . . ? N1 Cr O1 C41 -151.2(3) . . . . ? C1 Cr O1 C41 -58.9(2) . . . . ? N2 Cr O1 C41 128.5(2) . . . . ? C4 Cr O1 C38 165.12(19) . . . . ? N1 Cr O1 C38 -8.9(4) . . . . ? C1 Cr O1 C38 83.42(19) . . . . ? N2 Cr O1 C38 -89.14(19) . . . . ? C4 Cr C1 C2 -10.9(2) . . . . ? N1 Cr C1 C2 -109.2(2) . . . . ? O1 Cr C1 C2 87.1(2) . . . . ? N2 Cr C1 C2 127.0(4) . . . . ? C4 Cr C1 C5 178.4(3) . . . . ? N1 Cr C1 C5 80.2(2) . . . . ? O1 Cr C1 C5 -83.6(2) . . . . ? N2 Cr C1 C5 -43.7(6) . . . . ? C5 C1 C2 C3 -178.7(3) . . . . ? Cr C1 C2 C3 10.1(3) . . . . ? C5 C1 C2 C6 -0.6(5) . . . . ? Cr C1 C2 C6 -171.8(2) . . . . ? C1 C2 C3 C4 -2.1(4) . . . . ? C6 C2 C3 C4 179.6(3) . . . . ? C1 C2 C3 C7 176.6(3) . . . . ? C6 C2 C3 C7 -1.6(4) . . . . ? C2 C3 C4 C8 169.7(3) . . . . ? C7 C3 C4 C8 -9.0(5) . . . . ? C2 C3 C4 Cr -7.5(3) . . . . ? C7 C3 C4 Cr 173.8(2) . . . . ? N1 Cr C4 C3 105.4(2) . . . . ? C1 Cr C4 C3 10.0(2) . . . . ? O1 Cr C4 C3 -72.9(2) . . . . ? N2 Cr C4 C3 -161.9(2) . . . . ? N1 Cr C4 C8 -71.8(2) . . . . ? C1 Cr C4 C8 -167.1(2) . . . . ? O1 Cr C4 C8 109.9(2) . . . . ? N2 Cr C4 C8 20.9(3) . . . . ? C22 N1 C9 C14 -83.9(3) . . . . ? Cr N1 C9 C14 96.3(2) . . . . ? C22 N1 C9 C10 96.4(3) . . . . ? Cr N1 C9 C10 -83.4(2) . . . . ? C14 C9 C10 C11 1.3(4) . . . . ? N1 C9 C10 C11 -179.1(2) . . . . ? C14 C9 C10 C18 -180.0(2) . . . . ? N1 C9 C10 C18 -0.3(3) . . . . ? C9 C10 C11 C12 -1.3(4) . . . . ? C18 C10 C11 C12 180.0(2) . . . . ? C10 C11 C12 C13 0.4(4) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C9 -0.5(4) . . . . ? C12 C13 C14 C15 178.5(3) . . . . ? C10 C9 C14 C13 -0.4(4) . . . . ? N1 C9 C14 C13 179.9(2) . . . . ? C10 C9 C14 C15 -179.3(2) . . . . ? N1 C9 C14 C15 1.1(4) . . . . ? C13 C14 C15 C17 59.6(3) . . . . ? C9 C14 C15 C17 -121.5(3) . . . . ? C13 C14 C15 C16 -61.2(3) . . . . ? C9 C14 C15 C16 117.7(3) . . . . ? C11 C10 C18 C19 -28.5(3) . . . . ? C9 C10 C18 C19 152.8(2) . . . . ? C11 C10 C18 C20 94.6(3) . . . . ? C9 C10 C18 C20 -84.1(3) . . . . ? C9 N1 C22 C23 -170.3(2) . . . . ? Cr N1 C22 C23 9.5(4) . . . . ? C9 N1 C22 C21 7.8(3) . . . . ? Cr N1 C22 C21 -172.41(17) . . . . ? N1 C22 C23 C24 17.3(4) . . . . ? C21 C22 C23 C24 -160.9(3) . . . . ? C26 N2 C24 C23 166.9(2) . . . . ? Cr N2 C24 C23 -10.5(3) . . . . ? C26 N2 C24 C25 -9.3(3) . . . . ? Cr N2 C24 C25 173.26(18) . . . . ? C22 C23 C24 N2 -15.9(4) . . . . ? C22 C23 C24 C25 160.6(3) . . . . ? C24 N2 C26 C27 -80.0(3) . . . . ? Cr N2 C26 C27 97.5(2) . . . . ? C24 N2 C26 C31 102.2(3) . . . . ? Cr N2 C26 C31 -80.4(3) . . . . ? C31 C26 C27 C28 -0.4(4) . . . . ? N2 C26 C27 C28 -178.3(2) . . . . ? C31 C26 C27 C35 179.4(2) . . . . ? N2 C26 C27 C35 1.5(4) . . . . ? C26 C27 C28 C29 0.2(4) . . . . ? C35 C27 C28 C29 -179.6(3) . . . . ? C27 C28 C29 C30 0.3(5) . . . . ? C28 C29 C30 C31 -0.5(5) . . . . ? C29 C30 C31 C26 0.2(5) . . . . ? C29 C30 C31 C32 -178.7(3) . . . . ? C27 C26 C31 C30 0.2(4) . . . . ? N2 C26 C31 C30 178.1(2) . . . . ? C27 C26 C31 C32 179.2(2) . . . . ? N2 C26 C31 C32 -3.0(4) . . . . ? C30 C31 C32 C33 98.0(3) . . . . ? C26 C31 C32 C33 -81.0(3) . . . . ? C30 C31 C32 C34 -25.4(4) . . . . ? C26 C31 C32 C34 155.7(3) . . . . ? C28 C27 C35 C36 59.4(3) . . . . ? C26 C27 C35 C36 -120.4(3) . . . . ? C28 C27 C35 C37 -62.1(3) . . . . ? C26 C27 C35 C37 118.1(3) . . . . ? C41 O1 C38 C39 1.9(3) . . . . ? Cr O1 C38 C39 -146.6(2) . . . . ? O1 C38 C39 C40 -24.8(4) . . . . ? C38 C39 C40 C41 37.4(4) . . . . ? C38 O1 C41 C40 21.8(3) . . . . ? Cr O1 C41 C40 166.59(19) . . . . ? C39 C40 C41 O1 -36.6(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.854 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.078 data_klat636s _database_code_depnum_ccdc_archive 'CCDC 918025' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H75 Cr N2 O' _chemical_formula_weight 880.21 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' 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 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 13.834(4) _cell_length_b 17.440(5) _cell_length_c 20.034(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.087(5) _cell_angle_gamma 90.00 _cell_volume 4688(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 992 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 20.78 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 0.288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8989 _exptl_absorpt_correction_T_max 0.9452 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 33066 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8258 _reflns_number_gt 6210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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. H1-H4 were located from the diff. map and refined riding thermal parameters. ; _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^)+(0.1057P)^2^+1.9352P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8258 _refine_ls_number_parameters 500 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.053 _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 Cr Cr 0.30297(3) 0.02430(2) 0.32134(2) 0.02792(16) Uani 1 1 d . . . N1 N 0.18203(16) 0.10402(13) 0.29890(11) 0.0324(5) Uani 1 1 d . . . N2 N 0.20468(17) -0.06128(14) 0.28011(12) 0.0343(5) Uani 1 1 d . . . O1 O 0.38365(13) 0.11111(10) 0.38620(9) 0.0320(4) Uani 1 1 d . . . C1 C 0.4057(2) -0.05188(16) 0.38055(14) 0.0313(6) Uani 1 1 d D . . H1 H 0.390(2) -0.1017(13) 0.3608(15) 0.047 Uiso 1 1 d D . . H2 H 0.402(2) -0.0513(18) 0.4280(11) 0.047 Uiso 1 1 d D . . C2 C 0.5094(2) -0.02979(15) 0.37330(15) 0.0309(6) Uani 1 1 d D . . H3 H 0.558(2) -0.0707(15) 0.3819(16) 0.046 Uiso 1 1 d D . . H4 H 0.538(2) 0.0065(16) 0.4093(13) 0.046 Uiso 1 1 d D . . C3 C 0.5024(2) 0.00252(15) 0.30248(14) 0.0306(6) Uani 1 1 d . . . C4 C 0.4111(2) 0.02618(15) 0.26713(14) 0.0302(6) Uani 1 1 d . . . C5 C 0.5979(2) 0.00800(15) 0.28075(17) 0.0396(7) Uani 1 1 d . . . C6 C 0.6847(2) 0.02706(17) 0.3284(2) 0.0543(9) Uani 1 1 d . . . H6A H 0.6830 0.0369 0.3747 0.065 Uiso 1 1 calc R . . C7 C 0.7751(3) 0.0320(2) 0.3092(3) 0.0871(17) Uani 1 1 d . . . H7A H 0.8341 0.0450 0.3428 0.105 Uiso 1 1 calc R . . C8 C 0.7802(5) 0.0186(2) 0.2434(4) 0.112(3) Uani 1 1 d . . . H8A H 0.8418 0.0228 0.2306 0.135 Uiso 1 1 calc R . . C9 C 0.6946(5) -0.0012(2) 0.1956(3) 0.100(2) Uani 1 1 d . . . H9A H 0.6977 -0.0110 0.1495 0.120 Uiso 1 1 calc R . . C10 C 0.6038(3) -0.00705(18) 0.2129(2) 0.0613(11) Uani 1 1 d . . . H10A H 0.5457 -0.0212 0.1791 0.074 Uiso 1 1 calc R . . C11 C 0.3901(2) 0.06612(18) 0.20005(14) 0.0401(7) Uani 1 1 d . . . C12 C 0.4516(2) 0.12506(18) 0.18579(15) 0.0429(7) Uani 1 1 d . . . H12A H 0.5088 0.1399 0.2202 0.051 Uiso 1 1 calc R . . C13 C 0.4308(3) 0.1618(3) 0.12302(19) 0.0690(12) Uani 1 1 d . . . H13A H 0.4741 0.2008 0.1144 0.083 Uiso 1 1 calc R . . C14 C 0.3475(4) 0.1423(3) 0.0729(2) 0.0986(19) Uani 1 1 d . . . H14A H 0.3339 0.1671 0.0293 0.118 Uiso 1 1 calc R . . C15 C 0.2840(4) 0.0869(3) 0.08590(19) 0.0931(18) Uani 1 1 d . . . H15A H 0.2255 0.0745 0.0517 0.112 Uiso 1 1 calc R . . C16 C 0.3044(3) 0.0489(2) 0.14840(17) 0.0636(11) Uani 1 1 d . . . H16A H 0.2597 0.0107 0.1565 0.076 Uiso 1 1 calc R . . C17 C 0.1888(2) 0.17812(16) 0.33272(15) 0.0339(6) Uani 1 1 d . . . C18 C 0.2196(2) 0.24239(18) 0.30104(16) 0.0404(7) Uani 1 1 d . . . C19 C 0.2188(2) 0.31356(19) 0.33275(17) 0.0469(8) Uani 1 1 d . . . H19A H 0.2376 0.3579 0.3115 0.056 Uiso 1 1 calc R . . C20 C 0.1914(2) 0.32124(19) 0.39379(18) 0.0474(8) Uani 1 1 d . . . H20A H 0.1908 0.3704 0.4141 0.057 Uiso 1 1 calc R . . C21 C 0.1648(2) 0.25724(18) 0.42538(17) 0.0443(8) Uani 1 1 d . . . H21A H 0.1470 0.2626 0.4680 0.053 Uiso 1 1 calc R . . C22 C 0.1635(2) 0.18479(18) 0.39608(17) 0.0424(7) Uani 1 1 d . . . C23 C 0.1365(3) 0.1159(2) 0.4351(2) 0.0653(11) Uani 1 1 d . . . H23A H 0.1723 0.0708 0.4217 0.078 Uiso 1 1 calc R . . C24 C 0.1693(4) 0.1213(3) 0.5123(2) 0.0795(14) Uani 1 1 d . . . H24A H 0.1596 0.0716 0.5326 0.119 Uiso 1 1 calc R . . H24B H 0.1297 0.1604 0.5286 0.119 Uiso 1 1 calc R . . H24C H 0.2400 0.1354 0.5259 0.119 Uiso 1 1 calc R . . C25 C 0.0309(4) 0.0973(3) 0.4151(2) 0.0883(15) Uani 1 1 d . . . H25A H 0.0156 0.0592 0.4470 0.132 Uiso 1 1 calc R . . H25B H 0.0142 0.0764 0.3683 0.132 Uiso 1 1 calc R . . H25C H -0.0083 0.1438 0.4166 0.132 Uiso 1 1 calc R . . C26 C 0.2535(3) 0.2366(2) 0.23405(16) 0.0531(9) Uani 1 1 d . . . H26A H 0.2884 0.1863 0.2346 0.064 Uiso 1 1 calc R . . C27 C 0.1685(4) 0.2388(4) 0.1688(2) 0.109(2) Uani 1 1 d . . . H27A H 0.1313 0.1905 0.1644 0.164 Uiso 1 1 calc R . . H27B H 0.1961 0.2458 0.1285 0.164 Uiso 1 1 calc R . . H27C H 0.1237 0.2815 0.1717 0.164 Uiso 1 1 calc R . . C28 C 0.3281(3) 0.3000(2) 0.22761(19) 0.0552(9) Uani 1 1 d . . . H28A H 0.3785 0.3048 0.2712 0.083 Uiso 1 1 calc R . . H28B H 0.2927 0.3488 0.2166 0.083 Uiso 1 1 calc R . . H28C H 0.3607 0.2867 0.1909 0.083 Uiso 1 1 calc R . . C29 C 0.0109(2) 0.1493(2) 0.23999(19) 0.0535(9) Uani 1 1 d . . . H29A H 0.0392 0.2007 0.2505 0.080 Uiso 1 1 calc R . . H29B H -0.0353 0.1384 0.2689 0.080 Uiso 1 1 calc R . . H29C H -0.0249 0.1467 0.1914 0.080 Uiso 1 1 calc R . . C30 C 0.0945(2) 0.09021(18) 0.25433(15) 0.0381(7) Uani 1 1 d . . . C31 C 0.0696(2) 0.02013(19) 0.22078(16) 0.0434(8) Uani 1 1 d . . . H31A H 0.0142 0.0210 0.1819 0.052 Uiso 1 1 calc R . . C32 C 0.1151(2) -0.05035(19) 0.23678(15) 0.0405(7) Uani 1 1 d . . . C33 C 0.0528(2) -0.1196(2) 0.20407(19) 0.0579(10) Uani 1 1 d . . . H33A H 0.0898 -0.1487 0.1766 0.087 Uiso 1 1 calc R . . H33B H -0.0103 -0.1017 0.1744 0.087 Uiso 1 1 calc R . . H33C H 0.0392 -0.1525 0.2404 0.087 Uiso 1 1 calc R . . C34 C 0.2260(2) -0.14029(16) 0.30290(15) 0.0366(7) Uani 1 1 d . . . C35 C 0.2064(3) -0.16168(18) 0.36543(18) 0.0523(9) Uani 1 1 d . . . C36 C 0.2247(4) -0.2368(2) 0.3882(2) 0.0699(12) Uani 1 1 d . . . H36A H 0.2115 -0.2516 0.4308 0.084 Uiso 1 1 calc R . . C37 C 0.2618(3) -0.2904(2) 0.3500(2) 0.0624(10) Uani 1 1 d . . . H37A H 0.2735 -0.3417 0.3659 0.075 Uiso 1 1 calc R . . C38 C 0.2817(2) -0.26840(18) 0.28871(17) 0.0468(8) Uani 1 1 d . . . H38A H 0.3073 -0.3052 0.2626 0.056 Uiso 1 1 calc R . . C39 C 0.2653(2) -0.19361(17) 0.26392(15) 0.0378(7) Uani 1 1 d . . . C40 C 0.2924(2) -0.17337(19) 0.19736(16) 0.0458(8) Uani 1 1 d . . . H40A H 0.2665 -0.1208 0.1833 0.055 Uiso 1 1 calc R . . C41 C 0.4053(2) -0.17240(18) 0.20779(18) 0.0457(8) Uani 1 1 d . . . H41A H 0.4348 -0.1375 0.2456 0.069 Uiso 1 1 calc R . . H41B H 0.4220 -0.1548 0.1655 0.069 Uiso 1 1 calc R . . H41C H 0.4317 -0.2242 0.2190 0.069 Uiso 1 1 calc R . . C42 C 0.2471(3) -0.2295(3) 0.13835(19) 0.0664(11) Uani 1 1 d . . . H42A H 0.1748 -0.2320 0.1324 0.100 Uiso 1 1 calc R . . H42B H 0.2759 -0.2807 0.1497 0.100 Uiso 1 1 calc R . . H42C H 0.2621 -0.2116 0.0956 0.100 Uiso 1 1 calc R . . C43 C 0.1633(4) -0.1058(2) 0.4087(2) 0.0737(14) Uani 1 1 d . . . H43A H 0.1738 -0.0529 0.3925 0.088 Uiso 1 1 calc R . . C44 C 0.0518(4) -0.1177(3) 0.3966(2) 0.0881(15) Uani 1 1 d . . . H44A H 0.0206 -0.1137 0.3473 0.132 Uiso 1 1 calc R . . H44B H 0.0240 -0.0785 0.4216 0.132 Uiso 1 1 calc R . . H44C H 0.0389 -0.1687 0.4131 0.132 Uiso 1 1 calc R . . C45 C 0.2131(4) -0.1093(3) 0.4856(2) 0.0899(16) Uani 1 1 d . . . H45A H 0.1850 -0.0695 0.5097 0.135 Uiso 1 1 calc R . . H45B H 0.2850 -0.1010 0.4927 0.135 Uiso 1 1 calc R . . H45C H 0.2014 -0.1598 0.5036 0.135 Uiso 1 1 calc R . . C46 C 0.4044(3) 0.10739(19) 0.46054(14) 0.0447(8) Uani 1 1 d . . . H46A H 0.4555 0.0678 0.4784 0.054 Uiso 1 1 calc R . . H46B H 0.3432 0.0944 0.4754 0.054 Uiso 1 1 calc R . . C47 C 0.4415(3) 0.1846(2) 0.48656(17) 0.0568(9) Uani 1 1 d . . . H47A H 0.3877 0.2149 0.4986 0.068 Uiso 1 1 calc R . . H47B H 0.4976 0.1800 0.5279 0.068 Uiso 1 1 calc R . . C48 C 0.4751(4) 0.2216(3) 0.4292(2) 0.105(2) Uani 1 1 d . . . H48A H 0.5474 0.2324 0.4433 0.126 Uiso 1 1 calc R . . H48B H 0.4392 0.2705 0.4162 0.126 Uiso 1 1 calc R . . C49 C 0.4527(2) 0.16694(16) 0.37024(15) 0.0366(7) Uani 1 1 d . . . H49A H 0.4220 0.1942 0.3269 0.044 Uiso 1 1 calc R . . H49B H 0.5144 0.1414 0.3651 0.044 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 Cr 0.0228(3) 0.0341(3) 0.0259(3) 0.00085(17) 0.00398(18) -0.00575(17) N1 0.0229(12) 0.0422(13) 0.0310(12) 0.0045(10) 0.0043(10) -0.0028(10) N2 0.0282(13) 0.0422(13) 0.0334(13) -0.0081(10) 0.0094(10) -0.0110(10) O1 0.0266(10) 0.0398(10) 0.0277(10) -0.0010(8) 0.0027(8) -0.0044(8) C1 0.0291(15) 0.0347(14) 0.0300(15) 0.0022(12) 0.0067(12) -0.0039(12) C2 0.0256(15) 0.0280(14) 0.0398(16) 0.0002(12) 0.0092(12) 0.0002(11) C3 0.0338(16) 0.0257(13) 0.0347(15) -0.0060(11) 0.0133(13) -0.0066(11) C4 0.0324(16) 0.0318(14) 0.0286(14) -0.0072(11) 0.0114(12) -0.0103(11) C5 0.0435(19) 0.0234(13) 0.060(2) -0.0037(13) 0.0291(16) -0.0023(12) C6 0.0348(19) 0.0379(17) 0.097(3) -0.0005(17) 0.0304(19) -0.0027(14) C7 0.044(2) 0.042(2) 0.190(6) 0.000(3) 0.058(3) -0.0046(16) C8 0.110(4) 0.028(2) 0.253(8) -0.006(3) 0.147(5) -0.008(2) C9 0.151(5) 0.0289(19) 0.172(5) -0.014(2) 0.143(5) -0.016(3) C10 0.090(3) 0.0293(16) 0.087(3) -0.0092(17) 0.064(2) -0.0104(17) C11 0.0406(18) 0.0536(18) 0.0267(15) -0.0011(13) 0.0092(13) -0.0145(14) C12 0.0396(18) 0.0559(19) 0.0307(15) 0.0043(14) 0.0040(13) -0.0125(14) C13 0.058(2) 0.099(3) 0.045(2) 0.024(2) 0.0053(18) -0.029(2) C14 0.083(3) 0.166(5) 0.034(2) 0.040(3) -0.011(2) -0.056(3) C15 0.080(3) 0.155(5) 0.0303(19) 0.019(2) -0.0133(19) -0.057(3) C16 0.058(2) 0.096(3) 0.0319(17) 0.0017(18) 0.0011(16) -0.043(2) C17 0.0201(14) 0.0403(15) 0.0391(16) 0.0047(12) 0.0030(12) 0.0054(11) C18 0.0261(16) 0.0491(18) 0.0413(17) 0.0080(14) -0.0011(13) -0.0036(13) C19 0.0405(19) 0.0467(18) 0.049(2) 0.0085(15) 0.0033(15) -0.0067(14) C20 0.0358(18) 0.0425(17) 0.058(2) 0.0002(15) 0.0000(15) 0.0049(14) C21 0.0393(18) 0.0450(18) 0.0514(19) 0.0017(14) 0.0164(15) 0.0093(14) C22 0.0355(17) 0.0430(17) 0.0523(19) 0.0049(14) 0.0173(14) 0.0094(13) C23 0.098(3) 0.0442(19) 0.072(3) -0.0049(17) 0.056(2) 0.0033(19) C24 0.089(3) 0.090(3) 0.077(3) 0.034(2) 0.056(3) 0.036(3) C25 0.105(4) 0.095(3) 0.072(3) 0.000(2) 0.035(3) -0.037(3) C26 0.051(2) 0.067(2) 0.0387(18) 0.0064(16) 0.0070(16) -0.0212(17) C27 0.086(3) 0.190(6) 0.041(2) 0.026(3) -0.006(2) -0.073(4) C28 0.057(2) 0.0485(19) 0.062(2) 0.0095(16) 0.0186(18) -0.0061(16) C29 0.0277(17) 0.064(2) 0.061(2) 0.0193(17) -0.0033(15) -0.0022(15) C30 0.0259(16) 0.0515(18) 0.0352(16) 0.0084(13) 0.0039(12) -0.0041(13) C31 0.0244(16) 0.070(2) 0.0322(16) -0.0004(15) 0.0000(12) -0.0094(14) C32 0.0270(16) 0.062(2) 0.0326(16) -0.0121(14) 0.0078(13) -0.0131(14) C33 0.0322(18) 0.074(2) 0.065(2) -0.0327(19) 0.0065(16) -0.0151(16) C34 0.0298(16) 0.0418(16) 0.0388(16) -0.0100(13) 0.0096(13) -0.0171(12) C35 0.071(2) 0.0417(18) 0.055(2) -0.0132(15) 0.0358(18) -0.0304(16) C36 0.121(4) 0.043(2) 0.061(2) -0.0086(17) 0.053(2) -0.034(2) C37 0.091(3) 0.0424(19) 0.061(2) -0.0028(17) 0.033(2) -0.0201(19) C38 0.047(2) 0.0431(18) 0.053(2) -0.0100(15) 0.0162(16) -0.0094(14) C39 0.0288(16) 0.0451(17) 0.0390(16) -0.0068(13) 0.0072(13) -0.0096(12) C40 0.048(2) 0.0532(19) 0.0390(17) 0.0000(14) 0.0155(15) 0.0078(15) C41 0.049(2) 0.0383(16) 0.057(2) -0.0029(14) 0.0271(16) 0.0004(14) C42 0.052(2) 0.101(3) 0.046(2) -0.019(2) 0.0104(17) 0.004(2) C43 0.135(4) 0.0389(19) 0.072(3) -0.0112(17) 0.073(3) -0.031(2) C44 0.124(4) 0.088(3) 0.068(3) 0.007(2) 0.052(3) 0.039(3) C45 0.113(4) 0.106(3) 0.071(3) -0.044(3) 0.060(3) -0.056(3) C46 0.049(2) 0.0575(19) 0.0265(15) -0.0067(13) 0.0069(14) 0.0068(15) C47 0.070(3) 0.055(2) 0.0385(18) -0.0104(15) 0.0001(17) 0.0076(18) C48 0.132(5) 0.121(4) 0.071(3) -0.050(3) 0.044(3) -0.083(4) C49 0.0351(17) 0.0333(15) 0.0402(16) -0.0028(12) 0.0068(13) -0.0065(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C4 2.051(3) . ? Cr N2 2.052(2) . ? Cr C1 2.091(3) . ? Cr O1 2.1260(18) . ? Cr N1 2.137(2) . ? N1 C30 1.340(4) . ? N1 C17 1.452(4) . ? N2 C32 1.343(4) . ? N2 C34 1.459(4) . ? O1 C46 1.448(3) . ? O1 C49 1.453(3) . ? C1 C2 1.526(4) . ? C2 C3 1.508(4) . ? C3 C4 1.354(4) . ? C3 C5 1.491(4) . ? C4 C11 1.478(4) . ? C5 C6 1.381(5) . ? C5 C10 1.405(5) . ? C6 C7 1.398(5) . ? C7 C8 1.359(8) . ? C8 C9 1.373(9) . ? C9 C10 1.387(6) . ? C11 C16 1.403(4) . ? C11 C12 1.407(4) . ? C12 C13 1.378(5) . ? C13 C14 1.374(5) . ? C14 C15 1.373(6) . ? C15 C16 1.384(5) . ? C17 C22 1.401(4) . ? C17 C18 1.405(4) . ? C18 C19 1.396(5) . ? C18 C26 1.529(5) . ? C19 C20 1.372(5) . ? C20 C21 1.377(5) . ? C21 C22 1.391(4) . ? C22 C23 1.529(5) . ? C23 C25 1.454(6) . ? C23 C24 1.505(6) . ? C26 C27 1.531(5) . ? C26 C28 1.539(4) . ? C29 C30 1.523(4) . ? C30 C31 1.397(4) . ? C31 C32 1.383(5) . ? C32 C33 1.534(4) . ? C34 C35 1.396(4) . ? C34 C39 1.406(4) . ? C35 C36 1.390(5) . ? C35 C43 1.519(5) . ? C36 C37 1.384(5) . ? C37 C38 1.377(5) . ? C38 C39 1.394(4) . ? C39 C40 1.512(4) . ? C40 C41 1.524(5) . ? C40 C42 1.546(5) . ? C43 C44 1.516(7) . ? C43 C45 1.528(6) . ? C46 C47 1.490(5) . ? C47 C48 1.486(6) . ? C48 C49 1.491(5) . ? 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 C4 Cr N2 107.19(10) . . ? C4 Cr C1 80.11(11) . . ? N2 Cr C1 93.35(11) . . ? C4 Cr O1 88.30(9) . . ? N2 Cr O1 164.08(8) . . ? C1 Cr O1 85.56(10) . . ? C4 Cr N1 120.82(10) . . ? N2 Cr N1 88.87(10) . . ? C1 Cr N1 157.20(10) . . ? O1 Cr N1 86.15(8) . . ? C30 N1 C17 114.6(2) . . ? C30 N1 Cr 123.9(2) . . ? C17 N1 Cr 121.52(17) . . ? C32 N2 C34 114.9(2) . . ? C32 N2 Cr 125.0(2) . . ? C34 N2 Cr 119.81(17) . . ? C46 O1 C49 106.2(2) . . ? C46 O1 Cr 122.68(17) . . ? C49 O1 Cr 128.19(16) . . ? C2 C1 Cr 108.08(18) . . ? C3 C2 C1 109.7(2) . . ? C4 C3 C5 127.5(3) . . ? C4 C3 C2 116.3(2) . . ? C5 C3 C2 116.1(3) . . ? C3 C4 C11 124.8(2) . . ? C3 C4 Cr 115.2(2) . . ? C11 C4 Cr 118.8(2) . . ? C6 C5 C10 117.9(3) . . ? C6 C5 C3 119.8(3) . . ? C10 C5 C3 122.3(3) . . ? C5 C6 C7 120.7(4) . . ? C8 C7 C6 121.2(5) . . ? C7 C8 C9 118.7(4) . . ? C8 C9 C10 121.6(5) . . ? C9 C10 C5 119.9(5) . . ? C16 C11 C12 116.8(3) . . ? C16 C11 C4 120.9(3) . . ? C12 C11 C4 122.3(3) . . ? C13 C12 C11 121.5(3) . . ? C14 C13 C12 120.3(3) . . ? C15 C14 C13 119.7(3) . . ? C14 C15 C16 120.7(4) . . ? C15 C16 C11 121.0(3) . . ? C22 C17 C18 120.9(3) . . ? C22 C17 N1 119.7(2) . . ? C18 C17 N1 119.4(3) . . ? C19 C18 C17 117.8(3) . . ? C19 C18 C26 119.8(3) . . ? C17 C18 C26 122.4(3) . . ? C20 C19 C18 121.8(3) . . ? C19 C20 C21 119.5(3) . . ? C20 C21 C22 121.3(3) . . ? C21 C22 C17 118.5(3) . . ? C21 C22 C23 118.5(3) . . ? C17 C22 C23 123.0(3) . . ? C25 C23 C24 109.2(3) . . ? C25 C23 C22 112.9(4) . . ? C24 C23 C22 115.2(3) . . ? C18 C26 C27 114.3(3) . . ? C18 C26 C28 112.4(3) . . ? C27 C26 C28 107.6(3) . . ? N1 C30 C31 123.7(3) . . ? N1 C30 C29 121.7(3) . . ? C31 C30 C29 114.4(3) . . ? C32 C31 C30 128.4(3) . . ? N2 C32 C31 124.9(3) . . ? N2 C32 C33 119.9(3) . . ? C31 C32 C33 115.1(3) . . ? C35 C34 C39 120.5(3) . . ? C35 C34 N2 117.7(3) . . ? C39 C34 N2 121.8(3) . . ? C36 C35 C34 119.1(3) . . ? C36 C35 C43 118.9(3) . . ? C34 C35 C43 122.0(3) . . ? C37 C36 C35 121.2(3) . . ? C38 C37 C36 119.2(3) . . ? C37 C38 C39 121.8(3) . . ? C38 C39 C34 118.2(3) . . ? C38 C39 C40 118.6(3) . . ? C34 C39 C40 123.2(3) . . ? C39 C40 C41 110.3(3) . . ? C39 C40 C42 112.6(3) . . ? C41 C40 C42 108.8(3) . . ? C44 C43 C35 110.2(3) . . ? C44 C43 C45 110.3(3) . . ? C35 C43 C45 113.9(4) . . ? O1 C46 C47 106.5(3) . . ? C48 C47 C46 105.5(3) . . ? C47 C48 C49 107.0(3) . . ? O1 C49 C48 106.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Cr N1 C30 91.7(2) . . . . ? N2 Cr N1 C30 -17.7(2) . . . . ? C1 Cr N1 C30 -113.7(3) . . . . ? O1 Cr N1 C30 177.4(2) . . . . ? C4 Cr N1 C17 -89.4(2) . . . . ? N2 Cr N1 C17 161.2(2) . . . . ? C1 Cr N1 C17 65.2(3) . . . . ? O1 Cr N1 C17 -3.72(19) . . . . ? C4 Cr N2 C32 -102.0(2) . . . . ? C1 Cr N2 C32 177.3(2) . . . . ? O1 Cr N2 C32 91.7(4) . . . . ? N1 Cr N2 C32 20.0(2) . . . . ? C4 Cr N2 C34 84.2(2) . . . . ? C1 Cr N2 C34 3.5(2) . . . . ? O1 Cr N2 C34 -82.1(4) . . . . ? N1 Cr N2 C34 -153.8(2) . . . . ? C4 Cr O1 C46 -133.0(2) . . . . ? N2 Cr O1 C46 33.9(4) . . . . ? C1 Cr O1 C46 -52.8(2) . . . . ? N1 Cr O1 C46 106.0(2) . . . . ? C4 Cr O1 C49 25.1(2) . . . . ? N2 Cr O1 C49 -168.1(3) . . . . ? C1 Cr O1 C49 105.3(2) . . . . ? N1 Cr O1 C49 -96.0(2) . . . . ? C4 Cr C1 C2 28.31(19) . . . . ? N2 Cr C1 C2 135.19(19) . . . . ? O1 Cr C1 C2 -60.73(19) . . . . ? N1 Cr C1 C2 -129.7(2) . . . . ? Cr C1 C2 C3 -32.4(3) . . . . ? C1 C2 C3 C4 17.9(3) . . . . ? C1 C2 C3 C5 -164.7(2) . . . . ? C5 C3 C4 C11 -3.1(4) . . . . ? C2 C3 C4 C11 173.9(2) . . . . ? C5 C3 C4 Cr -170.5(2) . . . . ? C2 C3 C4 Cr 6.5(3) . . . . ? N2 Cr C4 C3 -110.7(2) . . . . ? C1 Cr C4 C3 -20.2(2) . . . . ? O1 Cr C4 C3 65.5(2) . . . . ? N1 Cr C4 C3 150.04(18) . . . . ? N2 Cr C4 C11 81.1(2) . . . . ? C1 Cr C4 C11 171.5(2) . . . . ? O1 Cr C4 C11 -102.7(2) . . . . ? N1 Cr C4 C11 -18.2(2) . . . . ? C4 C3 C5 C6 140.3(3) . . . . ? C2 C3 C5 C6 -36.6(4) . . . . ? C4 C3 C5 C10 -40.9(4) . . . . ? C2 C3 C5 C10 142.1(3) . . . . ? C10 C5 C6 C7 0.8(5) . . . . ? C3 C5 C6 C7 179.6(3) . . . . ? C5 C6 C7 C8 0.3(6) . . . . ? C6 C7 C8 C9 -0.9(6) . . . . ? C7 C8 C9 C10 0.5(6) . . . . ? C8 C9 C10 C5 0.5(6) . . . . ? C6 C5 C10 C9 -1.1(5) . . . . ? C3 C5 C10 C9 -179.9(3) . . . . ? C3 C4 C11 C16 140.2(3) . . . . ? Cr C4 C11 C16 -52.8(4) . . . . ? C3 C4 C11 C12 -42.8(4) . . . . ? Cr C4 C11 C12 124.2(3) . . . . ? C16 C11 C12 C13 -2.7(5) . . . . ? C4 C11 C12 C13 -179.8(3) . . . . ? C11 C12 C13 C14 1.2(7) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? C13 C14 C15 C16 -1.8(9) . . . . ? C14 C15 C16 C11 0.2(8) . . . . ? C12 C11 C16 C15 2.0(6) . . . . ? C4 C11 C16 C15 179.2(4) . . . . ? C30 N1 C17 C22 92.1(3) . . . . ? Cr N1 C17 C22 -86.9(3) . . . . ? C30 N1 C17 C18 -87.3(3) . . . . ? Cr N1 C17 C18 93.8(3) . . . . ? C22 C17 C18 C19 -3.6(4) . . . . ? N1 C17 C18 C19 175.8(3) . . . . ? C22 C17 C18 C26 176.4(3) . . . . ? N1 C17 C18 C26 -4.3(4) . . . . ? C17 C18 C19 C20 1.7(5) . . . . ? C26 C18 C19 C20 -178.3(3) . . . . ? C18 C19 C20 C21 0.6(5) . . . . ? C19 C20 C21 C22 -1.1(5) . . . . ? C20 C21 C22 C17 -0.8(5) . . . . ? C20 C21 C22 C23 178.1(3) . . . . ? C18 C17 C22 C21 3.2(4) . . . . ? N1 C17 C22 C21 -176.2(3) . . . . ? C18 C17 C22 C23 -175.6(3) . . . . ? N1 C17 C22 C23 5.0(5) . . . . ? C21 C22 C23 C25 93.0(4) . . . . ? C17 C22 C23 C25 -88.2(4) . . . . ? C21 C22 C23 C24 -33.4(5) . . . . ? C17 C22 C23 C24 145.4(3) . . . . ? C19 C18 C26 C27 -95.2(4) . . . . ? C17 C18 C26 C27 84.8(4) . . . . ? C19 C18 C26 C28 27.8(4) . . . . ? C17 C18 C26 C28 -152.1(3) . . . . ? C17 N1 C30 C31 -174.4(3) . . . . ? Cr N1 C30 C31 4.5(4) . . . . ? C17 N1 C30 C29 1.4(4) . . . . ? Cr N1 C30 C29 -179.7(2) . . . . ? N1 C30 C31 C32 16.2(5) . . . . ? C29 C30 C31 C32 -159.9(3) . . . . ? C34 N2 C32 C31 164.7(3) . . . . ? Cr N2 C32 C31 -9.4(4) . . . . ? C34 N2 C32 C33 -11.9(4) . . . . ? Cr N2 C32 C33 174.1(2) . . . . ? C30 C31 C32 N2 -14.0(5) . . . . ? C30 C31 C32 C33 162.7(3) . . . . ? C32 N2 C34 C35 -95.1(3) . . . . ? Cr N2 C34 C35 79.3(3) . . . . ? C32 N2 C34 C39 85.1(3) . . . . ? Cr N2 C34 C39 -100.5(3) . . . . ? C39 C34 C35 C36 -1.0(5) . . . . ? N2 C34 C35 C36 179.2(3) . . . . ? C39 C34 C35 C43 -179.6(3) . . . . ? N2 C34 C35 C43 0.6(5) . . . . ? C34 C35 C36 C37 -0.1(6) . . . . ? C43 C35 C36 C37 178.6(4) . . . . ? C35 C36 C37 C38 0.6(6) . . . . ? C36 C37 C38 C39 -0.1(6) . . . . ? C37 C38 C39 C34 -0.9(5) . . . . ? C37 C38 C39 C40 177.9(3) . . . . ? C35 C34 C39 C38 1.5(4) . . . . ? N2 C34 C39 C38 -178.7(3) . . . . ? C35 C34 C39 C40 -177.3(3) . . . . ? N2 C34 C39 C40 2.5(4) . . . . ? C38 C39 C40 C41 -70.3(4) . . . . ? C34 C39 C40 C41 108.4(3) . . . . ? C38 C39 C40 C42 51.5(4) . . . . ? C34 C39 C40 C42 -129.7(3) . . . . ? C36 C35 C43 C44 -79.7(5) . . . . ? C34 C35 C43 C44 98.9(4) . . . . ? C36 C35 C43 C45 44.9(5) . . . . ? C34 C35 C43 C45 -136.5(3) . . . . ? C49 O1 C46 C47 29.9(3) . . . . ? Cr O1 C46 C47 -167.9(2) . . . . ? O1 C46 C47 C48 -19.8(4) . . . . ? C46 C47 C48 C49 2.5(5) . . . . ? C46 O1 C49 C48 -28.0(4) . . . . ? Cr O1 C49 C48 171.1(3) . . . . ? C47 C48 C49 O1 15.5(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.906 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.062 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.013 0.000 0.000 445.1 55.0 2 -0.079 0.500 0.500 445.1 55.1 _platon_squeeze_details ; Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 Void space analysis is consistent with 2 molecules of cocrystallized pentane per compound molecule. ; _vrf_CHEMW03_klat636s ; PROBLEM: WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: 2 molecules of cocrystallized pentane per compound molecule were treated as bulk solvent. See _platon_squeeze_details. ; data_klat305 _database_code_depnum_ccdc_archive 'CCDC 918026' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H108 Cr2 N4 O Si2' _chemical_formula_weight 1157.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.404(5) _cell_length_b 14.089(5) _cell_length_c 18.924(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.268(7) _cell_angle_gamma 90.00 _cell_volume 3374(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 712 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 17.84 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _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 0.400 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9330 _exptl_absorpt_correction_T_max 0.9760 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 26696 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.1457 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11746 _reflns_number_gt 7471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0467P)^2] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881; 5540 Friedel pairs' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 11746 _refine_ls_number_parameters 732 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1285 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 0.40060(8) 0.87913(7) 0.73553(5) 0.0273(3) Uani 1 1 d D . . Cr2 Cr 0.29184(8) 1.01767(7) 0.75657(5) 0.0286(3) Uani 1 1 d D . . H1A H 0.170(3) 0.894(4) 0.720(3) 0.034 Uiso 1 1 d D . . H4A H 0.418(5) 0.993(4) 0.652(3) 0.034 Uiso 1 1 d . . . H1B H 0.229(3) 0.828(3) 0.718(3) 0.034 Uiso 1 1 d D . . H4B H 0.337(5) 1.054(5) 0.660(4) 0.034 Uiso 1 1 d . . . N1 N 0.4156(4) 0.7307(4) 0.7431(3) 0.0328(14) Uani 1 1 d . . . N2 N 0.5633(4) 0.8899(4) 0.7676(3) 0.0245(12) Uani 1 1 d . . . N3 N 0.2662(4) 1.0274(4) 0.8579(3) 0.0337(13) Uani 1 1 d . . . N4 N 0.2566(4) 1.1635(4) 0.7385(3) 0.0295(13) Uani 1 1 d . . . O O 0.9168(4) 0.4595(4) 0.7549(3) 0.0616(16) Uani 1 1 d . . . Si1 Si 0.9189(2) 0.4509(2) 0.84144(16) 0.0728(8) Uani 1 1 d . . . Si2 Si 0.84630(19) 0.48836(19) 0.67058(17) 0.0758(9) Uani 1 1 d . . . C1 C 0.2232(6) 0.8858(6) 0.7053(4) 0.0410(19) Uani 1 1 d D . . C2 C 0.1908(8) 0.9073(8) 0.6223(5) 0.090(4) Uani 1 1 d . . . H2A H 0.1699 0.8469 0.5945 0.108 Uiso 1 1 calc R . . H2B H 0.1274 0.9485 0.6088 0.108 Uiso 1 1 calc R . . C3 C 0.2652(7) 0.9502(8) 0.5983(5) 0.080(3) Uani 1 1 d . . . H3A H 0.2299 0.9986 0.5604 0.096 Uiso 1 1 calc R . . H3B H 0.2958 0.9020 0.5733 0.096 Uiso 1 1 calc R . . C4 C 0.3526(6) 0.9965(6) 0.6580(4) 0.039(2) Uani 1 1 d . . . C5 C 0.5061(6) 0.5781(5) 0.7873(4) 0.049(2) Uani 1 1 d . . . H5A H 0.4417 0.5566 0.7961 0.074 Uiso 1 1 calc R . . H5B H 0.5680 0.5586 0.8292 0.074 Uiso 1 1 calc R . . H5C H 0.5097 0.5498 0.7409 0.074 Uiso 1 1 calc R . . C6 C 0.5043(5) 0.6858(5) 0.7805(4) 0.0321(16) Uani 1 1 d . . . C7 C 0.6002(5) 0.7300(5) 0.8155(4) 0.0311(16) Uani 1 1 d . . . H7A H 0.6520 0.6930 0.8513 0.037 Uiso 1 1 calc R . . C8 C 0.6301(5) 0.8229(5) 0.8048(3) 0.0290(16) Uani 1 1 d . . . C9 C 0.7473(5) 0.8411(5) 0.8366(4) 0.0424(19) Uani 1 1 d . . . H9A H 0.7604 0.9096 0.8385 0.064 Uiso 1 1 calc R . . H9B H 0.7828 0.8108 0.8047 0.064 Uiso 1 1 calc R . . H9C H 0.7749 0.8147 0.8872 0.064 Uiso 1 1 calc R . . C10 C 0.3375(5) 0.6463(5) 0.6254(4) 0.0349(17) Uani 1 1 d . . . C11 C 0.2691(5) 0.5759(5) 0.5854(4) 0.0436(19) Uani 1 1 d . . . H11A H 0.2718 0.5570 0.5378 0.052 Uiso 1 1 calc R . . C12 C 0.1977(5) 0.5334(5) 0.6134(4) 0.0454(19) Uani 1 1 d . . . H12A H 0.1533 0.4839 0.5861 0.055 Uiso 1 1 calc R . . C13 C 0.1908(6) 0.5622(5) 0.6800(4) 0.048(2) Uani 1 1 d . . . H13A H 0.1400 0.5334 0.6982 0.058 Uiso 1 1 calc R . . C14 C 0.2558(5) 0.6322(5) 0.7221(4) 0.0380(18) Uani 1 1 d . . . C15 C 0.3342(5) 0.6707(5) 0.6961(4) 0.0341(17) Uani 1 1 d . . . C16 C 0.4108(5) 0.6948(5) 0.5914(4) 0.0417(19) Uani 1 1 d . . . H16A H 0.4328 0.7562 0.6186 0.050 Uiso 1 1 calc R . . C17 C 0.3567(6) 0.7186(6) 0.5087(4) 0.054(2) Uani 1 1 d . . . H17A H 0.2901 0.7519 0.5025 0.081 Uiso 1 1 calc R . . H17B H 0.3422 0.6599 0.4793 0.081 Uiso 1 1 calc R . . H17C H 0.4031 0.7594 0.4913 0.081 Uiso 1 1 calc R . . C18 C 0.5121(6) 0.6378(7) 0.6001(4) 0.067(3) Uani 1 1 d . . . H18A H 0.5555 0.6353 0.6530 0.100 Uiso 1 1 calc R . . H18B H 0.5520 0.6687 0.5714 0.100 Uiso 1 1 calc R . . H18C H 0.4932 0.5732 0.5812 0.100 Uiso 1 1 calc R . . C19 C 0.2391(6) 0.6652(5) 0.7946(4) 0.044(2) Uani 1 1 d . . . H19A H 0.2759 0.7275 0.8091 0.053 Uiso 1 1 calc R . . C20 C 0.1227(6) 0.6806(6) 0.7824(5) 0.065(3) Uani 1 1 d . . . H20A H 0.0923 0.7214 0.7386 0.097 Uiso 1 1 calc R . . H20B H 0.1144 0.7111 0.8267 0.097 Uiso 1 1 calc R . . H20C H 0.0861 0.6193 0.7740 0.097 Uiso 1 1 calc R . . C21 C 0.2832(8) 0.5975(6) 0.8595(5) 0.081(3) Uani 1 1 d . . . H21A H 0.3604 0.5957 0.8737 0.122 Uiso 1 1 calc R . . H21B H 0.2545 0.5339 0.8447 0.122 Uiso 1 1 calc R . . H21C H 0.2632 0.6192 0.9022 0.122 Uiso 1 1 calc R . . C22 C 0.6315(5) 1.0503(5) 0.8035(4) 0.0335(17) Uani 1 1 d . . . C23 C 0.6822(5) 1.1305(5) 0.7892(4) 0.0416(19) Uani 1 1 d . . . H23A H 0.6957 1.1821 0.8234 0.050 Uiso 1 1 calc R . . C24 C 0.7131(5) 1.1371(5) 0.7273(4) 0.045(2) Uani 1 1 d . . . H24A H 0.7482 1.1923 0.7187 0.054 Uiso 1 1 calc R . . C25 C 0.6923(5) 1.0623(5) 0.6778(4) 0.0372(18) Uani 1 1 d . . . H25A H 0.7153 1.0663 0.6355 0.045 Uiso 1 1 calc R . . C26 C 0.6396(5) 0.9819(5) 0.6871(4) 0.0320(16) Uani 1 1 d . . . C27 C 0.6111(5) 0.9764(4) 0.7518(4) 0.0277(15) Uani 1 1 d . . . C28 C 0.6168(6) 0.9038(5) 0.6303(4) 0.0407(19) Uani 1 1 d . . . H28A H 0.5748 0.8542 0.6457 0.049 Uiso 1 1 calc R . . C29 C 0.5524(6) 0.9370(6) 0.5529(4) 0.054(2) Uani 1 1 d . . . H29A H 0.4879 0.9680 0.5548 0.082 Uiso 1 1 calc R . . H29B H 0.5336 0.8824 0.5190 0.082 Uiso 1 1 calc R . . H29C H 0.5940 0.9822 0.5347 0.082 Uiso 1 1 calc R . . C30 C 0.7178(7) 0.8574(6) 0.6275(5) 0.075(3) Uani 1 1 d . . . H30A H 0.7645 0.8443 0.6786 0.113 Uiso 1 1 calc R . . H30B H 0.7536 0.9002 0.6028 0.113 Uiso 1 1 calc R . . H30C H 0.7005 0.7978 0.5994 0.113 Uiso 1 1 calc R . . C31 C 0.6037(6) 1.0457(5) 0.8745(4) 0.0398(19) Uani 1 1 d . . . H31A H 0.5634 0.9856 0.8732 0.048 Uiso 1 1 calc R . . C32 C 0.7014(7) 1.0427(7) 0.9437(4) 0.079(3) Uani 1 1 d . . . H32A H 0.7449 0.9879 0.9408 0.118 Uiso 1 1 calc R . . H32B H 0.6802 1.0371 0.9884 0.118 Uiso 1 1 calc R . . H32C H 0.7423 1.1011 0.9467 0.118 Uiso 1 1 calc R . . C33 C 0.5333(6) 1.1279(5) 0.8803(4) 0.051(2) Uani 1 1 d . . . H33A H 0.4690 1.1280 0.8365 0.076 Uiso 1 1 calc R . . H33B H 0.5712 1.1879 0.8825 0.076 Uiso 1 1 calc R . . H33C H 0.5143 1.1208 0.9258 0.076 Uiso 1 1 calc R . . C34 C 0.2740(6) 1.1091(5) 0.9765(4) 0.046(2) Uani 1 1 d . . . H34A H 0.3217 1.0594 1.0047 0.069 Uiso 1 1 calc R . . H34B H 0.2024 1.0970 0.9773 0.069 Uiso 1 1 calc R . . H34C H 0.2983 1.1710 0.9995 0.069 Uiso 1 1 calc R . . C35 C 0.2734(5) 1.1093(6) 0.8968(4) 0.0388(19) Uani 1 1 d . . . C36 C 0.2771(5) 1.1989(5) 0.8661(4) 0.0378(18) Uani 1 1 d . . . H36A H 0.2961 1.2497 0.9010 0.045 Uiso 1 1 calc R . . C37 C 0.2570(5) 1.2243(5) 0.7919(4) 0.0355(17) Uani 1 1 d . . . C38 C 0.2320(7) 1.3279(5) 0.7757(4) 0.057(2) Uani 1 1 d . . . H38A H 0.2435 1.3451 0.7288 0.085 Uiso 1 1 calc R . . H38B H 0.2781 1.3663 0.8167 0.085 Uiso 1 1 calc R . . H38C H 0.1580 1.3397 0.7710 0.085 Uiso 1 1 calc R . . C39 C 0.3133(5) 0.8848(6) 0.9399(3) 0.0332(15) Uani 1 1 d . . . C40 C 0.2787(6) 0.8106(6) 0.9740(4) 0.0422(18) Uani 1 1 d . . . H40A H 0.3294 0.7675 1.0042 0.051 Uiso 1 1 calc R . . C41 C 0.1753(6) 0.7971(6) 0.9658(4) 0.048(2) Uani 1 1 d . . . H41A H 0.1549 0.7469 0.9916 0.058 Uiso 1 1 calc R . . C42 C 0.1005(6) 0.8563(5) 0.9203(4) 0.049(2) Uani 1 1 d . . . H42A H 0.0282 0.8457 0.9142 0.059 Uiso 1 1 calc R . . C43 C 0.1281(5) 0.9324(5) 0.8824(4) 0.0403(19) Uani 1 1 d . . . C44 C 0.2366(5) 0.9454(5) 0.8935(3) 0.0304(16) Uani 1 1 d . . . C45 C 0.4291(5) 0.9001(5) 0.9563(4) 0.0403(18) Uani 1 1 d . . . H45A H 0.4377 0.9534 0.9239 0.048 Uiso 1 1 calc R . . C46 C 0.4846(5) 0.8148(6) 0.9393(4) 0.050(2) Uani 1 1 d . . . H46A H 0.4494 0.7951 0.8873 0.075 Uiso 1 1 calc R . . H46B H 0.4823 0.7628 0.9730 0.075 Uiso 1 1 calc R . . H46C H 0.5584 0.8310 0.9463 0.075 Uiso 1 1 calc R . . C47 C 0.4849(7) 0.9276(8) 1.0360(6) 0.108(4) Uani 1 1 d . . . H47A H 0.4410 0.9724 1.0524 0.162 Uiso 1 1 calc R . . H47B H 0.5525 0.9576 1.0401 0.162 Uiso 1 1 calc R . . H47C H 0.4975 0.8708 1.0676 0.162 Uiso 1 1 calc R . . C48 C 0.0427(5) 0.9957(7) 0.8346(4) 0.056(2) Uani 1 1 d . . . H48A H 0.0770 1.0458 0.8131 0.068 Uiso 1 1 calc R . . C49 C -0.0197(6) 1.0457(6) 0.8792(5) 0.072(3) Uani 1 1 d . . . H49A H 0.0286 1.0844 0.9189 0.108 Uiso 1 1 calc R . . H49B H -0.0534 0.9980 0.9016 0.108 Uiso 1 1 calc R . . H49C H -0.0740 1.0865 0.8456 0.108 Uiso 1 1 calc R . . C50 C -0.0330(6) 0.9418(6) 0.7704(5) 0.064(3) Uani 1 1 d . . . H50A H 0.0062 0.9113 0.7411 0.096 Uiso 1 1 calc R . . H50B H -0.0852 0.9858 0.7385 0.096 Uiso 1 1 calc R . . H50C H -0.0692 0.8932 0.7900 0.096 Uiso 1 1 calc R . . C51 C 0.1094(5) 1.1886(5) 0.6225(4) 0.0389(18) Uani 1 1 d . . . C52 C 0.0699(6) 1.2286(6) 0.5515(4) 0.053(2) Uani 1 1 d . . . H52A H -0.0032 1.2227 0.5238 0.063 Uiso 1 1 calc R . . C53 C 0.1341(7) 1.2760(5) 0.5214(4) 0.052(2) Uani 1 1 d . . . H53A H 0.1050 1.3048 0.4736 0.062 Uiso 1 1 calc R . . C54 C 0.2403(6) 1.2830(5) 0.5590(4) 0.0428(19) Uani 1 1 d . . . H54A H 0.2840 1.3149 0.5360 0.051 Uiso 1 1 calc R . . C55 C 0.2859(5) 1.2445(5) 0.6301(4) 0.0354(17) Uani 1 1 d . . . C56 C 0.2155(5) 1.1991(5) 0.6620(4) 0.0321(16) Uani 1 1 d . . . C57 C 0.0346(5) 1.1361(6) 0.6539(4) 0.052(2) Uani 1 1 d . . . H57A H 0.0778 1.0890 0.6910 0.062 Uiso 1 1 calc R . . C58 C -0.0510(6) 1.0810(8) 0.5955(5) 0.089(3) Uani 1 1 d . . . H58A H -0.0190 1.0431 0.5652 0.134 Uiso 1 1 calc R . . H58B H -0.1022 1.1254 0.5632 0.134 Uiso 1 1 calc R . . H58C H -0.0870 1.0388 0.6205 0.134 Uiso 1 1 calc R . . C59 C -0.0177(7) 1.2006(8) 0.6954(6) 0.089(3) Uani 1 1 d . . . H59A H -0.0697 1.1643 0.7105 0.133 Uiso 1 1 calc R . . H59B H -0.0532 1.2529 0.6626 0.133 Uiso 1 1 calc R . . H59C H 0.0360 1.2263 0.7400 0.133 Uiso 1 1 calc R . . C60 C 0.4025(6) 1.2477(5) 0.6678(4) 0.0396(18) Uani 1 1 d . . . H60A H 0.4218 1.1993 0.7088 0.048 Uiso 1 1 calc R . . C61 C 0.4420(7) 1.3453(6) 0.7027(6) 0.082(3) Uani 1 1 d . . . H61A H 0.4112 1.3593 0.7419 0.123 Uiso 1 1 calc R . . H61B H 0.4206 1.3943 0.6638 0.123 Uiso 1 1 calc R . . H61C H 0.5192 1.3443 0.7245 0.123 Uiso 1 1 calc R . . C62 C 0.4624(6) 1.2242(6) 0.6138(5) 0.066(3) Uani 1 1 d . . . H62A H 0.4306 1.1683 0.5841 0.099 Uiso 1 1 calc R . . H62B H 0.5365 1.2109 0.6424 0.099 Uiso 1 1 calc R . . H62C H 0.4583 1.2782 0.5804 0.099 Uiso 1 1 calc R . . C63 C 0.9354(16) 0.5665(11) 0.8835(9) 0.267(13) Uani 1 1 d . . . H63A H 0.8865 0.6111 0.8495 0.401 Uiso 1 1 calc R . . H63B H 1.0082 0.5879 0.8933 0.401 Uiso 1 1 calc R . . H63C H 0.9204 0.5634 0.9308 0.401 Uiso 1 1 calc R . . C64 C 1.0299(12) 0.3861(18) 0.8940(6) 0.308(16) Uani 1 1 d . . . H64A H 1.0209 0.3193 0.8788 0.461 Uiso 1 1 calc R . . H64B H 1.0382 0.3911 0.9473 0.461 Uiso 1 1 calc R . . H64C H 1.0930 0.4116 0.8855 0.461 Uiso 1 1 calc R . . C65 C 0.7948(9) 0.4138(12) 0.8475(7) 0.166(7) Uani 1 1 d . . . H65A H 0.7803 0.3484 0.8293 0.248 Uiso 1 1 calc R . . H65B H 0.7388 0.4557 0.8167 0.248 Uiso 1 1 calc R . . H65C H 0.7969 0.4171 0.8997 0.248 Uiso 1 1 calc R . . C66 C 0.8184(9) 0.6170(8) 0.6731(9) 0.184(8) Uani 1 1 d . . . H66A H 0.8847 0.6527 0.6856 0.276 Uiso 1 1 calc R . . H66B H 0.7848 0.6290 0.7110 0.276 Uiso 1 1 calc R . . H66D H 0.7709 0.6372 0.6240 0.276 Uiso 1 1 calc R . . C67 C 0.9216(7) 0.4598(10) 0.6075(6) 0.135(6) Uani 1 1 d . . . H67A H 0.9199 0.3911 0.5990 0.203 Uiso 1 1 calc R . . H67D H 0.9950 0.4806 0.6303 0.203 Uiso 1 1 calc R . . H67B H 0.8898 0.4925 0.5596 0.203 Uiso 1 1 calc R . . C68 C 0.7202(6) 0.4249(7) 0.6413(5) 0.075(3) Uani 1 1 d . . . H68D H 0.7333 0.3564 0.6445 0.113 Uiso 1 1 calc R . . H68A H 0.6797 0.4421 0.5896 0.113 Uiso 1 1 calc R . . H68B H 0.6799 0.4424 0.6742 0.113 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 0.0300(6) 0.0235(6) 0.0281(6) 0.0005(5) 0.0092(5) -0.0027(5) Cr2 0.0290(6) 0.0280(6) 0.0295(6) 0.0008(5) 0.0106(5) -0.0012(5) N1 0.045(4) 0.024(3) 0.033(3) 0.001(3) 0.017(3) -0.002(3) N2 0.030(3) 0.019(3) 0.029(3) -0.004(3) 0.016(2) -0.001(3) N3 0.035(3) 0.039(4) 0.027(3) 0.003(3) 0.010(2) -0.002(3) N4 0.038(3) 0.025(3) 0.027(3) 0.001(3) 0.012(3) -0.003(3) O 0.055(3) 0.065(4) 0.064(4) -0.009(3) 0.019(3) 0.011(3) Si1 0.0716(18) 0.079(2) 0.077(2) -0.0186(17) 0.0365(15) -0.0089(16) Si2 0.0478(15) 0.0588(18) 0.098(2) 0.0243(16) -0.0060(14) -0.0066(13) C1 0.044(4) 0.024(4) 0.056(5) 0.011(4) 0.018(4) 0.001(4) C2 0.090(7) 0.119(10) 0.041(6) 0.019(6) -0.006(5) -0.042(7) C3 0.078(7) 0.122(9) 0.031(5) -0.013(5) 0.008(5) -0.035(6) C4 0.043(4) 0.041(5) 0.044(4) -0.003(4) 0.027(4) 0.009(4) C5 0.048(5) 0.024(4) 0.062(6) 0.005(4) 0.000(4) 0.004(4) C6 0.040(4) 0.028(4) 0.029(4) 0.003(3) 0.012(3) 0.005(3) C7 0.031(4) 0.030(4) 0.030(4) -0.002(3) 0.007(3) 0.007(3) C8 0.030(4) 0.037(4) 0.023(4) 0.001(3) 0.013(3) 0.003(3) C9 0.038(4) 0.040(5) 0.049(5) 0.005(4) 0.014(4) 0.003(4) C10 0.033(4) 0.027(4) 0.039(4) -0.008(3) 0.004(3) 0.001(3) C11 0.046(5) 0.037(5) 0.043(5) -0.014(4) 0.008(4) 0.006(4) C12 0.047(4) 0.026(4) 0.059(5) -0.007(4) 0.010(4) -0.011(4) C13 0.054(5) 0.046(5) 0.044(5) 0.008(4) 0.015(4) -0.019(4) C14 0.041(4) 0.027(4) 0.039(4) 0.005(3) 0.002(4) -0.015(4) C15 0.036(4) 0.017(4) 0.040(4) 0.002(3) 0.000(3) -0.003(3) C16 0.043(4) 0.038(4) 0.050(5) -0.019(4) 0.022(4) -0.006(4) C17 0.061(5) 0.053(5) 0.054(5) -0.007(4) 0.027(4) -0.012(4) C18 0.044(5) 0.092(7) 0.060(6) -0.023(5) 0.012(4) -0.006(5) C19 0.058(5) 0.045(5) 0.032(4) 0.000(4) 0.018(4) -0.022(4) C20 0.071(6) 0.065(6) 0.070(6) -0.009(5) 0.041(5) -0.024(5) C21 0.140(9) 0.057(6) 0.051(6) 0.016(5) 0.039(6) -0.005(6) C22 0.026(4) 0.024(4) 0.048(5) -0.008(3) 0.009(3) -0.010(3) C23 0.040(4) 0.026(4) 0.059(5) -0.013(4) 0.015(4) -0.005(4) C24 0.040(4) 0.031(4) 0.062(6) 0.003(4) 0.017(4) -0.008(4) C25 0.033(4) 0.034(4) 0.050(5) 0.010(4) 0.021(4) 0.003(3) C26 0.033(4) 0.036(4) 0.028(4) 0.005(3) 0.012(3) 0.008(3) C27 0.021(3) 0.027(4) 0.031(4) 0.002(3) 0.003(3) -0.004(3) C28 0.058(5) 0.038(5) 0.032(4) 0.002(3) 0.023(4) -0.005(4) C29 0.054(5) 0.069(6) 0.042(5) -0.008(4) 0.018(4) 0.007(4) C30 0.093(7) 0.066(7) 0.052(6) -0.017(5) 0.004(5) 0.035(6) C31 0.060(5) 0.027(4) 0.035(4) -0.015(3) 0.020(4) -0.005(4) C32 0.099(7) 0.101(8) 0.034(5) -0.004(5) 0.019(5) 0.029(6) C33 0.058(5) 0.054(5) 0.046(5) -0.020(4) 0.023(4) -0.016(4) C34 0.054(5) 0.050(5) 0.038(5) -0.002(4) 0.020(4) -0.001(4) C35 0.032(4) 0.056(5) 0.032(4) 0.000(4) 0.015(3) 0.007(4) C36 0.048(5) 0.031(4) 0.037(4) -0.003(4) 0.017(4) 0.000(4) C37 0.038(4) 0.038(4) 0.036(4) 0.003(4) 0.018(3) -0.003(3) C38 0.091(6) 0.035(5) 0.050(5) 0.001(4) 0.030(5) 0.017(5) C39 0.037(4) 0.037(4) 0.030(4) -0.001(4) 0.017(3) 0.001(4) C40 0.044(4) 0.055(5) 0.023(4) 0.002(4) 0.007(3) 0.002(4) C41 0.045(5) 0.063(6) 0.041(5) 0.018(4) 0.019(4) -0.005(4) C42 0.033(4) 0.062(6) 0.055(5) 0.015(4) 0.019(4) -0.010(4) C43 0.030(4) 0.058(5) 0.037(4) 0.010(4) 0.016(3) 0.000(4) C44 0.032(4) 0.040(4) 0.024(4) 0.008(3) 0.015(3) -0.002(3) C45 0.038(4) 0.040(5) 0.039(4) -0.004(4) 0.009(3) 0.004(4) C46 0.042(4) 0.069(6) 0.040(5) -0.002(4) 0.016(4) 0.002(4) C47 0.042(5) 0.145(11) 0.122(9) -0.082(8) 0.007(6) 0.004(6) C48 0.029(4) 0.078(7) 0.058(5) 0.025(5) 0.010(4) 0.003(4) C49 0.049(5) 0.080(8) 0.085(7) 0.019(6) 0.020(5) 0.016(5) C50 0.035(4) 0.092(7) 0.069(6) 0.025(5) 0.022(4) 0.015(5) C51 0.034(4) 0.043(5) 0.040(4) 0.006(4) 0.011(3) 0.007(4) C52 0.037(4) 0.069(6) 0.049(5) 0.008(5) 0.011(4) 0.009(4) C53 0.074(6) 0.051(5) 0.033(4) 0.014(4) 0.020(4) 0.010(5) C54 0.054(5) 0.035(5) 0.044(5) 0.005(4) 0.022(4) 0.004(4) C55 0.041(4) 0.025(4) 0.042(4) 0.002(3) 0.014(4) 0.003(3) C56 0.036(4) 0.023(4) 0.037(4) -0.004(3) 0.012(3) 0.007(3) C57 0.029(4) 0.082(6) 0.045(5) 0.024(5) 0.011(4) 0.010(4) C58 0.055(6) 0.138(10) 0.055(6) 0.024(6) -0.008(5) -0.029(6) C59 0.071(6) 0.103(8) 0.119(9) 0.027(7) 0.068(6) 0.030(6) C60 0.054(5) 0.024(4) 0.047(5) 0.006(4) 0.026(4) -0.002(4) C61 0.070(6) 0.053(6) 0.121(9) -0.025(6) 0.030(6) -0.016(5) C62 0.059(6) 0.074(7) 0.077(6) 0.021(5) 0.038(5) 0.009(5) C63 0.50(3) 0.194(18) 0.232(19) -0.130(15) 0.29(2) -0.20(2) C64 0.233(17) 0.65(4) 0.050(8) 0.067(16) 0.061(9) 0.28(2) C65 0.111(10) 0.26(2) 0.128(11) 0.090(12) 0.037(8) -0.028(11) C66 0.112(10) 0.052(8) 0.30(2) 0.035(10) -0.046(11) -0.017(8) C67 0.060(6) 0.255(17) 0.076(8) 0.051(9) 0.003(6) -0.061(8) C68 0.067(6) 0.073(7) 0.075(7) 0.000(5) 0.007(5) -0.006(5) _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 N2 2.067(5) . ? Cr1 N1 2.101(6) . ? Cr1 C4 2.162(8) . ? Cr1 C1 2.256(7) . ? Cr1 Cr2 2.5450(15) . ? Cr2 N3 2.062(5) . ? Cr2 N4 2.110(6) . ? Cr2 C1 2.156(8) . ? Cr2 C4 2.287(7) . ? N1 C6 1.327(8) . ? N1 C15 1.434(8) . ? N2 C8 1.331(7) . ? N2 C27 1.454(8) . ? N3 C35 1.355(8) . ? N3 C44 1.457(8) . ? N4 C37 1.324(8) . ? N4 C56 1.457(8) . ? O Si2 1.615(6) . ? O Si1 1.633(6) . ? Si1 C65 1.782(11) . ? Si1 C64 1.750(13) . ? Si1 C63 1.794(14) . ? Si2 C67 1.844(11) . ? Si2 C68 1.829(8) . ? Si2 C66 1.854(12) . ? C1 C2 1.516(11) . ? C2 C3 1.366(11) . ? C3 C4 1.484(11) . ? C5 C6 1.523(9) . ? C6 C7 1.384(9) . ? C7 C8 1.402(9) . ? C8 C9 1.507(8) . ? C10 C11 1.392(9) . ? C10 C15 1.397(9) . ? C10 C16 1.504(9) . ? C11 C12 1.375(9) . ? C12 C13 1.356(10) . ? C13 C14 1.382(9) . ? C14 C15 1.408(9) . ? C14 C19 1.533(9) . ? C16 C18 1.538(10) . ? C16 C17 1.530(10) . ? C19 C21 1.512(10) . ? C19 C20 1.515(10) . ? C22 C27 1.392(8) . ? C22 C23 1.389(9) . ? C22 C31 1.510(9) . ? C23 C24 1.370(9) . ? C24 C25 1.376(9) . ? C25 C26 1.377(9) . ? C26 C27 1.401(8) . ? C26 C28 1.498(9) . ? C28 C29 1.507(9) . ? C28 C30 1.519(10) . ? C31 C32 1.516(9) . ? C31 C33 1.521(9) . ? C34 C35 1.507(9) . ? C35 C36 1.397(10) . ? C36 C37 1.385(9) . ? C37 C38 1.507(10) . ? C39 C40 1.385(10) . ? C39 C44 1.400(9) . ? C39 C45 1.495(8) . ? C40 C41 1.356(9) . ? C41 C42 1.368(9) . ? C42 C43 1.405(9) . ? C43 C44 1.411(9) . ? C43 C48 1.496(10) . ? C45 C46 1.504(9) . ? C45 C47 1.496(10) . ? C48 C50 1.506(11) . ? C48 C49 1.542(11) . ? C51 C56 1.379(9) . ? C51 C52 1.390(9) . ? C51 C57 1.517(9) . ? C52 C53 1.354(10) . ? C53 C54 1.370(10) . ? C54 C55 1.391(9) . ? C55 C56 1.428(9) . ? C55 C60 1.490(9) . ? C57 C58 1.518(11) . ? C57 C59 1.516(11) . ? C60 C62 1.529(10) . ? C60 C61 1.542(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 N2 Cr1 N1 89.1(2) . . ? N2 Cr1 C4 101.1(3) . . ? N1 Cr1 C4 143.9(3) . . ? N2 Cr1 C1 173.0(3) . . ? N1 Cr1 C1 97.4(3) . . ? C4 Cr1 C1 75.1(3) . . ? N2 Cr1 Cr2 120.08(15) . . ? N1 Cr1 Cr2 143.08(16) . . ? C4 Cr1 Cr2 57.45(19) . . ? C1 Cr1 Cr2 52.9(2) . . ? N3 Cr2 N4 89.4(2) . . ? N3 Cr2 C1 107.4(3) . . ? N4 Cr2 C1 136.6(3) . . ? N3 Cr2 C4 168.7(3) . . ? N4 Cr2 C4 96.6(3) . . ? C1 Cr2 C4 74.6(3) . . ? N3 Cr2 Cr1 118.44(16) . . ? N4 Cr2 Cr1 146.12(16) . . ? C1 Cr2 Cr1 56.64(19) . . ? C4 Cr2 Cr1 52.8(2) . . ? C6 N1 C15 114.5(5) . . ? C6 N1 Cr1 124.0(5) . . ? C15 N1 Cr1 120.6(4) . . ? C8 N2 C27 116.0(5) . . ? C8 N2 Cr1 124.3(4) . . ? C27 N2 Cr1 119.6(4) . . ? C35 N3 C44 114.0(5) . . ? C35 N3 Cr2 123.9(5) . . ? C44 N3 Cr2 122.2(4) . . ? C37 N4 C56 116.1(6) . . ? C37 N4 Cr2 124.2(5) . . ? C56 N4 Cr2 119.2(4) . . ? Si2 O Si1 145.1(4) . . ? O Si1 C65 112.2(5) . . ? O Si1 C64 109.8(4) . . ? C65 Si1 C64 116.6(9) . . ? O Si1 C63 109.6(5) . . ? C65 Si1 C63 102.6(8) . . ? C64 Si1 C63 105.3(10) . . ? O Si2 C67 108.6(4) . . ? O Si2 C68 110.9(4) . . ? C67 Si2 C68 110.2(5) . . ? O Si2 C66 106.1(5) . . ? C67 Si2 C66 112.8(7) . . ? C68 Si2 C66 108.1(5) . . ? C2 C1 Cr2 103.2(6) . . ? C2 C1 Cr1 100.9(5) . . ? Cr2 C1 Cr1 70.4(2) . . ? C3 C2 C1 116.2(7) . . ? C2 C3 C4 114.9(8) . . ? C3 C4 Cr1 99.4(6) . . ? C3 C4 Cr2 106.0(5) . . ? Cr1 C4 Cr2 69.7(2) . . ? N1 C6 C7 124.6(6) . . ? N1 C6 C5 120.4(6) . . ? C7 C6 C5 115.0(6) . . ? C6 C7 C8 127.9(6) . . ? N2 C8 C7 124.3(6) . . ? N2 C8 C9 121.4(6) . . ? C7 C8 C9 114.3(6) . . ? C11 C10 C15 118.2(7) . . ? C11 C10 C16 119.8(6) . . ? C15 C10 C16 121.9(6) . . ? C12 C11 C10 121.2(7) . . ? C13 C12 C11 119.8(7) . . ? C12 C13 C14 121.8(7) . . ? C13 C14 C15 118.3(7) . . ? C13 C14 C19 118.9(6) . . ? C15 C14 C19 122.8(6) . . ? C10 C15 C14 120.3(6) . . ? C10 C15 N1 118.7(6) . . ? C14 C15 N1 120.9(6) . . ? C10 C16 C18 113.3(7) . . ? C10 C16 C17 112.4(6) . . ? C18 C16 C17 109.1(6) . . ? C14 C19 C21 113.7(7) . . ? C14 C19 C20 110.7(6) . . ? C21 C19 C20 108.8(7) . . ? C27 C22 C23 117.8(6) . . ? C27 C22 C31 123.0(6) . . ? C23 C22 C31 119.2(6) . . ? C22 C23 C24 121.8(7) . . ? C23 C24 C25 118.6(7) . . ? C26 C25 C24 122.8(7) . . ? C25 C26 C27 117.1(6) . . ? C25 C26 C28 120.3(6) . . ? C27 C26 C28 122.5(6) . . ? C22 C27 C26 121.8(6) . . ? C22 C27 N2 118.7(5) . . ? C26 C27 N2 119.5(6) . . ? C26 C28 C29 112.6(6) . . ? C26 C28 C30 111.6(6) . . ? C29 C28 C30 109.4(6) . . ? C22 C31 C32 112.0(6) . . ? C22 C31 C33 111.9(6) . . ? C32 C31 C33 109.8(6) . . ? N3 C35 C36 123.4(6) . . ? N3 C35 C34 121.2(7) . . ? C36 C35 C34 115.4(7) . . ? C37 C36 C35 129.2(7) . . ? N4 C37 C36 123.9(7) . . ? N4 C37 C38 121.8(6) . . ? C36 C37 C38 114.3(6) . . ? C40 C39 C44 117.5(6) . . ? C40 C39 C45 119.8(6) . . ? C44 C39 C45 122.6(6) . . ? C41 C40 C39 122.7(7) . . ? C40 C41 C42 119.7(7) . . ? C41 C42 C43 121.7(7) . . ? C42 C43 C44 117.0(6) . . ? C42 C43 C48 119.1(6) . . ? C44 C43 C48 123.9(6) . . ? C39 C44 C43 121.4(6) . . ? C39 C44 N3 121.2(6) . . ? C43 C44 N3 117.3(6) . . ? C39 C45 C46 113.2(6) . . ? C39 C45 C47 112.7(6) . . ? C46 C45 C47 107.8(6) . . ? C43 C48 C50 111.4(7) . . ? C43 C48 C49 112.7(6) . . ? C50 C48 C49 109.2(6) . . ? C56 C51 C52 118.4(7) . . ? C56 C51 C57 122.4(7) . . ? C52 C51 C57 119.1(6) . . ? C53 C52 C51 121.0(7) . . ? C52 C53 C54 120.8(7) . . ? C53 C54 C55 121.6(7) . . ? C54 C55 C56 116.3(6) . . ? C54 C55 C60 120.5(6) . . ? C56 C55 C60 123.2(6) . . ? C51 C56 C55 121.7(7) . . ? C51 C56 N4 119.1(6) . . ? C55 C56 N4 119.2(6) . . ? C58 C57 C51 113.7(7) . . ? C58 C57 C59 108.5(7) . . ? C51 C57 C59 112.9(7) . . ? C55 C60 C62 111.9(6) . . ? C55 C60 C61 112.9(6) . . ? C62 C60 C61 107.3(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cr1 Cr2 N3 -87.5(2) . . . . ? N1 Cr1 Cr2 N3 50.4(3) . . . . ? C4 Cr1 Cr2 N3 -171.4(3) . . . . ? C1 Cr1 Cr2 N3 92.8(3) . . . . ? N2 Cr1 Cr2 N4 54.3(3) . . . . ? N1 Cr1 Cr2 N4 -167.9(4) . . . . ? C4 Cr1 Cr2 N4 -29.7(4) . . . . ? C1 Cr1 Cr2 N4 -125.4(4) . . . . ? N2 Cr1 Cr2 C1 179.7(3) . . . . ? N1 Cr1 Cr2 C1 -42.5(4) . . . . ? C4 Cr1 Cr2 C1 95.7(4) . . . . ? N2 Cr1 Cr2 C4 83.9(3) . . . . ? N1 Cr1 Cr2 C4 -138.2(4) . . . . ? C1 Cr1 Cr2 C4 -95.7(4) . . . . ? N2 Cr1 N1 C6 18.3(5) . . . . ? C4 Cr1 N1 C6 126.1(6) . . . . ? C1 Cr1 N1 C6 -159.1(5) . . . . ? Cr2 Cr1 N1 C6 -126.2(5) . . . . ? N2 Cr1 N1 C15 -150.1(5) . . . . ? C4 Cr1 N1 C15 -42.3(7) . . . . ? C1 Cr1 N1 C15 32.5(5) . . . . ? Cr2 Cr1 N1 C15 65.4(6) . . . . ? N1 Cr1 N2 C8 -22.0(5) . . . . ? C4 Cr1 N2 C8 -167.1(5) . . . . ? Cr2 Cr1 N2 C8 134.3(4) . . . . ? N1 Cr1 N2 C27 160.2(4) . . . . ? C4 Cr1 N2 C27 15.1(5) . . . . ? Cr2 Cr1 N2 C27 -43.5(4) . . . . ? N4 Cr2 N3 C35 -23.1(5) . . . . ? C1 Cr2 N3 C35 -162.4(5) . . . . ? C4 Cr2 N3 C35 99.3(15) . . . . ? Cr1 Cr2 N3 C35 136.7(5) . . . . ? N4 Cr2 N3 C44 155.8(5) . . . . ? C1 Cr2 N3 C44 16.5(5) . . . . ? C4 Cr2 N3 C44 -81.8(15) . . . . ? Cr1 Cr2 N3 C44 -44.4(5) . . . . ? N3 Cr2 N4 C37 17.8(5) . . . . ? C1 Cr2 N4 C37 132.9(5) . . . . ? C4 Cr2 N4 C37 -152.6(5) . . . . ? Cr1 Cr2 N4 C37 -129.2(5) . . . . ? N3 Cr2 N4 C56 -153.5(5) . . . . ? C1 Cr2 N4 C56 -38.5(6) . . . . ? C4 Cr2 N4 C56 36.1(5) . . . . ? Cr1 Cr2 N4 C56 59.5(6) . . . . ? Si2 O Si1 C65 36.1(9) . . . . ? Si2 O Si1 C64 167.6(11) . . . . ? Si2 O Si1 C63 -77.2(10) . . . . ? Si1 O Si2 C67 -174.8(7) . . . . ? Si1 O Si2 C68 -53.5(8) . . . . ? Si1 O Si2 C66 63.7(8) . . . . ? N3 Cr2 C1 C2 149.9(6) . . . . ? N4 Cr2 C1 C2 41.6(7) . . . . ? C4 Cr2 C1 C2 -41.7(6) . . . . ? Cr1 Cr2 C1 C2 -97.0(6) . . . . ? N3 Cr2 C1 Cr1 -113.1(2) . . . . ? N4 Cr2 C1 Cr1 138.6(3) . . . . ? C4 Cr2 C1 Cr1 55.3(2) . . . . ? N1 Cr1 C1 C2 -103.8(6) . . . . ? C4 Cr1 C1 C2 40.1(6) . . . . ? Cr2 Cr1 C1 C2 100.3(6) . . . . ? N1 Cr1 C1 Cr2 155.9(2) . . . . ? C4 Cr1 C1 Cr2 -60.2(3) . . . . ? Cr2 C1 C2 C3 48.2(11) . . . . ? Cr1 C1 C2 C3 -24.0(11) . . . . ? C1 C2 C3 C4 -18.4(15) . . . . ? C2 C3 C4 Cr1 52.4(10) . . . . ? C2 C3 C4 Cr2 -19.1(11) . . . . ? N2 Cr1 C4 C3 137.6(5) . . . . ? N1 Cr1 C4 C3 33.6(7) . . . . ? C1 Cr1 C4 C3 -48.4(5) . . . . ? Cr2 Cr1 C4 C3 -103.6(5) . . . . ? N2 Cr1 C4 Cr2 -118.74(19) . . . . ? N1 Cr1 C4 Cr2 137.2(3) . . . . ? C1 Cr1 C4 Cr2 55.2(2) . . . . ? N3 Cr2 C4 C3 136.4(13) . . . . ? N4 Cr2 C4 C3 -101.8(6) . . . . ? C1 Cr2 C4 C3 34.8(6) . . . . ? Cr1 Cr2 C4 C3 94.4(6) . . . . ? N3 Cr2 C4 Cr1 42.1(15) . . . . ? N4 Cr2 C4 Cr1 163.9(2) . . . . ? C1 Cr2 C4 Cr1 -59.5(2) . . . . ? C15 N1 C6 C7 165.0(6) . . . . ? Cr1 N1 C6 C7 -4.1(9) . . . . ? C15 N1 C6 C5 -15.0(9) . . . . ? Cr1 N1 C6 C5 175.9(5) . . . . ? N1 C6 C7 C8 -16.7(11) . . . . ? C5 C6 C7 C8 163.4(6) . . . . ? C27 N2 C8 C7 -170.2(6) . . . . ? Cr1 N2 C8 C7 11.9(8) . . . . ? C27 N2 C8 C9 7.3(8) . . . . ? Cr1 N2 C8 C9 -170.6(4) . . . . ? C6 C7 C8 N2 12.5(11) . . . . ? C6 C7 C8 C9 -165.2(6) . . . . ? C15 C10 C11 C12 2.0(10) . . . . ? C16 C10 C11 C12 -176.9(7) . . . . ? C10 C11 C12 C13 2.2(11) . . . . ? C11 C12 C13 C14 -1.6(12) . . . . ? C12 C13 C14 C15 -3.1(11) . . . . ? C12 C13 C14 C19 176.4(7) . . . . ? C11 C10 C15 C14 -6.8(10) . . . . ? C16 C10 C15 C14 172.1(6) . . . . ? C11 C10 C15 N1 169.5(6) . . . . ? C16 C10 C15 N1 -11.7(10) . . . . ? C13 C14 C15 C10 7.4(10) . . . . ? C19 C14 C15 C10 -172.2(6) . . . . ? C13 C14 C15 N1 -168.8(6) . . . . ? C19 C14 C15 N1 11.7(10) . . . . ? C6 N1 C15 C10 -81.9(8) . . . . ? Cr1 N1 C15 C10 87.6(7) . . . . ? C6 N1 C15 C14 94.3(7) . . . . ? Cr1 N1 C15 C14 -96.2(7) . . . . ? C11 C10 C16 C18 -82.0(8) . . . . ? C15 C10 C16 C18 99.1(8) . . . . ? C11 C10 C16 C17 42.2(9) . . . . ? C15 C10 C16 C17 -136.7(7) . . . . ? C13 C14 C19 C21 77.5(9) . . . . ? C15 C14 C19 C21 -102.9(8) . . . . ? C13 C14 C19 C20 -45.2(9) . . . . ? C15 C14 C19 C20 134.3(7) . . . . ? C27 C22 C23 C24 -1.0(10) . . . . ? C31 C22 C23 C24 177.3(6) . . . . ? C22 C23 C24 C25 0.6(11) . . . . ? C23 C24 C25 C26 1.5(10) . . . . ? C24 C25 C26 C27 -2.9(10) . . . . ? C24 C25 C26 C28 178.4(6) . . . . ? C23 C22 C27 C26 -0.5(9) . . . . ? C31 C22 C27 C26 -178.7(6) . . . . ? C23 C22 C27 N2 176.7(5) . . . . ? C31 C22 C27 N2 -1.6(9) . . . . ? C25 C26 C27 C22 2.3(9) . . . . ? C28 C26 C27 C22 -179.0(6) . . . . ? C25 C26 C27 N2 -174.8(5) . . . . ? C28 C26 C27 N2 3.8(9) . . . . ? C8 N2 C27 C22 -90.5(7) . . . . ? Cr1 N2 C27 C22 87.5(6) . . . . ? C8 N2 C27 C26 86.8(7) . . . . ? Cr1 N2 C27 C26 -95.2(6) . . . . ? C25 C26 C28 C29 -58.2(8) . . . . ? C27 C26 C28 C29 123.2(7) . . . . ? C25 C26 C28 C30 65.2(8) . . . . ? C27 C26 C28 C30 -113.4(7) . . . . ? C27 C22 C31 C32 112.3(7) . . . . ? C23 C22 C31 C32 -66.0(9) . . . . ? C27 C22 C31 C33 -123.9(7) . . . . ? C23 C22 C31 C33 57.8(8) . . . . ? C44 N3 C35 C36 -165.2(6) . . . . ? Cr2 N3 C35 C36 13.8(9) . . . . ? C44 N3 C35 C34 12.6(9) . . . . ? Cr2 N3 C35 C34 -168.4(4) . . . . ? N3 C35 C36 C37 12.0(12) . . . . ? C34 C35 C36 C37 -165.9(7) . . . . ? C56 N4 C37 C36 169.3(6) . . . . ? Cr2 N4 C37 C36 -2.4(9) . . . . ? C56 N4 C37 C38 -8.9(9) . . . . ? Cr2 N4 C37 C38 179.5(5) . . . . ? C35 C36 C37 N4 -18.2(12) . . . . ? C35 C36 C37 C38 160.0(7) . . . . ? C44 C39 C40 C41 -2.2(11) . . . . ? C45 C39 C40 C41 175.0(7) . . . . ? C39 C40 C41 C42 2.4(12) . . . . ? C40 C41 C42 C43 -1.2(12) . . . . ? C41 C42 C43 C44 -0.2(11) . . . . ? C41 C42 C43 C48 -178.8(8) . . . . ? C40 C39 C44 C43 0.7(10) . . . . ? C45 C39 C44 C43 -176.3(6) . . . . ? C40 C39 C44 N3 177.5(6) . . . . ? C45 C39 C44 N3 0.4(10) . . . . ? C42 C43 C44 C39 0.4(10) . . . . ? C48 C43 C44 C39 178.9(7) . . . . ? C42 C43 C44 N3 -176.5(6) . . . . ? C48 C43 C44 N3 2.1(10) . . . . ? C35 N3 C44 C39 -94.7(8) . . . . ? Cr2 N3 C44 C39 86.4(7) . . . . ? C35 N3 C44 C43 82.2(7) . . . . ? Cr2 N3 C44 C43 -96.7(6) . . . . ? C40 C39 C45 C46 57.1(9) . . . . ? C44 C39 C45 C46 -125.9(7) . . . . ? C40 C39 C45 C47 -65.4(9) . . . . ? C44 C39 C45 C47 111.5(8) . . . . ? C42 C43 C48 C50 -62.9(9) . . . . ? C44 C43 C48 C50 118.6(8) . . . . ? C42 C43 C48 C49 60.2(10) . . . . ? C44 C43 C48 C49 -118.3(8) . . . . ? C56 C51 C52 C53 0.7(11) . . . . ? C57 C51 C52 C53 -179.9(7) . . . . ? C51 C52 C53 C54 2.3(12) . . . . ? C52 C53 C54 C55 -2.0(12) . . . . ? C53 C54 C55 C56 -1.2(10) . . . . ? C53 C54 C55 C60 176.1(7) . . . . ? C52 C51 C56 C55 -4.0(10) . . . . ? C57 C51 C56 C55 176.7(7) . . . . ? C52 C51 C56 N4 175.7(6) . . . . ? C57 C51 C56 N4 -3.6(10) . . . . ? C54 C55 C56 C51 4.2(10) . . . . ? C60 C55 C56 C51 -173.0(7) . . . . ? C54 C55 C56 N4 -175.5(6) . . . . ? C60 C55 C56 N4 7.3(9) . . . . ? C37 N4 C56 C51 -91.0(8) . . . . ? Cr2 N4 C56 C51 81.1(7) . . . . ? C37 N4 C56 C55 88.7(7) . . . . ? Cr2 N4 C56 C55 -99.2(6) . . . . ? C56 C51 C57 C58 -144.7(8) . . . . ? C52 C51 C57 C58 36.0(10) . . . . ? C56 C51 C57 C59 91.2(9) . . . . ? C52 C51 C57 C59 -88.2(9) . . . . ? C54 C55 C60 C62 -42.3(9) . . . . ? C56 C55 C60 C62 134.8(7) . . . . ? C54 C55 C60 C61 78.9(9) . . . . ? C56 C55 C60 C61 -104.0(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.496 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.065 _vrf_PLAT223_klat305 ; PROBLEM: Large Solvent/Anion H Ueq(max)/Ueq(min) RESPONSE: There are large apparent thermal motion on the methyl moieties of the cocrystallized solvent. ; _vrf_PLAT413_klat305 ; PROBLEM: Short Inter XH3 .. XHn RESPONSE: The H-positions on the bridging alkyl chain are imprecise because of significant yet unresolvable disorder. ; data_klat247 _database_code_depnum_ccdc_archive 'CCDC 918027' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H104 Cr2 N4' _chemical_formula_weight 1081.55 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.187(4) _cell_length_b 13.567(4) _cell_length_c 18.405(6) _cell_angle_alpha 88.750(5) _cell_angle_beta 74.798(4) _cell_angle_gamma 88.291(4) _cell_volume 3175.8(17) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1011 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.31 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method ? _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9066 _exptl_absorpt_correction_T_max 0.9469 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 33019 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.12 _reflns_number_total 13753 _reflns_number_gt 10455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.1037P)^2^+1.2177P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13753 _refine_ls_number_parameters 679 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C7 C 0.4134(2) 0.26966(18) 0.41925(14) 0.0322(5) Uani 1 1 d . . . C8 C 0.4933(2) 0.20375(19) 0.38326(15) 0.0345(5) Uani 1 1 d . . . H2A H 0.5617 0.2173 0.3875 0.041 Uiso 1 1 calc R . . C9 C 0.4856(2) 0.12035(19) 0.34179(15) 0.0343(5) Uani 1 1 d . . . C6 C 0.4388(2) 0.3292(2) 0.48096(17) 0.0448(7) Uani 1 1 d . . . H4A H 0.3788 0.3728 0.5036 0.067 Uiso 1 1 calc R . . H4B H 0.5007 0.3688 0.4594 0.067 Uiso 1 1 calc R . . H4C H 0.4533 0.2843 0.5197 0.067 Uiso 1 1 calc R . . C10 C 0.5818(2) 0.0507(2) 0.3263(2) 0.0519(8) Uani 1 1 d . . . H5A H 0.5697 -0.0056 0.2975 0.078 Uiso 1 1 calc R . . H5B H 0.5937 0.0272 0.3742 0.078 Uiso 1 1 calc R . . H5C H 0.6435 0.0860 0.2973 0.078 Uiso 1 1 calc R . . C16 C 0.23984(19) 0.33545(18) 0.45588(14) 0.0321(5) Uani 1 1 d . . . C11 C 0.2261(2) 0.43768(19) 0.44505(16) 0.0389(6) Uani 1 1 d . . . C12 C 0.1466(3) 0.4872(2) 0.49844(19) 0.0526(8) Uani 1 1 d . . . H8A H 0.1359 0.5561 0.4922 0.063 Uiso 1 1 calc R . . C13 C 0.0836(3) 0.4390(3) 0.55971(19) 0.0584(8) Uani 1 1 d . . . H9A H 0.0306 0.4746 0.5952 0.070 Uiso 1 1 calc R . . C14 C 0.0978(3) 0.3397(2) 0.56925(17) 0.0512(7) Uani 1 1 d . . . H10A H 0.0538 0.3068 0.6115 0.061 Uiso 1 1 calc R . . C15 C 0.1752(2) 0.2858(2) 0.51837(15) 0.0388(6) Uani 1 1 d . . . C17 C 0.2937(3) 0.4959(2) 0.37939(19) 0.0509(8) Uani 1 1 d . . . H12A H 0.3349 0.4480 0.3417 0.061 Uiso 1 1 calc R . . C18 C 0.2276(3) 0.5632(2) 0.3402(2) 0.0569(8) Uani 1 1 d . . . H13A H 0.1774 0.5234 0.3234 0.085 Uiso 1 1 calc R . . H13B H 0.2739 0.5962 0.2967 0.085 Uiso 1 1 calc R . . H13C H 0.1892 0.6128 0.3757 0.085 Uiso 1 1 calc R . . C19 C 0.3717(3) 0.5598(3) 0.4052(3) 0.0803(13) Uani 1 1 d . . . H14A H 0.4150 0.5178 0.4298 0.120 Uiso 1 1 calc R . . H14B H 0.3328 0.6089 0.4409 0.120 Uiso 1 1 calc R . . H14C H 0.4170 0.5934 0.3615 0.120 Uiso 1 1 calc R . . C20 C 0.1881(3) 0.1759(2) 0.53214(19) 0.0573(9) Uani 1 1 d . . . H15A H 0.2294 0.1465 0.4836 0.069 Uiso 1 1 calc R . . C21 C 0.0835(4) 0.1239(3) 0.5559(3) 0.0922(15) Uani 1 1 d . . . H16A H 0.0963 0.0533 0.5634 0.138 Uiso 1 1 calc R . . H16B H 0.0463 0.1329 0.5165 0.138 Uiso 1 1 calc R . . H16C H 0.0407 0.1519 0.6030 0.138 Uiso 1 1 calc R . . C22 C 0.2493(5) 0.1552(4) 0.5901(4) 0.114(2) Uani 1 1 d . . . H17A H 0.2567 0.0838 0.5971 0.171 Uiso 1 1 calc R . . H17B H 0.2117 0.1848 0.6381 0.171 Uiso 1 1 calc R . . H17C H 0.3192 0.1837 0.5727 0.171 Uiso 1 1 calc R . . C28 C 0.4054(2) -0.00197(18) 0.28993(15) 0.0333(5) Uani 1 1 d . . . C23 C 0.3689(2) -0.07959(19) 0.34112(17) 0.0408(6) Uani 1 1 d . . . C24 C 0.3897(3) -0.1762(2) 0.3156(2) 0.0522(8) Uani 1 1 d . . . H20A H 0.3672 -0.2297 0.3497 0.063 Uiso 1 1 calc R . . C25 C 0.4425(3) -0.1952(2) 0.2417(2) 0.0584(9) Uani 1 1 d . . . H21A H 0.4591 -0.2613 0.2258 0.070 Uiso 1 1 calc R . . C26 C 0.4708(3) -0.1185(2) 0.19127(19) 0.0482(7) Uani 1 1 d . . . H22A H 0.5035 -0.1325 0.1400 0.058 Uiso 1 1 calc R . . C27 C 0.4527(2) -0.02040(19) 0.21362(16) 0.0382(6) Uani 1 1 d . . . C29 C 0.3114(3) -0.0624(2) 0.42278(17) 0.0494(7) Uani 1 1 d . . . H24A H 0.2948 0.0098 0.4288 0.059 Uiso 1 1 calc R . . C30 C 0.3783(4) -0.0922(5) 0.4762(3) 0.1015(17) Uani 1 1 d . . . H25A H 0.4443 -0.0567 0.4621 0.152 Uiso 1 1 calc R . . H25B H 0.3934 -0.1634 0.4730 0.152 Uiso 1 1 calc R . . H25C H 0.3399 -0.0758 0.5279 0.152 Uiso 1 1 calc R . . C31 C 0.2081(4) -0.1161(3) 0.4445(2) 0.0798(12) Uani 1 1 d . . . H26A H 0.1655 -0.0963 0.4101 0.120 Uiso 1 1 calc R . . H26B H 0.1699 -0.0993 0.4962 0.120 Uiso 1 1 calc R . . H26C H 0.2222 -0.1875 0.4414 0.120 Uiso 1 1 calc R . . C32 C 0.4883(2) 0.0617(2) 0.15635(17) 0.0433(6) Uani 1 1 d . . . H27A H 0.4698 0.1262 0.1825 0.052 Uiso 1 1 calc R . . C33 C 0.4346(3) 0.0587(3) 0.0938(2) 0.0611(9) Uani 1 1 d . . . H28A H 0.4588 0.1131 0.0581 0.092 Uiso 1 1 calc R . . H28B H 0.3583 0.0653 0.1148 0.092 Uiso 1 1 calc R . . H28C H 0.4515 -0.0042 0.0676 0.092 Uiso 1 1 calc R . . C34 C 0.6073(3) 0.0580(5) 0.1197(3) 0.121(2) Uani 1 1 d . . . H29A H 0.6451 0.0608 0.1588 0.181 Uiso 1 1 calc R . . H29B H 0.6262 0.1143 0.0850 0.181 Uiso 1 1 calc R . . H29C H 0.6264 -0.0035 0.0918 0.181 Uiso 1 1 calc R . . C36 C 0.3083(2) 0.26788(19) 0.04030(15) 0.0368(6) Uani 1 1 d . . . C37 C 0.2675(2) 0.1866(2) 0.01327(15) 0.0397(6) Uani 1 1 d . . . H31A H 0.2988 0.1712 -0.0380 0.048 Uiso 1 1 calc R . . C38 C 0.1870(2) 0.12456(18) 0.05128(15) 0.0359(6) Uani 1 1 d . . . C35 C 0.3855(3) 0.3273(2) -0.01966(17) 0.0538(8) Uani 1 1 d . . . H33A H 0.4095 0.3831 0.0039 0.081 Uiso 1 1 calc R . . H33B H 0.3506 0.3520 -0.0576 0.081 Uiso 1 1 calc R . . H33C H 0.4460 0.2850 -0.0438 0.081 Uiso 1 1 calc R . . C39 C 0.1407(3) 0.0637(2) -0.00048(17) 0.0484(7) Uani 1 1 d . . . H34A H 0.0846 0.0229 0.0300 0.073 Uiso 1 1 calc R . . H34B H 0.1959 0.0212 -0.0314 0.073 Uiso 1 1 calc R . . H34C H 0.1118 0.1080 -0.0332 0.073 Uiso 1 1 calc R . . C40 C 0.4087(2) 0.41850(19) 0.13472(15) 0.0373(6) Uani 1 1 d . . . C41 C 0.4299(3) 0.5176(2) 0.14245(17) 0.0464(7) Uani 1 1 d . . . H36A H 0.4957 0.5340 0.1502 0.056 Uiso 1 1 calc R . . C42 C 0.3578(3) 0.5919(2) 0.13905(18) 0.0520(8) Uani 1 1 d . . . H37A H 0.3747 0.6588 0.1432 0.062 Uiso 1 1 calc R . . C43 C 0.2612(3) 0.5689(2) 0.12958(18) 0.0497(7) Uani 1 1 d . . . H38A H 0.2113 0.6202 0.1277 0.060 Uiso 1 1 calc R . . C44 C 0.2356(2) 0.4713(2) 0.12268(17) 0.0434(7) Uani 1 1 d . . . C45 C 0.3106(2) 0.39583(18) 0.12390(14) 0.0346(5) Uani 1 1 d . . . C46 C 0.4927(2) 0.3412(2) 0.13610(16) 0.0426(6) Uani 1 1 d . . . H41A H 0.4686 0.2766 0.1225 0.051 Uiso 1 1 calc R . . C47 C 0.5990(3) 0.3638(3) 0.0800(2) 0.0644(10) Uani 1 1 d . . . H42A H 0.5894 0.3706 0.0291 0.097 Uiso 1 1 calc R . . H42B H 0.6495 0.3097 0.0813 0.097 Uiso 1 1 calc R . . H42C H 0.6256 0.4254 0.0939 0.097 Uiso 1 1 calc R . . C48 C 0.5100(3) 0.3307(3) 0.21500(18) 0.0533(8) Uani 1 1 d . . . H43A H 0.4430 0.3169 0.2515 0.080 Uiso 1 1 calc R . . H43B H 0.5376 0.3921 0.2282 0.080 Uiso 1 1 calc R . . H43C H 0.5603 0.2763 0.2158 0.080 Uiso 1 1 calc R . . C49 C 0.1283(3) 0.4500(2) 0.1109(2) 0.0629(10) Uani 1 1 d . . . H44A H 0.1138 0.3795 0.1258 0.076 Uiso 1 1 calc R . . C50 C 0.0402(3) 0.5116(4) 0.1605(4) 0.1048(19) Uani 1 1 d . . . H45A H -0.0268 0.4950 0.1507 0.157 Uiso 1 1 calc R . . H45B H 0.0534 0.5817 0.1494 0.157 Uiso 1 1 calc R . . H45C H 0.0371 0.4977 0.2135 0.157 Uiso 1 1 calc R . . C51 C 0.1290(4) 0.4600(4) 0.0279(3) 0.0997(17) Uani 1 1 d . . . H46A H 0.0592 0.4457 0.0221 0.149 Uiso 1 1 calc R . . H46B H 0.1810 0.4133 -0.0017 0.149 Uiso 1 1 calc R . . H46C H 0.1474 0.5274 0.0100 0.149 Uiso 1 1 calc R . . C57 C 0.0561(2) 0.06285(19) 0.15375(15) 0.0355(6) Uani 1 1 d . . . C52 C -0.0421(2) 0.1105(2) 0.16041(18) 0.0463(7) Uani 1 1 d . . . C53 C -0.1328(3) 0.0549(3) 0.1862(2) 0.0611(9) Uani 1 1 d . . . H49A H -0.1998 0.0859 0.1913 0.073 Uiso 1 1 calc R . . C54 C -0.1268(3) -0.0432(3) 0.2043(2) 0.0676(11) Uani 1 1 d . . . H50A H -0.1892 -0.0797 0.2210 0.081 Uiso 1 1 calc R . . C55 C -0.0309(3) -0.0886(3) 0.19823(19) 0.0571(9) Uani 1 1 d . . . H51A H -0.0280 -0.1565 0.2114 0.069 Uiso 1 1 calc R . . C56 C 0.0634(2) -0.0374(2) 0.17300(15) 0.0397(6) Uani 1 1 d . . . C58 C -0.0546(3) 0.2180(3) 0.1408(3) 0.0715(12) Uani 1 1 d . . . H53A H 0.0135 0.2508 0.1373 0.086 Uiso 1 1 calc R . . C59 C -0.0806(5) 0.2301(4) 0.0639(3) 0.1068(18) Uani 1 1 d . . . H54A H -0.0244 0.1990 0.0248 0.160 Uiso 1 1 calc R . . H54B H -0.0866 0.3004 0.0519 0.160 Uiso 1 1 calc R . . H54C H -0.1473 0.1984 0.0663 0.160 Uiso 1 1 calc R . . C60 C -0.1409(4) 0.2705(4) 0.2008(4) 0.113(2) Uani 1 1 d . . . H55A H -0.1244 0.2646 0.2496 0.169 Uiso 1 1 calc R . . H55B H -0.2086 0.2402 0.2042 0.169 Uiso 1 1 calc R . . H55C H -0.1450 0.3404 0.1869 0.169 Uiso 1 1 calc R . . C61 C 0.1671(2) -0.0923(2) 0.16733(17) 0.0453(7) Uani 1 1 d . . . H56A H 0.2209 -0.0420 0.1676 0.054 Uiso 1 1 calc R . . C62 C 0.2056(4) -0.1503(3) 0.0947(2) 0.0839(13) Uani 1 1 d . . . H57A H 0.2095 -0.1060 0.0514 0.126 Uiso 1 1 calc R . . H57B H 0.1566 -0.2030 0.0942 0.126 Uiso 1 1 calc R . . H57C H 0.2755 -0.1792 0.0921 0.126 Uiso 1 1 calc R . . C63 C 0.1634(3) -0.1632(2) 0.2341(2) 0.0581(8) Uani 1 1 d . . . H58A H 0.1371 -0.1276 0.2814 0.087 Uiso 1 1 calc R . . H58B H 0.2342 -0.1900 0.2311 0.087 Uiso 1 1 calc R . . H58C H 0.1165 -0.2174 0.2325 0.087 Uiso 1 1 calc R . . C1 C 0.1710(2) 0.31638(19) 0.28890(16) 0.0353(6) Uani 1 1 d . . . C2 C 0.0547(3) 0.3096(3) 0.3223(3) 0.0969(18) Uani 1 1 d . . . H60A H 0.0316 0.3675 0.3550 0.116 Uiso 1 1 calc R . . H60B H 0.0204 0.3162 0.2806 0.116 Uiso 1 1 calc R . . C3 C 0.0146(3) 0.2234(3) 0.3656(3) 0.0825(14) Uani 1 1 d . . . H61A H -0.0629 0.2283 0.3754 0.099 Uiso 1 1 calc R . . H61B H 0.0305 0.2296 0.4149 0.099 Uiso 1 1 calc R . . C4 C 0.0447(3) 0.1245(3) 0.3412(2) 0.0841(15) Uani 1 1 d . . . H62A H 0.0008 0.1065 0.3076 0.101 Uiso 1 1 calc R . . H62B H 0.0246 0.0809 0.3863 0.101 Uiso 1 1 calc R . . C5 C 0.1604(2) 0.0974(2) 0.29998(16) 0.0357(6) Uani 1 1 d . . . C64 C 0.7198(7) 0.4095(10) 0.3667(5) 0.251(8) Uani 1 1 d D . . H64A H 0.6580 0.3761 0.3974 0.377 Uiso 1 1 calc R . . H64B H 0.7608 0.4345 0.3994 0.377 Uiso 1 1 calc R . . H64C H 0.7634 0.3629 0.3310 0.377 Uiso 1 1 calc R . . C65 C 0.6898(9) 0.4828(8) 0.3298(10) 0.292(12) Uani 1 1 d D . . H65A H 0.6541 0.4484 0.2969 0.351 Uiso 1 1 calc R . . H65B H 0.6321 0.5134 0.3691 0.351 Uiso 1 1 calc R . . C66 C 0.7283(9) 0.5600(10) 0.2876(5) 0.242(9) Uani 1 1 d D . . H66A H 0.7940 0.5329 0.2538 0.290 Uiso 1 1 calc R . . H66B H 0.7515 0.6020 0.3232 0.290 Uiso 1 1 calc R . . C67 C 0.6947(11) 0.6260(10) 0.2433(10) 0.328(13) Uani 1 1 d D . . H67A H 0.6382 0.6659 0.2769 0.394 Uiso 1 1 calc R . . H67B H 0.6607 0.5880 0.2112 0.394 Uiso 1 1 calc R . . C68 C 0.7626(11) 0.6949(7) 0.1938(8) 0.248(7) Uani 1 1 d D . . H68A H 0.7198 0.7440 0.1746 0.373 Uiso 1 1 calc R . . H68B H 0.8089 0.6593 0.1516 0.373 Uiso 1 1 calc R . . H68C H 0.8053 0.7281 0.2218 0.373 Uiso 1 1 calc R . . Cr1 Cr 0.27792(3) 0.19764(3) 0.31931(2) 0.02584(12) Uani 1 1 d . . . Cr2 Cr 0.20779(3) 0.20488(3) 0.20231(2) 0.02619(12) Uani 1 1 d . . . H59A H 0.203(2) 0.337(2) 0.3225(16) 0.031 Uiso 1 1 d . . . H63A H 0.189(2) 0.077(2) 0.3313(17) 0.031 Uiso 1 1 d . . . H59B H 0.186(2) 0.371(2) 0.2562(16) 0.031 Uiso 1 1 d . . . H63B H 0.162(2) 0.049(2) 0.2705(16) 0.031 Uiso 1 1 d . . . N1 N 0.32066(16) 0.27890(14) 0.40343(11) 0.0286(4) Uani 1 1 d . . . N2 N 0.40059(16) 0.09796(14) 0.31875(12) 0.0298(4) Uani 1 1 d . . . N3 N 0.28314(16) 0.29571(15) 0.11228(12) 0.0318(4) Uani 1 1 d . . . N4 N 0.15071(16) 0.11973(15) 0.12569(12) 0.0317(4) 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 C7 0.0364(13) 0.0310(12) 0.0310(13) -0.0009(10) -0.0117(11) -0.0057(10) C8 0.0306(12) 0.0383(13) 0.0388(14) -0.0025(11) -0.0164(11) -0.0041(10) C9 0.0323(13) 0.0368(13) 0.0362(13) -0.0015(11) -0.0135(11) 0.0011(10) C6 0.0513(17) 0.0437(15) 0.0471(16) -0.0118(13) -0.0259(14) -0.0007(13) C10 0.0381(15) 0.0573(18) 0.067(2) -0.0182(16) -0.0258(15) 0.0112(13) C16 0.0324(13) 0.0332(12) 0.0322(13) -0.0070(10) -0.0104(10) -0.0031(10) C11 0.0427(15) 0.0333(13) 0.0402(15) -0.0076(11) -0.0096(12) 0.0001(11) C12 0.059(2) 0.0435(16) 0.0515(18) -0.0126(14) -0.0079(15) 0.0102(14) C13 0.055(2) 0.065(2) 0.0466(18) -0.0169(16) 0.0015(15) 0.0135(16) C14 0.0487(17) 0.0624(19) 0.0363(15) -0.0033(14) -0.0002(13) -0.0007(15) C15 0.0427(15) 0.0440(14) 0.0284(13) -0.0049(11) -0.0067(11) -0.0040(12) C17 0.0594(19) 0.0277(13) 0.0576(19) -0.0006(13) -0.0010(15) -0.0014(13) C18 0.077(2) 0.0397(16) 0.0519(19) -0.0005(14) -0.0133(17) -0.0041(15) C19 0.069(2) 0.050(2) 0.127(4) 0.028(2) -0.037(3) -0.0154(18) C20 0.072(2) 0.0451(17) 0.0416(17) 0.0061(14) 0.0082(16) -0.0076(16) C21 0.111(4) 0.078(3) 0.087(3) 0.023(2) -0.021(3) -0.048(3) C22 0.117(4) 0.083(3) 0.158(5) 0.063(3) -0.068(4) -0.013(3) C28 0.0353(13) 0.0302(12) 0.0394(14) -0.0039(10) -0.0190(11) 0.0037(10) C23 0.0511(16) 0.0312(12) 0.0482(16) -0.0026(11) -0.0273(14) 0.0025(11) C24 0.074(2) 0.0294(13) 0.062(2) 0.0013(13) -0.0344(18) 0.0033(13) C25 0.078(2) 0.0326(14) 0.074(2) -0.0184(15) -0.037(2) 0.0150(15) C26 0.0538(18) 0.0426(15) 0.0510(17) -0.0157(13) -0.0186(15) 0.0100(13) C27 0.0375(14) 0.0369(13) 0.0442(15) -0.0079(11) -0.0178(12) 0.0054(11) C29 0.072(2) 0.0369(14) 0.0431(16) 0.0064(12) -0.0219(15) -0.0018(14) C30 0.104(4) 0.157(5) 0.056(3) 0.004(3) -0.043(3) -0.001(3) C31 0.087(3) 0.087(3) 0.060(2) 0.008(2) -0.008(2) -0.024(2) C32 0.0425(15) 0.0466(15) 0.0402(15) -0.0064(12) -0.0095(13) 0.0006(12) C33 0.069(2) 0.065(2) 0.053(2) 0.0060(17) -0.0225(17) -0.0042(18) C34 0.042(2) 0.182(6) 0.138(5) 0.083(4) -0.028(3) -0.024(3) C36 0.0394(14) 0.0361(13) 0.0352(14) 0.0051(11) -0.0097(11) -0.0068(11) C37 0.0498(16) 0.0418(14) 0.0269(12) -0.0026(11) -0.0084(11) -0.0035(12) C38 0.0426(14) 0.0329(12) 0.0346(13) -0.0037(10) -0.0140(12) -0.0024(11) C35 0.066(2) 0.0591(19) 0.0338(15) 0.0073(14) -0.0063(14) -0.0222(16) C39 0.0599(19) 0.0490(16) 0.0419(16) -0.0069(13) -0.0216(14) -0.0108(14) C40 0.0415(14) 0.0375(13) 0.0320(13) 0.0042(11) -0.0077(11) -0.0101(11) C41 0.0548(18) 0.0453(15) 0.0413(16) 0.0056(13) -0.0148(14) -0.0211(14) C42 0.074(2) 0.0324(14) 0.0495(18) 0.0022(13) -0.0138(16) -0.0149(14) C43 0.063(2) 0.0318(13) 0.0509(18) 0.0058(13) -0.0094(15) -0.0002(13) C44 0.0468(16) 0.0339(13) 0.0488(17) 0.0091(12) -0.0120(13) -0.0044(12) C45 0.0415(14) 0.0304(12) 0.0322(13) 0.0067(10) -0.0099(11) -0.0080(11) C46 0.0361(14) 0.0490(16) 0.0431(16) 0.0059(13) -0.0109(12) -0.0084(12) C47 0.0458(18) 0.086(3) 0.055(2) 0.0150(19) -0.0019(16) -0.0067(17) C48 0.0497(18) 0.065(2) 0.0481(18) 0.0158(15) -0.0183(15) -0.0115(15) C49 0.0508(19) 0.0422(16) 0.103(3) 0.0194(18) -0.034(2) -0.0012(14) C50 0.054(2) 0.083(3) 0.169(6) 0.018(3) -0.018(3) 0.014(2) C51 0.092(3) 0.105(4) 0.127(4) 0.012(3) -0.075(3) 0.002(3) C57 0.0340(13) 0.0415(13) 0.0342(13) -0.0070(11) -0.0131(11) -0.0104(11) C52 0.0372(15) 0.0560(17) 0.0520(17) -0.0073(14) -0.0215(13) -0.0069(13) C53 0.0340(16) 0.092(3) 0.062(2) -0.0009(19) -0.0190(15) -0.0135(16) C54 0.0476(19) 0.094(3) 0.067(2) 0.016(2) -0.0233(17) -0.0358(19) C55 0.061(2) 0.0589(19) 0.057(2) 0.0135(16) -0.0220(16) -0.0315(17) C56 0.0450(15) 0.0413(14) 0.0356(14) -0.0013(11) -0.0141(12) -0.0138(12) C58 0.0442(18) 0.0525(19) 0.128(4) -0.011(2) -0.040(2) 0.0038(15) C59 0.119(4) 0.087(3) 0.111(4) 0.029(3) -0.031(3) 0.032(3) C60 0.090(3) 0.103(4) 0.167(6) -0.060(4) -0.074(4) 0.042(3) C61 0.0559(18) 0.0302(13) 0.0496(17) -0.0020(12) -0.0129(14) -0.0071(12) C62 0.134(4) 0.057(2) 0.054(2) -0.0035(18) -0.014(2) 0.027(2) C63 0.072(2) 0.0486(17) 0.058(2) 0.0040(15) -0.0261(18) -0.0052(16) C1 0.0403(14) 0.0297(12) 0.0391(14) -0.0050(11) -0.0161(12) 0.0037(11) C2 0.0358(18) 0.058(2) 0.179(5) -0.041(3) 0.006(2) 0.0049(16) C3 0.0407(19) 0.109(3) 0.078(3) 0.024(3) 0.0157(18) 0.017(2) C4 0.077(3) 0.074(3) 0.075(3) -0.023(2) 0.033(2) -0.041(2) C5 0.0457(15) 0.0322(13) 0.0349(14) 0.0024(11) -0.0198(12) -0.0112(11) C64 0.163(9) 0.46(2) 0.103(6) -0.092(9) 0.039(6) -0.172(11) C65 0.181(11) 0.233(14) 0.52(3) -0.194(17) -0.202(16) 0.128(11) C66 0.206(12) 0.40(2) 0.102(6) -0.005(9) 0.015(7) -0.172(14) C67 0.284(19) 0.240(16) 0.55(4) -0.11(2) -0.27(2) 0.135(15) C68 0.39(2) 0.128(8) 0.306(16) 0.036(9) -0.219(15) -0.062(10) Cr1 0.0264(2) 0.02418(19) 0.0282(2) -0.00139(15) -0.00933(16) -0.00137(14) Cr2 0.0265(2) 0.02444(19) 0.0286(2) -0.00039(15) -0.00858(16) -0.00268(14) N1 0.0312(10) 0.0285(9) 0.0267(10) -0.0016(8) -0.0081(8) -0.0032(8) N2 0.0319(10) 0.0271(9) 0.0326(11) -0.0036(8) -0.0121(9) 0.0004(8) N3 0.0342(11) 0.0285(10) 0.0340(11) 0.0019(8) -0.0109(9) -0.0049(8) N4 0.0321(11) 0.0313(10) 0.0336(11) -0.0019(8) -0.0113(9) -0.0044(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C7 N1 1.331(3) . ? C7 C8 1.397(4) . ? C7 C6 1.520(3) . ? C8 C9 1.399(4) . ? C9 N2 1.343(3) . ? C9 C10 1.527(4) . ? C16 C11 1.410(4) . ? C16 C15 1.410(4) . ? C16 N1 1.449(3) . ? C11 C12 1.400(4) . ? C11 C17 1.522(4) . ? C12 C13 1.378(5) . ? C13 C14 1.369(5) . ? C14 C15 1.392(4) . ? C15 C20 1.520(4) . ? C17 C19 1.537(5) . ? C17 C18 1.539(5) . ? C20 C22 1.514(6) . ? C20 C21 1.523(5) . ? C28 C27 1.404(4) . ? C28 C23 1.406(4) . ? C28 N2 1.460(3) . ? C23 C24 1.397(4) . ? C23 C29 1.515(4) . ? C24 C25 1.382(5) . ? C25 C26 1.372(5) . ? C26 C27 1.397(4) . ? C27 C32 1.514(4) . ? C29 C31 1.519(5) . ? C29 C30 1.525(5) . ? C32 C33 1.504(4) . ? C32 C34 1.537(5) . ? C36 N3 1.338(3) . ? C36 C37 1.398(4) . ? C36 C35 1.524(4) . ? C37 C38 1.401(4) . ? C38 N4 1.328(3) . ? C38 C39 1.527(4) . ? C40 C41 1.399(4) . ? C40 C45 1.403(4) . ? C40 C46 1.507(4) . ? C41 C42 1.378(5) . ? C42 C43 1.376(5) . ? C43 C44 1.393(4) . ? C44 C45 1.406(4) . ? C44 C49 1.524(4) . ? C45 N3 1.451(3) . ? C46 C48 1.531(4) . ? C46 C47 1.542(4) . ? C49 C50 1.517(6) . ? C49 C51 1.528(6) . ? C57 C52 1.406(4) . ? C57 C56 1.405(4) . ? C57 N4 1.457(3) . ? C52 C53 1.402(4) . ? C52 C58 1.509(5) . ? C53 C54 1.370(5) . ? C54 C55 1.368(5) . ? C55 C56 1.407(4) . ? C56 C61 1.518(4) . ? C58 C60 1.533(6) . ? C58 C59 1.545(7) . ? C61 C62 1.526(5) . ? C61 C63 1.537(4) . ? C1 C2 1.500(4) . ? C1 Cr2 2.172(3) . ? C1 Cr1 2.266(3) . ? C2 C3 1.434(6) . ? C3 C4 1.436(6) . ? C4 C5 1.553(5) . ? C5 Cr1 2.194(3) . ? C5 Cr2 2.258(3) . ? C64 C65 1.301(11) . ? C65 C66 1.322(12) . ? C66 C67 1.341(11) . ? C67 C68 1.446(14) . ? Cr1 N2 2.075(2) . ? Cr1 N1 2.121(2) . ? Cr1 Cr2 2.5557(8) . ? Cr2 N3 2.091(2) . ? Cr2 N4 2.138(2) . ? 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 C7 C8 123.8(2) . . ? N1 C7 C6 121.6(2) . . ? C8 C7 C6 114.6(2) . . ? C7 C8 C9 128.5(2) . . ? N2 C9 C8 124.7(2) . . ? N2 C9 C10 120.5(2) . . ? C8 C9 C10 114.7(2) . . ? C11 C16 C15 120.6(2) . . ? C11 C16 N1 121.0(2) . . ? C15 C16 N1 118.4(2) . . ? C12 C11 C16 117.6(3) . . ? C12 C11 C17 119.1(3) . . ? C16 C11 C17 123.3(2) . . ? C13 C12 C11 122.0(3) . . ? C14 C13 C12 119.7(3) . . ? C13 C14 C15 121.3(3) . . ? C14 C15 C16 118.8(3) . . ? C14 C15 C20 119.1(3) . . ? C16 C15 C20 122.1(2) . . ? C11 C17 C19 111.2(3) . . ? C11 C17 C18 112.3(3) . . ? C19 C17 C18 108.5(2) . . ? C22 C20 C15 111.8(3) . . ? C22 C20 C21 109.4(3) . . ? C15 C20 C21 112.7(3) . . ? C27 C28 C23 121.0(2) . . ? C27 C28 N2 120.2(2) . . ? C23 C28 N2 118.6(2) . . ? C24 C23 C28 118.2(3) . . ? C24 C23 C29 119.2(3) . . ? C28 C23 C29 122.6(2) . . ? C25 C24 C23 121.1(3) . . ? C26 C25 C24 119.9(3) . . ? C25 C26 C27 121.5(3) . . ? C26 C27 C28 118.0(3) . . ? C26 C27 C32 119.6(3) . . ? C28 C27 C32 122.4(2) . . ? C23 C29 C31 111.2(3) . . ? C23 C29 C30 112.3(3) . . ? C31 C29 C30 110.0(3) . . ? C33 C32 C27 111.6(2) . . ? C33 C32 C34 107.1(3) . . ? C27 C32 C34 113.1(3) . . ? N3 C36 C37 124.9(2) . . ? N3 C36 C35 120.3(2) . . ? C37 C36 C35 114.8(2) . . ? C36 C37 C38 129.0(3) . . ? N4 C38 C37 124.0(2) . . ? N4 C38 C39 121.8(2) . . ? C37 C38 C39 114.2(2) . . ? C41 C40 C45 118.2(3) . . ? C41 C40 C46 118.9(2) . . ? C45 C40 C46 122.8(2) . . ? C42 C41 C40 121.7(3) . . ? C41 C42 C43 119.7(3) . . ? C42 C43 C44 120.8(3) . . ? C43 C44 C45 119.3(3) . . ? C43 C44 C49 118.7(3) . . ? C45 C44 C49 121.9(2) . . ? C40 C45 C44 120.2(2) . . ? C40 C45 N3 122.2(2) . . ? C44 C45 N3 117.6(2) . . ? C40 C46 C48 110.7(3) . . ? C40 C46 C47 112.9(2) . . ? C48 C46 C47 108.3(3) . . ? C50 C49 C44 112.8(4) . . ? C50 C49 C51 111.7(4) . . ? C44 C49 C51 111.4(3) . . ? C52 C57 C56 121.1(2) . . ? C52 C57 N4 118.4(2) . . ? C56 C57 N4 120.4(2) . . ? C53 C52 C57 118.2(3) . . ? C53 C52 C58 118.4(3) . . ? C57 C52 C58 123.4(3) . . ? C54 C53 C52 121.3(3) . . ? C53 C54 C55 120.1(3) . . ? C54 C55 C56 121.7(3) . . ? C57 C56 C55 117.6(3) . . ? C57 C56 C61 123.3(2) . . ? C55 C56 C61 119.1(3) . . ? C52 C58 C60 112.0(4) . . ? C52 C58 C59 111.0(3) . . ? C60 C58 C59 108.8(4) . . ? C56 C61 C62 113.1(3) . . ? C56 C61 C63 112.9(3) . . ? C62 C61 C63 108.3(3) . . ? C2 C1 Cr2 104.5(2) . . ? C2 C1 Cr1 118.5(3) . . ? Cr2 C1 Cr1 70.27(8) . . ? C3 C2 C1 118.9(3) . . ? C2 C3 C4 123.8(4) . . ? C3 C4 C5 120.8(3) . . ? C4 C5 Cr1 115.1(2) . . ? C4 C5 Cr2 106.4(2) . . ? Cr1 C5 Cr2 70.04(8) . . ? C66 C65 C64 140.5(13) . . ? C65 C66 C67 136.9(14) . . ? C66 C67 C68 123.6(13) . . ? N2 Cr1 N1 89.42(8) . . ? N2 Cr1 C5 100.14(10) . . ? N1 Cr1 C5 143.35(10) . . ? N2 Cr1 C1 164.71(10) . . ? N1 Cr1 C1 96.20(9) . . ? C5 Cr1 C1 83.78(10) . . ? N2 Cr1 Cr2 117.05(6) . . ? N1 Cr1 Cr2 146.45(6) . . ? C5 Cr1 Cr2 56.16(7) . . ? C1 Cr1 Cr2 53.14(7) . . ? N3 Cr2 N4 89.14(8) . . ? N3 Cr2 C1 97.82(10) . . ? N4 Cr2 C1 146.41(9) . . ? N3 Cr2 C5 168.19(9) . . ? N4 Cr2 C5 95.34(9) . . ? C1 Cr2 C5 84.47(11) . . ? N3 Cr2 Cr1 118.12(6) . . ? N4 Cr2 Cr1 144.86(6) . . ? C1 Cr2 Cr1 56.59(7) . . ? C5 Cr2 Cr1 53.80(7) . . ? C7 N1 C16 116.3(2) . . ? C7 N1 Cr1 124.08(17) . . ? C16 N1 Cr1 118.71(15) . . ? C9 N2 C28 113.3(2) . . ? C9 N2 Cr1 123.34(16) . . ? C28 N2 Cr1 123.33(15) . . ? C36 N3 C45 114.8(2) . . ? C36 N3 Cr2 123.62(16) . . ? C45 N3 Cr2 121.56(16) . . ? C38 N4 C57 115.5(2) . . ? C38 N4 Cr2 124.40(16) . . ? C57 N4 Cr2 119.50(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C7 C8 C9 -18.8(4) . . . . ? C6 C7 C8 C9 159.3(3) . . . . ? C7 C8 C9 N2 11.7(5) . . . . ? C7 C8 C9 C10 -165.7(3) . . . . ? C15 C16 C11 C12 0.2(4) . . . . ? N1 C16 C11 C12 -179.7(2) . . . . ? C15 C16 C11 C17 179.3(3) . . . . ? N1 C16 C11 C17 -0.5(4) . . . . ? C16 C11 C12 C13 0.1(5) . . . . ? C17 C11 C12 C13 -179.1(3) . . . . ? C11 C12 C13 C14 -0.4(5) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C13 C14 C15 C20 179.4(3) . . . . ? C11 C16 C15 C14 -0.2(4) . . . . ? N1 C16 C15 C14 179.7(2) . . . . ? C11 C16 C15 C20 -179.6(3) . . . . ? N1 C16 C15 C20 0.2(4) . . . . ? C12 C11 C17 C19 73.3(4) . . . . ? C16 C11 C17 C19 -105.9(3) . . . . ? C12 C11 C17 C18 -48.5(4) . . . . ? C16 C11 C17 C18 132.3(3) . . . . ? C14 C15 C20 C22 -79.8(4) . . . . ? C16 C15 C20 C22 99.6(4) . . . . ? C14 C15 C20 C21 44.0(4) . . . . ? C16 C15 C20 C21 -136.6(3) . . . . ? C27 C28 C23 C24 6.0(4) . . . . ? N2 C28 C23 C24 -169.4(2) . . . . ? C27 C28 C23 C29 -176.1(2) . . . . ? N2 C28 C23 C29 8.6(4) . . . . ? C28 C23 C24 C25 -1.6(4) . . . . ? C29 C23 C24 C25 -179.6(3) . . . . ? C23 C24 C25 C26 -3.1(5) . . . . ? C24 C25 C26 C27 3.5(5) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C25 C26 C27 C32 178.2(3) . . . . ? C23 C28 C27 C26 -5.6(4) . . . . ? N2 C28 C27 C26 169.7(2) . . . . ? C23 C28 C27 C32 177.1(2) . . . . ? N2 C28 C27 C32 -7.6(4) . . . . ? C24 C23 C29 C31 -54.3(4) . . . . ? C28 C23 C29 C31 127.7(3) . . . . ? C24 C23 C29 C30 69.5(4) . . . . ? C28 C23 C29 C30 -108.5(4) . . . . ? C26 C27 C32 C33 61.7(4) . . . . ? C28 C27 C32 C33 -121.1(3) . . . . ? C26 C27 C32 C34 -59.1(4) . . . . ? C28 C27 C32 C34 118.1(4) . . . . ? N3 C36 C37 C38 7.2(5) . . . . ? C35 C36 C37 C38 -171.8(3) . . . . ? C36 C37 C38 N4 -15.9(5) . . . . ? C36 C37 C38 C39 162.4(3) . . . . ? C45 C40 C41 C42 -0.5(4) . . . . ? C46 C40 C41 C42 177.7(3) . . . . ? C40 C41 C42 C43 1.5(5) . . . . ? C41 C42 C43 C44 -0.6(5) . . . . ? C42 C43 C44 C45 -1.3(5) . . . . ? C42 C43 C44 C49 -178.9(3) . . . . ? C41 C40 C45 C44 -1.4(4) . . . . ? C46 C40 C45 C44 -179.6(3) . . . . ? C41 C40 C45 N3 177.4(2) . . . . ? C46 C40 C45 N3 -0.8(4) . . . . ? C43 C44 C45 C40 2.3(4) . . . . ? C49 C44 C45 C40 179.8(3) . . . . ? C43 C44 C45 N3 -176.6(3) . . . . ? C49 C44 C45 N3 0.9(4) . . . . ? C41 C40 C46 C48 69.6(3) . . . . ? C45 C40 C46 C48 -112.2(3) . . . . ? C41 C40 C46 C47 -52.1(4) . . . . ? C45 C40 C46 C47 126.1(3) . . . . ? C43 C44 C49 C50 -42.6(5) . . . . ? C45 C44 C49 C50 139.9(3) . . . . ? C43 C44 C49 C51 83.9(4) . . . . ? C45 C44 C49 C51 -93.6(4) . . . . ? C56 C57 C52 C53 -0.6(4) . . . . ? N4 C57 C52 C53 178.9(3) . . . . ? C56 C57 C52 C58 179.8(3) . . . . ? N4 C57 C52 C58 -0.7(4) . . . . ? C57 C52 C53 C54 -0.3(5) . . . . ? C58 C52 C53 C54 179.4(4) . . . . ? C52 C53 C54 C55 0.9(6) . . . . ? C53 C54 C55 C56 -0.6(6) . . . . ? C52 C57 C56 C55 0.8(4) . . . . ? N4 C57 C56 C55 -178.7(2) . . . . ? C52 C57 C56 C61 -179.7(3) . . . . ? N4 C57 C56 C61 0.9(4) . . . . ? C54 C55 C56 C57 -0.2(5) . . . . ? C54 C55 C56 C61 -179.8(3) . . . . ? C53 C52 C58 C60 45.3(4) . . . . ? C57 C52 C58 C60 -135.1(3) . . . . ? C53 C52 C58 C59 -76.6(5) . . . . ? C57 C52 C58 C59 103.1(4) . . . . ? C57 C56 C61 C62 -97.3(3) . . . . ? C55 C56 C61 C62 82.3(4) . . . . ? C57 C56 C61 C63 139.3(3) . . . . ? C55 C56 C61 C63 -41.1(4) . . . . ? Cr2 C1 C2 C3 68.5(5) . . . . ? Cr1 C1 C2 C3 -6.6(6) . . . . ? C1 C2 C3 C4 -47.8(8) . . . . ? C2 C3 C4 C5 39.6(7) . . . . ? C3 C4 C5 Cr1 22.0(5) . . . . ? C3 C4 C5 Cr2 -53.2(5) . . . . ? C64 C65 C66 C67 169.4(19) . . . . ? C65 C66 C67 C68 -169.7(18) . . . . ? C4 C5 Cr1 N2 144.9(3) . . . . ? Cr2 C5 Cr1 N2 -115.87(8) . . . . ? C4 C5 Cr1 N1 42.0(3) . . . . ? Cr2 C5 Cr1 N1 141.24(12) . . . . ? C4 C5 Cr1 C1 -50.0(3) . . . . ? Cr2 C5 Cr1 C1 49.20(9) . . . . ? C4 C5 Cr1 Cr2 -99.2(3) . . . . ? C2 C1 Cr1 N2 150.3(3) . . . . ? Cr2 C1 Cr1 N2 54.1(3) . . . . ? C2 C1 Cr1 N1 -98.7(3) . . . . ? Cr2 C1 Cr1 N1 165.08(7) . . . . ? C2 C1 Cr1 C5 44.4(3) . . . . ? Cr2 C1 Cr1 C5 -51.80(9) . . . . ? C2 C1 Cr1 Cr2 96.2(3) . . . . ? C2 C1 Cr2 N3 125.9(3) . . . . ? Cr1 C1 Cr2 N3 -118.64(8) . . . . ? C2 C1 Cr2 N4 25.5(3) . . . . ? Cr1 C1 Cr2 N4 141.03(13) . . . . ? C2 C1 Cr2 C5 -65.8(3) . . . . ? Cr1 C1 Cr2 C5 49.69(9) . . . . ? C2 C1 Cr2 Cr1 -115.5(3) . . . . ? C4 C5 Cr2 N3 161.1(4) . . . . ? Cr1 C5 Cr2 N3 49.7(5) . . . . ? C4 C5 Cr2 N4 -87.0(2) . . . . ? Cr1 C5 Cr2 N4 161.67(8) . . . . ? C4 C5 Cr2 C1 59.3(2) . . . . ? Cr1 C5 Cr2 C1 -52.07(9) . . . . ? C4 C5 Cr2 Cr1 111.4(2) . . . . ? N2 Cr1 Cr2 N3 -85.79(10) . . . . ? N1 Cr1 Cr2 N3 52.75(13) . . . . ? C5 Cr1 Cr2 N3 -169.80(12) . . . . ? C1 Cr1 Cr2 N3 80.34(11) . . . . ? N2 Cr1 Cr2 N4 51.06(12) . . . . ? N1 Cr1 Cr2 N4 -170.40(14) . . . . ? C5 Cr1 Cr2 N4 -32.95(14) . . . . ? C1 Cr1 Cr2 N4 -142.81(14) . . . . ? N2 Cr1 Cr2 C1 -166.13(11) . . . . ? N1 Cr1 Cr2 C1 -27.59(14) . . . . ? C5 Cr1 Cr2 C1 109.86(13) . . . . ? N2 Cr1 Cr2 C5 84.02(12) . . . . ? N1 Cr1 Cr2 C5 -137.45(14) . . . . ? C1 Cr1 Cr2 C5 -109.86(13) . . . . ? C8 C7 N1 C16 167.9(2) . . . . ? C6 C7 N1 C16 -10.1(3) . . . . ? C8 C7 N1 Cr1 -1.3(3) . . . . ? C6 C7 N1 Cr1 -179.23(18) . . . . ? C11 C16 N1 C7 91.7(3) . . . . ? C15 C16 N1 C7 -88.1(3) . . . . ? C11 C16 N1 Cr1 -98.5(2) . . . . ? C15 C16 N1 Cr1 81.6(2) . . . . ? N2 Cr1 N1 C7 17.2(2) . . . . ? C5 Cr1 N1 C7 123.6(2) . . . . ? C1 Cr1 N1 C7 -148.5(2) . . . . ? Cr2 Cr1 N1 C7 -126.64(17) . . . . ? N2 Cr1 N1 C16 -151.69(17) . . . . ? C5 Cr1 N1 C16 -45.3(2) . . . . ? C1 Cr1 N1 C16 42.56(18) . . . . ? Cr2 Cr1 N1 C16 64.4(2) . . . . ? C8 C9 N2 C28 -168.5(2) . . . . ? C10 C9 N2 C28 8.8(4) . . . . ? C8 C9 N2 Cr1 14.3(4) . . . . ? C10 C9 N2 Cr1 -168.4(2) . . . . ? C27 C28 N2 C9 -88.3(3) . . . . ? C23 C28 N2 C9 87.1(3) . . . . ? C27 C28 N2 Cr1 88.9(3) . . . . ? C23 C28 N2 Cr1 -95.6(2) . . . . ? N1 Cr1 N2 C9 -23.2(2) . . . . ? C5 Cr1 N2 C9 -167.6(2) . . . . ? C1 Cr1 N2 C9 88.7(4) . . . . ? Cr2 Cr1 N2 C9 135.34(19) . . . . ? N1 Cr1 N2 C28 159.82(19) . . . . ? C5 Cr1 N2 C28 15.4(2) . . . . ? C1 Cr1 N2 C28 -88.3(4) . . . . ? Cr2 Cr1 N2 C28 -41.7(2) . . . . ? C37 C36 N3 C45 -163.1(3) . . . . ? C35 C36 N3 C45 15.8(4) . . . . ? C37 C36 N3 Cr2 15.9(4) . . . . ? C35 C36 N3 Cr2 -165.2(2) . . . . ? C40 C45 N3 C36 -89.4(3) . . . . ? C44 C45 N3 C36 89.4(3) . . . . ? C40 C45 N3 Cr2 91.6(3) . . . . ? C44 C45 N3 Cr2 -89.6(3) . . . . ? N4 Cr2 N3 C36 -21.8(2) . . . . ? C1 Cr2 N3 C36 -168.9(2) . . . . ? C5 Cr2 N3 C36 90.7(5) . . . . ? Cr1 Cr2 N3 C36 134.98(19) . . . . ? N4 Cr2 N3 C45 157.11(19) . . . . ? C1 Cr2 N3 C45 10.1(2) . . . . ? C5 Cr2 N3 C45 -90.3(5) . . . . ? Cr1 Cr2 N3 C45 -46.1(2) . . . . ? C37 C38 N4 C57 170.6(3) . . . . ? C39 C38 N4 C57 -7.6(4) . . . . ? C37 C38 N4 Cr2 -0.1(4) . . . . ? C39 C38 N4 Cr2 -178.3(2) . . . . ? C52 C57 N4 C38 -85.9(3) . . . . ? C56 C57 N4 C38 93.6(3) . . . . ? C52 C57 N4 Cr2 85.3(3) . . . . ? C56 C57 N4 Cr2 -95.2(3) . . . . ? N3 Cr2 N4 C38 14.5(2) . . . . ? C1 Cr2 N4 C38 117.4(2) . . . . ? C5 Cr2 N4 C38 -154.6(2) . . . . ? Cr1 Cr2 N4 C38 -128.40(18) . . . . ? N3 Cr2 N4 C57 -155.88(19) . . . . ? C1 Cr2 N4 C57 -53.0(3) . . . . ? C5 Cr2 N4 C57 35.1(2) . . . . ? Cr1 Cr2 N4 C57 61.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.703 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.072 _vrf_PLAT027_klat247 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 22.50 Deg. RESPONSE: Despite repeated attempts this compound consistently deposited as small, multiple, weakly-diffracting crystals. The structure presented represents the best of several trials. ; _vrf_PLAT230_klat247 ; PROBLEM: Hirshfeld Test RESPONSE: The is significant yet unresolvable disorder on the C1-C2-C3-C4 chain. ; _vrf_PLAT241_klat247 ; PROBLEM: Check High Ueq as Compared to Neighbors for C2 RESPONSE: The is significant yet unresolvable disorder on the C1-C2-C3-C4 chain. ; _vrf_PLAT360_klat247 ; PROBLEM: Short C(sp3)-C(sp3) Bond RESPONSE: Disorder along the pentane solvent axis causes libration shortening of the C-C bonds ; _vrf_PLAT413_klat247 ; PROBLEM: Short Inter XH3 .. XHn RESPONSE: H-positions on the C1-C2-C3-C4 are imprecise. see response to PLAT241. ; data_klat348g _database_code_depnum_ccdc_archive 'CCDC 918028' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H55 Cr N2 O' _chemical_formula_weight 595.83 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 Orthorhombic _symmetry_space_group_name_H-M Pnma 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 16.702(3) _cell_length_b 20.310(4) _cell_length_c 9.768(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3313.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 825 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 20.85 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8810 _exptl_absorpt_correction_T_max 0.9243 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 30650 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.37 _reflns_number_total 4153 _reflns_number_gt 2721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+0.5266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4153 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.10935(3) 0.2500 0.05200(5) 0.02832(17) Uani 1 2 d S . . N1 N 0.16364(11) 0.17785(8) 0.17472(17) 0.0261(4) Uani 1 1 d . A . C1 C 0.03004(16) 0.18261(15) -0.0611(3) 0.0559(8) Uani 1 1 d . . . H1A H 0.0188 0.1939 -0.1578 0.067 Uiso 1 1 calc R . . H1B H 0.0382 0.1349 -0.0455 0.067 Uiso 1 1 calc R . . C2 C -0.01335(14) 0.21604(13) 0.0368(3) 0.0442(6) Uani 1 1 d . . . H2 H -0.0430 0.1925 0.1037 0.053 Uiso 1 1 calc R . . C3 C 0.26808(18) 0.13161(11) 0.3260(3) 0.0511(7) Uani 1 1 d . C . H3A H 0.2680 0.1398 0.4249 0.077 Uiso 1 1 calc R . . H3B H 0.3234 0.1277 0.2936 0.077 Uiso 1 1 calc R . . H3C H 0.2392 0.0907 0.3067 0.077 Uiso 1 1 calc R . . C4 C 0.22750(13) 0.18816(9) 0.2533(2) 0.0264(5) Uani 1 1 d . . . C5 C 0.26011(16) 0.2500 0.2803(3) 0.0257(6) Uani 1 2 d S . . H5 H 0.3113 0.2500 0.3226 0.031 Uiso 1 2 calc SR . . C6 C 0.07808(16) 0.0927(3) 0.2596(3) 0.033(2) Uani 0.50 1 d PR A 1 C7 C 0.04771(16) 0.0290(3) 0.2589(3) 0.0482(19) Uani 0.50 1 d PR A 1 H7 H 0.0062 0.0170 0.3204 0.058 Uiso 0.50 1 calc PR B 1 C8 C 0.0786(5) -0.0171(4) 0.1673(10) 0.057(2) Uani 0.50 1 d P A 1 H8 H 0.0584 -0.0608 0.1670 0.068 Uiso 0.50 1 calc PR A 1 C9 C 0.1371(5) 0.0004(3) 0.0788(7) 0.0482(16) Uani 0.50 1 d P A 1 H9 H 0.1573 -0.0314 0.0163 0.058 Uiso 0.50 1 calc PR A 1 C10 C 0.1690(4) 0.0646(4) 0.0773(9) 0.0350(17) Uani 0.50 1 d P A 1 C11 C 0.1405(7) 0.1108(10) 0.1674(18) 0.029(2) Uani 0.50 1 d P A 1 C12 C 0.0449(8) 0.1415(5) 0.3621(10) 0.035(2) Uani 0.50 1 d P A 1 H12 H 0.0490 0.1861 0.3193 0.042 Uiso 0.50 1 calc PR A 1 C13 C -0.0441(3) 0.1308(3) 0.3991(7) 0.0554(15) Uani 0.50 1 d P A 1 H13A H -0.0759 0.1281 0.3149 0.083 Uiso 0.50 1 calc PR A 1 H13B H -0.0631 0.1678 0.4548 0.083 Uiso 0.50 1 calc PR A 1 H13C H -0.0498 0.0898 0.4509 0.083 Uiso 0.50 1 calc PR A 1 C14 C 0.0920(4) 0.1443(4) 0.4981(8) 0.0501(16) Uani 0.50 1 d P A 1 H14A H 0.0669 0.1764 0.5595 0.075 Uiso 0.50 1 calc PR A 1 H14B H 0.1474 0.1577 0.4797 0.075 Uiso 0.50 1 calc PR A 1 H14C H 0.0917 0.1008 0.5413 0.075 Uiso 0.50 1 calc PR A 1 C15 C 0.2311(5) 0.0805(3) -0.0253(7) 0.0356(15) Uani 0.50 1 d P A 1 H15 H 0.2482 0.1269 -0.0069 0.043 Uiso 0.50 1 calc PR A 1 C16 C 0.3075(4) 0.0374(4) -0.0131(9) 0.0470(18) Uani 0.50 1 d P A 1 H16A H 0.3284 0.0401 0.0805 0.070 Uiso 0.50 1 calc PR A 1 H16B H 0.3481 0.0534 -0.0774 0.070 Uiso 0.50 1 calc PR A 1 H16C H 0.2942 -0.0084 -0.0346 0.070 Uiso 0.50 1 calc PR A 1 C17 C 0.2026(4) 0.0788(4) -0.1712(7) 0.0606(18) Uani 0.50 1 d P A 1 H17A H 0.1882 0.0335 -0.1960 0.091 Uiso 0.50 1 calc PR A 1 H17B H 0.2453 0.0944 -0.2318 0.091 Uiso 0.50 1 calc PR A 1 H17C H 0.1555 0.1072 -0.1811 0.091 Uiso 0.50 1 calc PR A 1 C6' C 0.0643(4) 0.1048(3) 0.2945(7) 0.0250(12) Uani 0.50 1 d P A 2 C7' C 0.0226(4) 0.0454(3) 0.2969(7) 0.0476(17) Uani 0.50 1 d P A 2 H7' H -0.0155 0.0373 0.3672 0.057 Uiso 0.50 1 calc PR A 2 C8' C 0.0361(5) -0.0016(4) 0.1986(8) 0.056(2) Uani 0.50 1 d P A 2 H8' H 0.0075 -0.0420 0.2029 0.067 Uiso 0.50 1 calc PR A 2 C9' C 0.0892(5) 0.0082(4) 0.0951(8) 0.0519(18) Uani 0.50 1 d P A 2 H9' H 0.0976 -0.0255 0.0293 0.062 Uiso 0.50 1 calc PR A 2 C10' C 0.1316(4) 0.0672(4) 0.0843(9) 0.0360(17) Uani 0.50 1 d P A 2 C11' C 0.1180(7) 0.1142(8) 0.1877(16) 0.0221(19) Uani 0.50 1 d P A 2 C12' C 0.0497(8) 0.1544(6) 0.4061(9) 0.0291(19) Uani 0.50 1 d P A 2 H12' H 0.0877 0.1919 0.3924 0.035 Uiso 0.50 1 calc PR A 2 C13' C -0.0342(4) 0.1818(3) 0.4068(6) 0.0562(15) Uani 0.50 1 d P A 2 H13D H -0.0724 0.1462 0.4240 0.084 Uiso 0.50 1 calc PR A 2 H13E H -0.0457 0.2020 0.3178 0.084 Uiso 0.50 1 calc PR A 2 H13F H -0.0389 0.2151 0.4790 0.084 Uiso 0.50 1 calc PR A 2 C14' C 0.0669(4) 0.1238(3) 0.5473(6) 0.0486(15) Uani 0.50 1 d P A 2 H14D H 0.0606 0.1575 0.6184 0.073 Uiso 0.50 1 calc PR A 2 H14E H 0.1217 0.1067 0.5491 0.073 Uiso 0.50 1 calc PR A 2 H14F H 0.0292 0.0877 0.5643 0.073 Uiso 0.50 1 calc PR A 2 C15' C 0.1903(4) 0.0772(4) -0.0291(8) 0.0408(17) Uani 0.50 1 d P A 2 H15' H 0.2002 0.1256 -0.0373 0.049 Uiso 0.50 1 calc PR A 2 C16' C 0.2702(5) 0.0442(6) 0.0027(9) 0.057(3) Uani 0.50 1 d P A 2 H16D H 0.2941 0.0647 0.0839 0.086 Uiso 0.50 1 calc PR A 2 H16E H 0.3064 0.0494 -0.0755 0.086 Uiso 0.50 1 calc PR A 2 H16F H 0.2615 -0.0028 0.0201 0.086 Uiso 0.50 1 calc PR A 2 C17' C 0.1634(4) 0.0526(3) -0.1677(6) 0.0446(14) Uani 0.50 1 d P A 2 H17D H 0.1537 0.0050 -0.1630 0.067 Uiso 0.50 1 calc PR A 2 H17E H 0.2052 0.0615 -0.2356 0.067 Uiso 0.50 1 calc PR A 2 H17F H 0.1140 0.0752 -0.1944 0.067 Uiso 0.50 1 calc PR A 2 O1 O 0.20979(16) 0.2501(8) -0.0971(2) 0.0371(7) Uani 1 2 d S C -1 C18 C 0.1986(3) 0.2394(9) -0.2428(4) 0.047(4) Uani 0.50 1 d P C -1 H18A H 0.1663 0.2754 -0.2831 0.056 Uiso 0.50 1 calc PR C -1 H18B H 0.1707 0.1971 -0.2592 0.056 Uiso 0.50 1 calc PR C -1 C19 C 0.2804(3) 0.238(3) -0.3051(6) 0.096(11) Uani 0.50 1 d P C -1 H19A H 0.2816 0.2637 -0.3913 0.115 Uiso 0.50 1 calc PR C -1 H19B H 0.2972 0.1923 -0.3248 0.115 Uiso 0.50 1 calc PR C -1 C20 C 0.3350(3) 0.2692(6) -0.1979(5) 0.083(6) Uani 0.50 1 d P C -1 H20A H 0.3351 0.3179 -0.2045 0.100 Uiso 0.50 1 calc PR C -1 H20B H 0.3906 0.2527 -0.2052 0.100 Uiso 0.50 1 calc PR C -1 C21 C 0.2943(2) 0.2454(14) -0.0657(4) 0.052(3) Uani 0.50 1 d P C -1 H21A H 0.3096 0.1995 -0.0442 0.063 Uiso 0.50 1 calc PR C -1 H21B H 0.3085 0.2740 0.0128 0.063 Uiso 0.50 1 calc PR C -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 Cr1 0.0248(3) 0.0325(3) 0.0277(3) 0.000 -0.0044(2) 0.000 N1 0.0310(9) 0.0227(8) 0.0246(9) -0.0024(7) -0.0027(8) -0.0030(7) C1 0.0420(15) 0.0671(18) 0.0587(18) -0.0254(15) -0.0221(13) 0.0040(13) C2 0.0247(12) 0.0517(14) 0.0562(17) -0.0040(12) -0.0090(11) -0.0055(10) C3 0.079(2) 0.0264(12) 0.0483(16) -0.0064(11) -0.0324(14) 0.0114(12) C4 0.0320(11) 0.0246(10) 0.0227(10) -0.0013(8) -0.0015(8) 0.0044(8) C5 0.0229(14) 0.0303(14) 0.0240(15) 0.000 -0.0030(12) 0.000 C6 0.032(3) 0.037(4) 0.031(4) -0.010(3) -0.001(3) -0.003(3) C7 0.046(4) 0.044(4) 0.054(5) -0.004(4) 0.001(3) -0.023(3) C8 0.072(5) 0.025(3) 0.072(6) -0.009(4) -0.021(5) -0.015(4) C9 0.061(4) 0.034(3) 0.049(4) -0.012(3) -0.018(4) -0.006(3) C10 0.043(4) 0.028(3) 0.034(4) -0.005(2) -0.015(4) 0.001(4) C11 0.020(6) 0.036(4) 0.032(6) 0.004(4) 0.000(4) -0.006(5) C12 0.034(3) 0.042(6) 0.029(6) 0.006(4) 0.001(5) -0.008(4) C13 0.035(3) 0.058(4) 0.073(4) 0.011(3) 0.009(3) -0.006(3) C14 0.049(4) 0.064(4) 0.038(4) -0.003(3) 0.012(3) -0.002(3) C15 0.051(4) 0.029(3) 0.026(3) -0.007(2) -0.009(4) 0.019(4) C16 0.056(5) 0.034(3) 0.051(4) -0.005(3) -0.009(4) 0.005(4) C17 0.070(5) 0.062(5) 0.049(4) -0.006(4) -0.015(4) 0.022(4) C6' 0.031(3) 0.024(2) 0.020(3) -0.007(2) 0.001(2) -0.008(2) C7' 0.054(4) 0.049(3) 0.039(3) -0.014(3) 0.010(3) -0.021(3) C8' 0.076(6) 0.040(4) 0.052(4) -0.013(3) 0.010(4) -0.026(4) C9' 0.079(5) 0.035(4) 0.042(4) -0.012(3) 0.001(4) -0.017(4) C10' 0.046(4) 0.034(3) 0.029(3) -0.005(2) -0.002(4) -0.006(4) C11' 0.025(6) 0.023(3) 0.018(4) -0.003(3) 0.002(4) -0.008(5) C12' 0.030(4) 0.034(4) 0.023(5) -0.006(3) 0.006(4) -0.005(3) C13' 0.049(3) 0.074(4) 0.045(3) -0.013(3) 0.006(3) 0.005(3) C14' 0.060(4) 0.056(4) 0.030(3) 0.001(3) 0.000(3) -0.005(3) C15' 0.044(4) 0.037(3) 0.042(4) -0.009(2) 0.000(4) -0.001(4) C16' 0.047(5) 0.090(7) 0.035(3) -0.018(4) 0.000(4) -0.023(6) C17' 0.057(4) 0.046(4) 0.031(3) -0.005(3) 0.000(3) 0.012(3) O1 0.0315(14) 0.0533(17) 0.0266(12) -0.001(7) -0.0040(11) 0.023(5) C18 0.046(2) 0.066(11) 0.028(2) -0.001(3) -0.0084(17) -0.008(4) C19 0.057(3) 0.20(3) 0.034(3) -0.017(10) 0.005(2) -0.006(8) C20 0.044(3) 0.174(17) 0.031(2) -0.001(4) 0.007(2) -0.015(4) C21 0.0259(18) 0.095(7) 0.036(2) -0.026(7) -0.0030(16) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.0991(17) . ? Cr1 N1 2.0991(17) 8_565 ? Cr1 C2 2.167(2) 8_565 ? Cr1 C2 2.167(2) . ? Cr1 C1 2.202(3) 8_565 ? Cr1 C1 2.202(3) . ? Cr1 O1 2.222(3) . ? N1 C4 1.331(3) . ? N1 C11 1.42(2) . ? N1 C11' 1.506(16) . ? C1 C2 1.378(4) . ? C2 C2 1.379(5) 8_565 ? C3 C4 1.511(3) . ? C4 C5 1.394(2) . ? C5 C4 1.394(2) 8_565 ? C6 C7 1.390(9) . ? C6 C11 1.425(12) . ? C6 C12 1.513(9) . ? C7 C8 1.394(9) . ? C8 C9 1.353(12) . ? C9 C10 1.410(11) . ? C10 C11 1.371(19) . ? C10 C15 1.478(11) . ? C12 C14 1.545(11) . ? C12 C13 1.545(14) . ? C15 C17 1.504(9) . ? C15 C16 1.552(8) . ? C6' C7' 1.395(9) . ? C6' C11' 1.389(12) . ? C6' C12' 1.504(9) . ? C7' C8' 1.373(9) . ? C8' C9' 1.360(11) . ? C9' C10' 1.395(11) . ? C10' C11' 1.408(18) . ? C10' C15' 1.493(10) . ? C12' C13' 1.507(15) . ? C12' C14' 1.540(12) . ? C15' C17' 1.511(10) . ? C15' C16' 1.526(10) . ? O1 C21 1.447(5) . ? O1 C18 1.452(6) . ? C18 C19 1.496(7) . ? C19 C20 1.53(2) . ? C20 C21 1.538(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 N1 88.54(9) . 8_565 ? N1 Cr1 C2 132.05(9) . 8_565 ? N1 Cr1 C2 103.04(9) 8_565 8_565 ? N1 Cr1 C2 103.04(9) . . ? N1 Cr1 C2 132.05(9) 8_565 . ? C2 Cr1 C2 37.11(14) 8_565 . ? N1 Cr1 C1 168.61(9) . 8_565 ? N1 Cr1 C1 96.46(9) 8_565 8_565 ? C2 Cr1 C1 36.77(10) 8_565 8_565 ? C2 Cr1 C1 66.08(10) . 8_565 ? N1 Cr1 C1 96.46(9) . . ? N1 Cr1 C1 168.61(9) 8_565 . ? C2 Cr1 C1 66.08(10) 8_565 . ? C2 Cr1 C1 36.77(10) . . ? C1 Cr1 C1 76.86(16) 8_565 . ? N1 Cr1 O1 92.8(3) . . ? N1 Cr1 O1 92.7(3) 8_565 . ? C2 Cr1 O1 131.96(17) 8_565 . ? C2 Cr1 O1 132.0(2) . . ? C1 Cr1 O1 97.2(2) 8_565 . ? C1 Cr1 O1 97.2(3) . . ? C4 N1 C11 113.5(7) . . ? C4 N1 C11' 119.5(6) . . ? C4 N1 Cr1 124.46(13) . . ? C11 N1 Cr1 121.6(7) . . ? C11' N1 Cr1 115.4(6) . . ? C2 C1 Cr1 70.25(14) . . ? C1 C2 C2 119.51(18) . 8_565 ? C1 C2 Cr1 72.98(15) . . ? C2 C2 Cr1 71.44(7) 8_565 . ? N1 C4 C5 124.32(19) . . ? N1 C4 C3 120.73(19) . . ? C5 C4 C3 114.9(2) . . ? C4 C5 C4 128.6(3) 8_565 . ? C7 C6 C11 120.2(8) . . ? C7 C6 C12 118.6(5) . . ? C11 C6 C12 121.2(9) . . ? C6 C7 C8 119.6(4) . . ? C9 C8 C7 120.1(6) . . ? C8 C9 C10 121.5(7) . . ? C11 C10 C9 119.7(10) . . ? C11 C10 C15 122.0(9) . . ? C9 C10 C15 118.3(7) . . ? C10 C11 C6 119.0(15) . . ? C10 C11 N1 126.5(10) . . ? C6 C11 N1 114.5(11) . . ? C6 C12 C14 114.0(9) . . ? C6 C12 C13 114.5(7) . . ? C14 C12 C13 107.1(8) . . ? C10 C15 C17 114.5(7) . . ? C10 C15 C16 113.7(6) . . ? C17 C15 C16 108.7(6) . . ? C7' C6' C11' 117.0(9) . . ? C7' C6' C12' 119.1(7) . . ? C11' C6' C12' 123.9(10) . . ? C8' C7' C6' 120.5(6) . . ? C9' C8' C7' 121.6(6) . . ? C8' C9' C10' 121.0(7) . . ? C9' C10' C11' 116.4(8) . . ? C9' C10' C15' 120.4(7) . . ? C11' C10' C15' 123.1(8) . . ? C6' C11' C10' 123.4(12) . . ? C6' C11' N1 120.5(11) . . ? C10' C11' N1 116.1(8) . . ? C6' C12' C13' 113.7(7) . . ? C6' C12' C14' 110.4(9) . . ? C13' C12' C14' 108.6(8) . . ? C10' C15' C17' 115.1(6) . . ? C10' C15' C16' 111.3(7) . . ? C17' C15' C16' 107.2(6) . . ? C21 O1 C18 108.9(3) . . ? C21 O1 Cr1 126.6(2) . . ? C18 O1 Cr1 123.1(3) . . ? O1 C18 C19 106.5(5) . . ? C18 C19 C20 105.0(14) . . ? C19 C20 C21 100.4(11) . . ? O1 C21 C20 103.5(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cr1 N1 C4 -20.7(2) 8_565 . . . ? C2 Cr1 N1 C4 -126.99(18) 8_565 . . . ? C2 Cr1 N1 C4 -153.67(17) . . . . ? C1 Cr1 N1 C4 -137.0(5) 8_565 . . . ? C1 Cr1 N1 C4 169.58(18) . . . . ? O1 Cr1 N1 C4 72.0(4) . . . . ? N1 Cr1 N1 C11 167.3(5) 8_565 . . . ? C2 Cr1 N1 C11 61.0(6) 8_565 . . . ? C2 Cr1 N1 C11 34.3(5) . . . . ? C1 Cr1 N1 C11 51.0(8) 8_565 . . . ? C1 Cr1 N1 C11 -2.4(5) . . . . ? O1 Cr1 N1 C11 -100.0(6) . . . . ? N1 Cr1 N1 C11' 149.8(5) 8_565 . . . ? C2 Cr1 N1 C11' 43.5(5) 8_565 . . . ? C2 Cr1 N1 C11' 16.8(5) . . . . ? C1 Cr1 N1 C11' 33.5(7) 8_565 . . . ? C1 Cr1 N1 C11' -19.9(5) . . . . ? O1 Cr1 N1 C11' -117.5(6) . . . . ? N1 Cr1 C1 C2 103.16(17) . . . . ? N1 Cr1 C1 C2 -12.5(6) 8_565 . . . ? C2 Cr1 C1 C2 -30.25(15) 8_565 . . . ? C1 Cr1 C1 C2 -67.47(19) 8_565 . . . ? O1 Cr1 C1 C2 -163.2(3) . . . . ? Cr1 C1 C2 C2 56.24(10) . . . 8_565 ? N1 Cr1 C2 C1 -83.29(18) . . . . ? N1 Cr1 C2 C1 176.71(16) 8_565 . . . ? C2 Cr1 C2 C1 130.25(16) 8_565 . . . ? C1 Cr1 C2 C1 100.3(3) 8_565 . . . ? O1 Cr1 C2 C1 22.7(5) . . . . ? N1 Cr1 C2 C2 146.46(6) . . . 8_565 ? N1 Cr1 C2 C2 46.46(8) 8_565 . . 8_565 ? C1 Cr1 C2 C2 -29.99(11) 8_565 . . 8_565 ? C1 Cr1 C2 C2 -130.25(16) . . . 8_565 ? O1 Cr1 C2 C2 -107.5(5) . . . 8_565 ? C11 N1 C4 C5 -177.8(6) . . . . ? C11' N1 C4 C5 -160.5(5) . . . . ? Cr1 N1 C4 C5 9.6(3) . . . . ? C11 N1 C4 C3 -0.6(6) . . . . ? C11' N1 C4 C3 16.7(6) . . . . ? Cr1 N1 C4 C3 -173.15(17) . . . . ? N1 C4 C5 C4 11.9(5) . . . 8_565 ? C3 C4 C5 C4 -165.4(2) . . . 8_565 ? C11 C6 C7 C8 -0.1(9) . . . . ? C12 C6 C7 C8 -178.6(7) . . . . ? C6 C7 C8 C9 -0.6(9) . . . . ? C7 C8 C9 C10 0.6(11) . . . . ? C8 C9 C10 C11 0.2(14) . . . . ? C8 C9 C10 C15 -178.1(7) . . . . ? C9 C10 C11 C6 -1.0(19) . . . . ? C15 C10 C11 C6 177.3(9) . . . . ? C9 C10 C11 N1 -177.0(11) . . . . ? C15 C10 C11 N1 1(2) . . . . ? C7 C6 C11 C10 1.0(17) . . . . ? C12 C6 C11 C10 179.4(11) . . . . ? C7 C6 C11 N1 177.4(7) . . . . ? C12 C6 C11 N1 -4.1(17) . . . . ? C4 N1 C11 C10 -87.1(17) . . . . ? C11' N1 C11 C10 158(6) . . . . ? Cr1 N1 C11 C10 85.7(14) . . . . ? C4 N1 C11 C6 96.7(10) . . . . ? C11' N1 C11 C6 -18(4) . . . . ? Cr1 N1 C11 C6 -90.5(13) . . . . ? C7 C6 C12 C14 92.2(8) . . . . ? C11 C6 C12 C14 -86.3(12) . . . . ? C7 C6 C12 C13 -31.7(10) . . . . ? C11 C6 C12 C13 149.8(11) . . . . ? C11 C10 C15 C17 -112.5(11) . . . . ? C9 C10 C15 C17 65.8(8) . . . . ? C11 C10 C15 C16 121.7(11) . . . . ? C9 C10 C15 C16 -59.9(9) . . . . ? C11' C6' C7' C8' 1.2(13) . . . . ? C12' C6' C7' C8' -178.3(9) . . . . ? C6' C7' C8' C9' -0.9(13) . . . . ? C7' C8' C9' C10' -0.7(14) . . . . ? C8' C9' C10' C11' 1.9(14) . . . . ? C8' C9' C10' C15' 179.5(8) . . . . ? C7' C6' C11' C10' 0.0(18) . . . . ? C12' C6' C11' C10' 179.6(11) . . . . ? C7' C6' C11' N1 178.0(9) . . . . ? C12' C6' C11' N1 -2.4(18) . . . . ? C9' C10' C11' C6' -1.5(18) . . . . ? C15' C10' C11' C6' -179.1(10) . . . . ? C9' C10' C11' N1 -179.6(9) . . . . ? C15' C10' C11' N1 2.8(17) . . . . ? C4 N1 C11' C6' 78.9(12) . . . . ? C11 N1 C11' C6' 152(6) . . . . ? Cr1 N1 C11' C6' -92.1(12) . . . . ? C4 N1 C11' C10' -102.9(11) . . . . ? C11 N1 C11' C10' -30(4) . . . . ? Cr1 N1 C11' C10' 86.1(11) . . . . ? C7' C6' C12' C13' -64.9(11) . . . . ? C11' C6' C12' C13' 115.6(12) . . . . ? C7' C6' C12' C14' 57.5(11) . . . . ? C11' C6' C12' C14' -122.1(11) . . . . ? C9' C10' C15' C17' 41.8(11) . . . . ? C11' C10' C15' C17' -140.7(10) . . . . ? C9' C10' C15' C16' -80.5(9) . . . . ? C11' C10' C15' C16' 97.0(12) . . . . ? N1 Cr1 O1 C21 -39.6(18) . . . . ? N1 Cr1 O1 C21 49.1(18) 8_565 . . . ? C2 Cr1 O1 C21 159.4(16) 8_565 . . . ? C2 Cr1 O1 C21 -150.0(16) . . . . ? C1 Cr1 O1 C21 146.0(18) 8_565 . . . ? C1 Cr1 O1 C21 -136.5(18) . . . . ? N1 Cr1 O1 C18 125.3(13) . . . . ? N1 Cr1 O1 C18 -146.0(13) 8_565 . . . ? C2 Cr1 O1 C18 -35.7(16) 8_565 . . . ? C2 Cr1 O1 C18 15.0(15) . . . . ? C1 Cr1 O1 C18 -49.1(13) 8_565 . . . ? C1 Cr1 O1 C18 28.5(13) . . . . ? C21 O1 C18 C19 -9(3) . . . . ? Cr1 O1 C18 C19 -176(2) . . . . ? O1 C18 C19 C20 -17(3) . . . . ? C18 C19 C20 C21 34(3) . . . . ? C18 O1 C21 C20 30(2) . . . . ? Cr1 O1 C21 C20 -163.0(10) . . . . ? C19 C20 C21 O1 -39(2) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.728 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.069 _vrf_PLAT220_klat348g ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) RESPONSE: Most of the molecule display disorder causing a large range of Ueq. ; _vrf_PLAT413_klat348g ; PROBLEM: Short Inter XH3 .. XHn H23B .. H40A RESPONSE: H-atom positions are less precise because of the observed disorder. ;