Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Gregory A. Solan' 'Vernon Gibson' 'Claire Newton' 'Carl Redshaw' A.J.P.White D.J.Williams _publ_contact_author_name 'Dr Gregory A Solan' _publ_contact_author_address ; Department of Chemistry University of Leicester University Road Leicester LE1 7RH UNITED KINGDOM ; _publ_contact_author_email GAS8@LE.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Low Valent Chromium Complexes Bearing the N,O-chelating Pyridyl-enolate Ligands [OC(But)(=2-CHN5H3Me-x)]- (x-3,4,5 and 6) ; data_Compound_1 _database_code_CSD 216348 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H32 N2 O2 Cr' _chemical_formula_weight 432.52 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.883(4) _cell_length_b 10.2348(13) _cell_length_c 11.578(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.894(15) _cell_angle_gamma 90.00 _cell_volume 2350.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.32 _cell_measurement_theta_max 12.47 _exptl_crystal_description prisms _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method ? _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.68 _diffrn_reflns_number 2106 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2045 _reflns_number_observed 1733 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1101P)^2^+0.7950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2045 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_obs 0.0531 _refine_ls_wR_factor_all 0.1518 _refine_ls_wR_factor_obs 0.1418 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.052 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.5000 0.16430(5) 0.7500 0.0263(2) Uani 1 d S . N N 0.47520(11) 0.1733(2) 0.5716(2) 0.0274(5) Uani 1 d . . O O 0.59419(10) 0.1893(2) 0.7141(2) 0.0327(5) Uani 1 d . . C1 C 0.50407(13) 0.2721(2) 0.5134(2) 0.0286(6) Uani 1 d . . C2 C 0.4769(2) 0.3069(3) 0.4017(2) 0.0357(7) Uani 1 d . . H2A H 0.4946(2) 0.3799(3) 0.3631(2) 0.043 Uiso 1 calc R . C3 C 0.4254(2) 0.2358(3) 0.3492(2) 0.0419(7) Uani 1 d . . H3A H 0.4067(2) 0.2598(3) 0.2745(2) 0.050 Uiso 1 calc R . C4 C 0.4004(2) 0.1279(3) 0.4058(3) 0.0396(7) Uani 1 d . . H4A H 0.3669(2) 0.0737(3) 0.3681(3) 0.048 Uiso 1 calc R . C5 C 0.42519(14) 0.1009(3) 0.5175(2) 0.0321(6) Uani 1 d . . C6 C 0.56419(14) 0.3362(2) 0.5619(2) 0.0300(6) Uani 1 d . . H6A H 0.57508(14) 0.4180(2) 0.5291(2) 0.036 Uiso 1 calc R . C7 C 0.60702(14) 0.2911(3) 0.6504(2) 0.0288(6) Uani 1 d . . C8 C 0.39895(15) -0.0110(3) 0.5846(3) 0.0389(7) Uani 1 d . . H8A H 0.3724(10) -0.0690(12) 0.5320(4) 0.058 Uiso 1 calc R . H8B H 0.3704(9) 0.0225(3) 0.6437(13) 0.058 Uiso 1 calc R . H8C H 0.4369(2) -0.0596(13) 0.6220(16) 0.058 Uiso 1 calc R . C9 C 0.67503(15) 0.3547(3) 0.6841(2) 0.0345(6) Uani 1 d . . C10 C 0.6931(2) 0.4651(3) 0.6024(3) 0.0452(8) Uani 1 d . . H10A H 0.7370(2) 0.5018(3) 0.6285(3) 0.068 Uiso 1 calc R . H10B H 0.6587(2) 0.5337(3) 0.6026(3) 0.068 Uiso 1 calc R . H10C H 0.6951(2) 0.4306(3) 0.5238(3) 0.068 Uiso 1 calc R . C11 C 0.6718(2) 0.4092(4) 0.8068(3) 0.0626(11) Uani 1 d . . H11A H 0.7149(2) 0.4508(4) 0.8310(3) 0.094 Uiso 1 calc R . H11B H 0.6630(2) 0.3378(4) 0.8602(3) 0.094 Uiso 1 calc R . H11C H 0.6355(2) 0.4738(4) 0.8078(3) 0.094 Uiso 1 calc R . C12 C 0.7291(2) 0.2485(3) 0.6823(3) 0.0539(9) Uani 1 d . . H12A H 0.7734(2) 0.2867(3) 0.7037(3) 0.081 Uiso 1 calc R . H12B H 0.7290(2) 0.2111(3) 0.6044(3) 0.081 Uiso 1 calc R . H12C H 0.7195(2) 0.1797(3) 0.7377(3) 0.081 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0338(4) 0.0257(4) 0.0195(3) 0.000 0.0016(2) 0.000 N 0.0317(11) 0.0261(11) 0.0241(11) -0.0036(8) 0.0008(9) 0.0041(9) O 0.0368(10) 0.0332(10) 0.0282(10) 0.0088(8) 0.0027(8) -0.0012(8) C1 0.0378(14) 0.0244(12) 0.0238(12) -0.0019(10) 0.0036(10) 0.0059(11) C2 0.048(2) 0.0325(14) 0.0257(14) 0.0031(11) -0.0001(12) 0.0070(12) C3 0.053(2) 0.047(2) 0.0244(14) -0.0014(13) -0.0080(12) 0.0116(14) C4 0.042(2) 0.042(2) 0.034(2) -0.0099(13) -0.0077(12) 0.0028(13) C5 0.0372(14) 0.0298(14) 0.0291(14) -0.0094(11) 0.0011(11) 0.0040(11) C6 0.043(2) 0.0218(12) 0.0250(13) 0.0012(10) 0.0039(11) 0.0015(11) C7 0.0404(15) 0.0247(12) 0.0222(12) -0.0042(10) 0.0093(11) 0.0000(11) C8 0.043(2) 0.0351(15) 0.038(2) -0.0073(12) 0.0025(12) -0.0053(12) C9 0.042(2) 0.0362(15) 0.0261(14) -0.0034(11) 0.0040(12) -0.0053(12) C10 0.047(2) 0.038(2) 0.051(2) 0.0055(14) 0.0047(14) -0.0074(13) C11 0.077(2) 0.077(3) 0.034(2) -0.019(2) 0.005(2) -0.027(2) C12 0.043(2) 0.051(2) 0.067(2) 0.013(2) 0.000(2) 0.0032(15) _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 O 1.962(2) 2_656 ? Cr O 1.962(2) . ? Cr N 2.093(2) . ? Cr N 2.093(2) 2_656 ? N C5 1.358(4) . ? N C1 1.364(3) . ? O C7 1.312(3) . ? C1 C2 1.412(4) . ? C1 C6 1.444(4) . ? C2 C3 1.367(4) . ? C3 C4 1.392(5) . ? C4 C5 1.380(4) . ? C5 C8 1.498(4) . ? C6 C7 1.367(4) . ? C7 C9 1.528(4) . ? C9 C12 1.530(4) . ? C9 C11 1.531(4) . ? C9 C10 1.532(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 O Cr O 165.04(11) 2_656 . ? O Cr N 92.24(8) 2_656 . ? O Cr N 87.11(8) . . ? O Cr N 87.11(8) 2_656 2_656 ? O Cr N 92.24(8) . 2_656 ? N Cr N 174.98(11) . 2_656 ? C5 N C1 119.7(2) . . ? C5 N Cr 123.2(2) . . ? C1 N Cr 116.2(2) . . ? C7 O Cr 116.6(2) . . ? N C1 C2 119.5(2) . . ? N C1 C6 120.6(2) . . ? C2 C1 C6 119.8(2) . . ? C3 C2 C1 120.1(3) . . ? C2 C3 C4 119.6(3) . . ? C5 C4 C3 118.9(3) . . ? N C5 C4 121.8(3) . . ? N C5 C8 116.6(2) . . ? C4 C5 C8 121.6(3) . . ? C7 C6 C1 126.5(2) . . ? O C7 C6 123.7(2) . . ? O C7 C9 113.4(2) . . ? C6 C7 C9 122.9(2) . . ? C7 C9 C12 107.7(2) . . ? C7 C9 C11 107.5(2) . . ? C12 C9 C11 110.2(3) . . ? C7 C9 C10 113.4(2) . . ? C12 C9 C10 108.8(3) . . ? C11 C9 C10 109.3(3) . . ? _refine_diff_density_max 0.719 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.082 #===END data_Compound_2 _database_code_CSD 216349 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H18 N2 Cl2 Cr' _chemical_formula_weight 337.20 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.712(2) _cell_length_b 7.8885(7) _cell_length_c 8.0404(13) _cell_angle_alpha 116.841(9) _cell_angle_beta 112.573(13) _cell_angle_gamma 93.814(11) _cell_volume 385.54(12) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 5.19 _cell_measurement_theta_max 12.47 _exptl_crystal_description 'platy rhombs' _exptl_crystal_colour Purple _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.67 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method ? _exptl_crystal_F_000 174 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.7296 _exptl_absorpt_correction_T_max 0.9865 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.74 _diffrn_reflns_number 1372 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1267 _reflns_number_observed 1114 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.1099P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0227(120) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1260 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_obs 0.0274 _refine_ls_wR_factor_all 0.0743 _refine_ls_wR_factor_obs 0.0699 _refine_ls_goodness_of_fit_all 1.104 _refine_ls_goodness_of_fit_obs 1.127 _refine_ls_restrained_S_all 1.122 _refine_ls_restrained_S_obs 1.127 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.0000 0.0000 0.5000 0.0235(2) Uani 1 d S . Cl Cl 0.11460(7) 0.20444(8) 0.40327(8) 0.0344(2) Uani 1 d . . N N 0.2812(2) 0.1037(2) 0.7599(2) 0.0246(4) Uani 1 d . . C1 C 0.4231(3) 0.0184(3) 0.7357(3) 0.0267(4) Uani 1 d . . C2 C 0.6138(3) 0.0975(3) 0.8973(3) 0.0312(5) Uani 1 d . . H2A H 0.7108(3) 0.0368(3) 0.8777(3) 0.037 Uiso 1 calc R . C3 C 0.6606(3) 0.2655(3) 1.0868(3) 0.0348(5) Uani 1 d . . H3A H 0.7901(3) 0.3221(3) 1.1967(3) 0.042 Uiso 1 calc R . C4 C 0.5144(3) 0.3493(3) 1.1129(3) 0.0340(5) Uani 1 d . . H4A H 0.5429(3) 0.4626(3) 1.2417(3) 0.041 Uiso 1 calc R . C5 C 0.3260(3) 0.2653(3) 0.9480(3) 0.0283(5) Uani 1 d . . C6 C 0.3618(3) -0.1664(4) 0.5277(3) 0.0344(5) Uani 1 d . . H6A H 0.4750(3) -0.2127(4) 0.5267(3) 0.052 Uiso 1 d R . H6B H 0.3073(3) -0.1376(4) 0.4160(3) 0.052 Uiso 1 d R . H6C H 0.2635(3) -0.2683(4) 0.5057(3) 0.052 Uiso 1 d R . C7 C 0.1602(3) 0.3465(4) 0.9692(4) 0.0403(6) Uani 1 d . . H7A H 0.2105(3) 0.4664(4) 1.1063(4) 0.060 Uiso 1 d R . H7B H 0.0639(3) 0.2485(4) 0.9550(4) 0.060 Uiso 1 d R . H7C H 0.0990(3) 0.3773(4) 0.8601(4) 0.060 Uiso 1 d 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 0.0177(3) 0.0270(3) 0.0215(3) 0.0106(2) 0.0075(2) 0.0057(2) Cl 0.0259(3) 0.0406(4) 0.0368(3) 0.0231(3) 0.0116(2) 0.0062(2) N 0.0216(8) 0.0270(9) 0.0251(8) 0.0142(7) 0.0099(7) 0.0059(7) C1 0.0247(10) 0.0337(11) 0.0289(10) 0.0197(9) 0.0146(8) 0.0087(8) C2 0.0231(10) 0.0422(12) 0.0370(11) 0.0267(10) 0.0142(9) 0.0102(9) C3 0.0230(10) 0.0416(13) 0.0327(11) 0.0232(10) 0.0032(8) 0.0001(9) C4 0.0347(11) 0.0294(11) 0.0284(10) 0.0138(9) 0.0082(9) 0.0028(9) C5 0.0297(10) 0.0251(10) 0.0271(10) 0.0130(8) 0.0115(8) 0.0060(8) C6 0.0309(11) 0.0428(13) 0.0314(11) 0.0170(10) 0.0180(9) 0.0160(10) C7 0.0354(12) 0.0343(12) 0.0362(12) 0.0079(10) 0.0154(10) 0.0122(10) _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 N 2.117(2) 2_556 ? Cr N 2.117(2) . ? Cr Cl 2.3361(6) 2_556 ? Cr Cl 2.3361(6) . ? N C5 1.353(3) . ? N C1 1.353(3) . ? C1 C2 1.385(3) . ? C1 C6 1.498(3) . ? C2 C3 1.378(3) . ? C3 C4 1.382(3) . ? C4 C5 1.381(3) . ? C5 C7 1.501(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cr N 180.0 2_556 . ? N Cr Cl 89.62(5) 2_556 2_556 ? N Cr Cl 90.38(5) . 2_556 ? N Cr Cl 90.38(5) 2_556 . ? N Cr Cl 89.62(5) . . ? Cl Cr Cl 180.0 2_556 . ? C5 N C1 119.1(2) . . ? C5 N Cr 120.46(13) . . ? C1 N Cr 120.29(13) . . ? N C1 C2 121.2(2) . . ? N C1 C6 116.5(2) . . ? C2 C1 C6 122.3(2) . . ? C3 C2 C1 119.7(2) . . ? C2 C3 C4 119.0(2) . . ? C5 C4 C3 119.5(2) . . ? N C5 C4 121.6(2) . . ? N C5 C7 116.7(2) . . ? C4 C5 C7 121.8(2) . . ? _refine_diff_density_max 0.294 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.055 #===END data_Compound_3 _database_code_CSD 216350 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H48 N3 O3 Cr' _chemical_formula_weight 622.77 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 10.957(2) _cell_length_b 18.642(3) _cell_length_c 16.593(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.94(2) _cell_angle_gamma 90.00 _cell_volume 3388.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.70 _cell_measurement_theta_max 21.44 _exptl_crystal_description 'prismatic needles' _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method ? _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 3.069 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.2862 _exptl_absorpt_correction_T_max 0.8937 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5298 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0811 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 59.98 _reflns_number_total 5298 _reflns_number_observed 4237 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1880P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(12) _refine_ls_number_reflns 5298 _refine_ls_number_parameters 776 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_obs 0.0881 _refine_ls_wR_factor_all 0.2414 _refine_ls_wR_factor_obs 0.2169 _refine_ls_goodness_of_fit_all 1.031 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max 0.020 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.04644(15) 0.14525(8) 0.28047(10) 0.0219(4) Uani 1 d . . O1 O 0.1927(8) 0.1372(4) 0.2188(5) 0.030(2) Uani 1 d . . O2 O 0.0589(7) 0.0455(4) 0.3021(5) 0.027(2) Uani 1 d . . O3 O -0.0893(8) 0.1493(4) 0.3514(5) 0.029(2) Uani 1 d . . N1 N 0.0341(9) 0.2571(5) 0.2472(6) 0.027(2) Uani 1 d . . N2 N 0.1647(9) 0.1619(5) 0.3834(6) 0.028(2) Uani 1 d . . N3 N -0.0750(9) 0.1102(5) 0.1845(6) 0.032(2) Uani 1 d . . C1 C 0.1409(13) 0.2911(6) 0.2375(8) 0.038(3) Uani 1 d . . C2 C 0.1454(14) 0.3683(7) 0.2371(9) 0.047(4) Uani 1 d . . H2A H 0.2197(14) 0.3919(7) 0.2323(9) 0.056 Uiso 1 calc R . C3 C 0.0407(16) 0.4066(6) 0.2436(9) 0.050(4) Uani 1 d . . H3A H 0.0427(16) 0.4564(6) 0.2463(9) 0.060 Uiso 1 calc R . C4 C -0.0696(17) 0.3698(6) 0.2460(9) 0.050(4) Uani 1 d . . H4A H -0.1424(17) 0.3954(6) 0.2472(9) 0.060 Uiso 1 calc R . C5 C -0.0728(13) 0.2956(6) 0.2468(7) 0.035(3) Uani 1 d . . C6 C 0.2578(13) 0.2575(7) 0.2239(10) 0.046(3) Uani 1 d . . H6A H 0.3260(13) 0.2872(7) 0.2250(10) 0.055 Uiso 1 calc R . C7 C 0.2772(11) 0.1870(7) 0.2096(8) 0.033(3) Uani 1 d . . C8 C -0.1908(13) 0.2600(7) 0.2467(10) 0.045(3) Uani 1 d . . H8A H -0.2532(13) 0.2936(7) 0.2312(10) 0.068 Uiso 1 d R . H8B H -0.2072(13) 0.2417(7) 0.2995(10) 0.068 Uiso 1 d R . H8C H -0.1900(13) 0.2210(7) 0.2089(10) 0.068 Uiso 1 d R . C9 C 0.4018(14) 0.1590(8) 0.1785(9) 0.048(3) Uani 1 d . . C10 C 0.4380(36) 0.2014(20) 0.1061(23) 0.151(13) Uani 1 d U . H10A H 0.4431(36) 0.2513(20) 0.1200(23) 0.226 Uiso 1 calc R . H10B H 0.3782(36) 0.1949(20) 0.0638(23) 0.226 Uiso 1 calc R . H10C H 0.5161(36) 0.1851(20) 0.0880(23) 0.226 Uiso 1 calc R . C11 C 0.3937(26) 0.0808(14) 0.1563(20) 0.112(9) Uani 1 d U . H11A H 0.3704(26) 0.0535(14) 0.2027(20) 0.167 Uiso 1 calc R . H11B H 0.4717(26) 0.0645(14) 0.1382(20) 0.167 Uiso 1 calc R . H11C H 0.3339(26) 0.0745(14) 0.1140(20) 0.167 Uiso 1 calc R . C12 C 0.4919(32) 0.1617(20) 0.2477(24) 0.151(13) Uani 1 d U . H12A H 0.4622(32) 0.1334(20) 0.2916(24) 0.226 Uiso 1 calc R . H12B H 0.5022(32) 0.2105(20) 0.2651(24) 0.226 Uiso 1 calc R . H12C H 0.5690(32) 0.1430(20) 0.2308(24) 0.226 Uiso 1 calc R . C21 C 0.2546(11) 0.1108(6) 0.3980(7) 0.031(3) Uani 1 d . . C22 C 0.3514(13) 0.1254(8) 0.4522(9) 0.044(3) Uani 1 d . . H22A H 0.4148(13) 0.0926(8) 0.4581(9) 0.053 Uiso 1 calc R . C23 C 0.3533(15) 0.1882(9) 0.4969(10) 0.054(4) Uani 1 d . . H23A H 0.4192(15) 0.1992(9) 0.5308(10) 0.065 Uiso 1 calc R . C24 C 0.2532(15) 0.2346(9) 0.4895(9) 0.054(4) Uani 1 d . . H24A H 0.2476(15) 0.2749(9) 0.5223(9) 0.065 Uiso 1 calc R . C25 C 0.1645(13) 0.2201(7) 0.4339(7) 0.040(3) Uani 1 d . . C26 C 0.2510(11) 0.0427(6) 0.3606(8) 0.035(3) Uani 1 d . . H26A H 0.3225(11) 0.0159(6) 0.3643(8) 0.042 Uiso 1 calc R . C27 C 0.1569(11) 0.0113(6) 0.3199(7) 0.030(2) Uani 1 d . . C28 C 0.0581(15) 0.2724(7) 0.4304(8) 0.046(3) Uani 1 d . . H28A H -0.0164(15) 0.2472(7) 0.4182(8) 0.069 Uiso 1 d R . H28B H 0.0726(15) 0.3074(7) 0.3893(8) 0.069 Uiso 1 d R . H28C H 0.0515(15) 0.2959(7) 0.4816(8) 0.069 Uiso 1 d R . C29 C 0.1547(13) -0.0680(6) 0.2930(8) 0.041(3) Uani 1 d . . C30 C 0.2755(15) -0.1057(7) 0.3025(14) 0.068(5) Uani 1 d . . H30A H 0.3012(15) -0.1045(7) 0.3581(14) 0.102 Uiso 1 calc R . H30B H 0.3353(15) -0.0819(7) 0.2703(14) 0.102 Uiso 1 calc R . H30C H 0.2672(15) -0.1546(7) 0.2852(14) 0.102 Uiso 1 calc R . C31 C 0.1157(23) -0.0706(9) 0.2040(11) 0.078(6) Uani 1 d . . H31A H 0.0386(23) -0.0467(9) 0.1970(11) 0.116 Uiso 1 calc R . H31B H 0.1080(23) -0.1197(9) 0.1871(11) 0.116 Uiso 1 calc R . H31C H 0.1760(23) -0.0470(9) 0.1721(11) 0.116 Uiso 1 calc R . C32 C 0.0552(18) -0.1062(8) 0.3429(15) 0.078(6) Uani 1 d . . H32A H -0.0211(18) -0.0815(8) 0.3360(15) 0.117 Uiso 1 calc R . H32B H 0.0788(18) -0.1060(8) 0.3989(15) 0.117 Uiso 1 calc R . H32C H 0.0463(18) -0.1549(8) 0.3246(15) 0.117 Uiso 1 calc R . C41 C -0.1699(11) 0.0694(6) 0.2091(8) 0.036(3) Uani 1 d . . C42 C -0.2440(16) 0.0330(8) 0.1476(9) 0.053(4) Uani 1 d . . H42A H -0.3095(16) 0.0046(8) 0.1627(9) 0.063 Uiso 1 calc R . C43 C -0.2169(16) 0.0406(9) 0.0672(10) 0.060(4) Uani 1 d . . H43A H -0.2628(16) 0.0167(9) 0.0279(10) 0.072 Uiso 1 calc R . C44 C -0.1248(16) 0.0824(9) 0.0468(10) 0.057(4) Uani 1 d . . H44A H -0.1082(16) 0.0882(9) -0.0076(10) 0.068 Uiso 1 calc R . C45 C -0.0514(14) 0.1180(6) 0.1034(8) 0.041(3) Uani 1 d . . C46 C -0.2094(11) 0.0614(6) 0.2884(8) 0.033(2) Uani 1 d . . H46A H -0.2689(11) 0.0268(6) 0.2968(8) 0.039 Uiso 1 calc R . C47 C -0.1702(11) 0.0989(6) 0.3549(7) 0.030(3) Uani 1 d . . C48 C 0.0486(15) 0.1648(8) 0.0753(8) 0.050(4) Uani 1 d . . H48A H 0.1242(15) 0.1389(8) 0.0789(8) 0.074 Uiso 1 d R . H48B H 0.0534(15) 0.2066(8) 0.1090(8) 0.074 Uiso 1 d R . H48C H 0.0335(15) 0.1791(8) 0.0205(8) 0.074 Uiso 1 d R . C49 C -0.2232(13) 0.0868(7) 0.4391(8) 0.042(3) Uani 1 d . . C50 C -0.3144(18) 0.0239(9) 0.4429(11) 0.069(5) Uani 1 d . . H50A H -0.3831(18) 0.0337(9) 0.4079(11) 0.103 Uiso 1 calc R . H50B H -0.3417(18) 0.0183(9) 0.4972(11) 0.103 Uiso 1 calc R . H50C H -0.2751(18) -0.0194(9) 0.4258(11) 0.103 Uiso 1 calc R . C51 C -0.2887(20) 0.1559(9) 0.4630(12) 0.076(6) Uani 1 d . . H51A H -0.3560(20) 0.1643(9) 0.4265(12) 0.113 Uiso 1 calc R . H51B H -0.2327(20) 0.1954(9) 0.4606(12) 0.113 Uiso 1 calc R . H51C H -0.3184(20) 0.1512(9) 0.5168(12) 0.113 Uiso 1 calc R . C52 C -0.1147(22) 0.0702(13) 0.4950(11) 0.086(7) Uani 1 d . . H52A H -0.0763(22) 0.0266(13) 0.4779(11) 0.130 Uiso 1 calc R . H52B H -0.1426(22) 0.0647(13) 0.5492(11) 0.130 Uiso 1 calc R . H52C H -0.0570(22) 0.1089(13) 0.4930(11) 0.130 Uiso 1 calc R . Cr' Cr 0.52107(15) 0.59721(9) 0.30496(10) 0.0223(4) Uani 1 d . . O1' O 0.3773(8) 0.5835(4) 0.2371(5) 0.031(2) Uani 1 d . . O2' O 0.5334(7) 0.6921(4) 0.2636(5) 0.030(2) Uani 1 d . . O3' O 0.6747(8) 0.6130(4) 0.3627(5) 0.034(2) Uani 1 d . . N1' N 0.4068(9) 0.6473(5) 0.3940(5) 0.028(2) Uani 1 d . . N2' N 0.6249(9) 0.5611(5) 0.2044(5) 0.027(2) Uani 1 d . . N3' N 0.5118(9) 0.4930(5) 0.3614(5) 0.028(2) Uani 1 d . . C1' C 0.3105(11) 0.6829(6) 0.3677(7) 0.028(2) Uani 1 d . . C2' C 0.2364(14) 0.7245(7) 0.4202(9) 0.047(3) Uani 1 d . . H2'A H 0.1700(14) 0.7502(7) 0.3998(9) 0.057 Uiso 1 calc R . C3' C 0.2643(15) 0.7263(8) 0.5013(9) 0.056(4) Uani 1 d . . H3'A H 0.2185(15) 0.7540(8) 0.5362(9) 0.067 Uiso 1 calc R . C4' C 0.3634(14) 0.6855(8) 0.5303(8) 0.049(4) Uani 1 d . . H4'A H 0.3812(14) 0.6835(8) 0.5852(8) 0.058 Uiso 1 calc R . C5' C 0.4348(12) 0.6480(6) 0.4756(7) 0.032(3) Uani 1 d . . C6' C 0.2649(11) 0.6820(6) 0.2839(7) 0.030(2) Uani 1 d . . H6'A H 0.2092(11) 0.7174(6) 0.2687(7) 0.036 Uiso 1 calc R . C7' C 0.2973(10) 0.6339(6) 0.2274(6) 0.026(2) Uani 1 d . . C8' C 0.5435(15) 0.6092(9) 0.5105(8) 0.051(4) Uani 1 d . . H8'1 H 0.5302(15) 0.5990(9) 0.5664(8) 0.076 Uiso 1 d R . H8'2 H 0.6144(15) 0.6391(9) 0.5056(8) 0.076 Uiso 1 d R . H8'3 H 0.5558(15) 0.5652(9) 0.4818(8) 0.076 Uiso 1 d R . C9' C 0.2412(13) 0.6355(7) 0.1407(7) 0.035(3) Uani 1 d . . C10' C 0.1853(17) 0.5636(9) 0.1224(10) 0.059(4) Uani 1 d . . H10D H 0.1191(17) 0.5550(9) 0.1583(10) 0.088 Uiso 1 calc R . H10E H 0.2459(17) 0.5268(9) 0.1295(10) 0.088 Uiso 1 calc R . H10F H 0.1553(17) 0.5630(9) 0.0677(10) 0.088 Uiso 1 calc R . C11' C 0.3467(16) 0.6492(10) 0.0835(8) 0.060(4) Uani 1 d . . H11D H 0.3823(16) 0.6952(10) 0.0952(8) 0.090 Uiso 1 calc R . H11E H 0.3166(16) 0.6486(10) 0.0288(8) 0.090 Uiso 1 calc R . H11F H 0.4073(16) 0.6125(10) 0.0906(8) 0.090 Uiso 1 calc R . C12' C 0.1450(17) 0.6949(8) 0.1296(11) 0.062(4) Uani 1 d . . H12D H 0.1814(17) 0.7407(8) 0.1414(11) 0.093 Uiso 1 calc R . H12E H 0.0787(17) 0.6866(8) 0.1655(11) 0.093 Uiso 1 calc R . H12F H 0.1148(17) 0.6947(8) 0.0750(11) 0.093 Uiso 1 calc R . C21' C 0.7156(12) 0.6064(7) 0.1793(8) 0.036(3) Uani 1 d . . C22' C 0.8056(14) 0.5819(8) 0.1261(8) 0.048(4) Uani 1 d . . H22B H 0.8690(14) 0.6122(8) 0.1116(8) 0.057 Uiso 1 calc R . C23' C 0.7999(14) 0.5134(9) 0.0956(10) 0.054(4) Uani 1 d . . H23B H 0.8600(14) 0.4965(9) 0.0615(10) 0.064 Uiso 1 calc R . C24' C 0.7028(16) 0.4701(8) 0.1167(9) 0.054(4) Uani 1 d . . H24B H 0.6959(16) 0.4242(8) 0.0953(9) 0.065 Uiso 1 calc R . C25' C 0.6153(12) 0.4951(6) 0.1698(7) 0.035(3) Uani 1 d . . C26' C 0.7221(12) 0.6818(7) 0.1997(7) 0.036(3) Uani 1 d . . H26B H 0.7929(12) 0.7061(7) 0.1859(7) 0.043 Uiso 1 calc R . C27' C 0.6340(11) 0.7205(6) 0.2372(8) 0.032(3) Uani 1 d . . C28' C 0.5089(15) 0.4474(7) 0.1866(9) 0.048(3) Uani 1 d . . H28D H 0.5113(15) 0.4329(7) 0.2421(9) 0.072 Uiso 1 d R . H28E H 0.5130(15) 0.4058(7) 0.1527(9) 0.072 Uiso 1 d R . H28F H 0.4342(15) 0.4728(7) 0.1754(9) 0.072 Uiso 1 d R . C29' C 0.6417(14) 0.8019(7) 0.2465(10) 0.048(4) Uani 1 d . . C30' C 0.5476(18) 0.8342(8) 0.1871(13) 0.068(5) Uani 1 d . . H30D H 0.5692(18) 0.8220(8) 0.1330(13) 0.102 Uiso 1 calc R . H30E H 0.5467(18) 0.8854(8) 0.1930(13) 0.102 Uiso 1 calc R . H30F H 0.4681(18) 0.8154(8) 0.1984(13) 0.102 Uiso 1 calc R . C31' C 0.6066(22) 0.8215(9) 0.3321(11) 0.073(5) Uani 1 d . . H31D H 0.6111(22) 0.8726(9) 0.3388(11) 0.109 Uiso 1 calc R . H31E H 0.6618(22) 0.7987(9) 0.3696(11) 0.109 Uiso 1 calc R . H31F H 0.5249(22) 0.8056(9) 0.3418(11) 0.109 Uiso 1 calc R . C32' C 0.7703(17) 0.8325(9) 0.2308(14) 0.075(6) Uani 1 d . . H32D H 0.7940(17) 0.8206(9) 0.1769(14) 0.112 Uiso 1 calc R . H32E H 0.8278(17) 0.8122(9) 0.2686(14) 0.112 Uiso 1 calc R . H32F H 0.7689(17) 0.8837(9) 0.2369(14) 0.112 Uiso 1 calc R . C41' C 0.6168(13) 0.4592(7) 0.3733(7) 0.040(3) Uani 1 d . . C42' C 0.6211(16) 0.3831(8) 0.3884(8) 0.052(4) Uani 1 d . . H42B H 0.6952(16) 0.3593(8) 0.3945(8) 0.062 Uiso 1 calc R . C43' C 0.5105(18) 0.3460(7) 0.3938(10) 0.058(4) Uani 1 d . . H43B H 0.5095(18) 0.2965(7) 0.4004(10) 0.070 Uiso 1 calc R . C44' C 0.4033(16) 0.3842(7) 0.3890(10) 0.052(4) Uani 1 d . . H44B H 0.3295(16) 0.3607(7) 0.3965(10) 0.063 Uiso 1 calc R . C45' C 0.4034(12) 0.4558(6) 0.3736(8) 0.036(3) Uani 1 d . . C46' C 0.7331(13) 0.4930(7) 0.3787(7) 0.040(3) Uani 1 d . . H46B H 0.8002(13) 0.4625(7) 0.3810(7) 0.048 Uiso 1 calc R . C47' C 0.7585(13) 0.5641(8) 0.3810(8) 0.040(3) Uani 1 d . . C48' C 0.2846(13) 0.4952(7) 0.3731(10) 0.048(3) Uani 1 d . . H48D H 0.2802(13) 0.5250(7) 0.3260(10) 0.071 Uiso 1 d R . H48E H 0.2790(13) 0.5246(7) 0.4205(10) 0.071 Uiso 1 d R . H48F H 0.2184(13) 0.4615(7) 0.3718(10) 0.071 Uiso 1 d R . C49' C 0.8840(13) 0.5934(10) 0.4039(9) 0.055(4) Uani 1 d . . C50' C 0.9611(22) 0.5350(14) 0.4422(17) 0.101(7) Uani 1 d U . H50D H 0.9684(22) 0.4957(14) 0.4052(17) 0.151 Uiso 1 calc R . H50E H 0.9232(22) 0.5186(14) 0.4906(17) 0.151 Uiso 1 calc R . H50F H 1.0408(22) 0.5536(14) 0.4551(17) 0.151 Uiso 1 calc R . C51' C 0.8707(21) 0.6537(13) 0.4589(17) 0.098(7) Uani 1 d U . H51D H 0.8263(21) 0.6386(13) 0.5053(17) 0.147 Uiso 1 calc R . H51E H 0.8271(21) 0.6917(13) 0.4321(17) 0.147 Uiso 1 calc R . H51F H 0.9500(21) 0.6705(13) 0.4755(17) 0.147 Uiso 1 calc R . C52' C 0.9526(19) 0.6109(13) 0.3286(15) 0.088(6) Uani 1 d U . H52D H 0.9579(19) 0.5688(13) 0.2955(15) 0.133 Uiso 1 calc R . H52E H 1.0333(19) 0.6271(13) 0.3428(15) 0.133 Uiso 1 calc R . H52F H 0.9103(19) 0.6480(13) 0.2993(15) 0.133 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0209(10) 0.0165(8) 0.0286(8) 0.0006(6) 0.0079(7) 0.0035(7) O1 0.036(5) 0.027(4) 0.028(4) -0.002(3) 0.012(4) 0.005(3) O2 0.025(4) 0.019(3) 0.038(4) 0.005(3) 0.004(4) 0.002(3) O3 0.027(5) 0.020(4) 0.040(4) -0.004(3) 0.010(4) -0.004(3) N1 0.026(5) 0.025(4) 0.030(4) 0.001(4) -0.002(4) 0.002(4) N2 0.029(5) 0.023(4) 0.031(5) 0.001(4) 0.008(4) -0.004(4) N3 0.026(5) 0.024(4) 0.046(6) -0.006(4) 0.000(5) 0.016(4) C1 0.045(8) 0.025(6) 0.045(7) -0.008(5) 0.010(6) -0.006(5) C2 0.058(10) 0.029(6) 0.055(8) -0.001(5) 0.024(7) -0.017(6) C3 0.077(11) 0.024(6) 0.050(7) -0.016(5) 0.014(7) 0.005(7) C4 0.082(12) 0.019(6) 0.050(7) 0.000(5) 0.019(7) 0.016(7) C5 0.047(8) 0.030(6) 0.029(5) 0.001(4) 0.012(5) 0.017(5) C6 0.034(8) 0.033(7) 0.071(9) 0.000(6) 0.024(7) -0.017(6) C7 0.022(6) 0.032(6) 0.044(6) -0.001(5) 0.009(5) 0.004(5) C8 0.035(7) 0.032(6) 0.069(9) 0.006(6) 0.003(7) 0.015(5) C9 0.040(8) 0.051(8) 0.052(8) 0.006(6) 0.016(7) 0.008(6) C10 0.152(18) 0.158(17) 0.143(17) 0.027(13) 0.043(14) 0.020(14) C11 0.103(14) 0.096(12) 0.137(15) -0.030(11) 0.038(12) 0.016(11) C12 0.117(17) 0.177(18) 0.158(18) -0.014(14) -0.005(14) 0.032(14) C21 0.024(6) 0.035(6) 0.035(6) 0.009(5) -0.003(5) -0.010(5) C22 0.035(8) 0.044(7) 0.054(8) -0.002(6) -0.013(6) 0.000(6) C23 0.042(9) 0.060(9) 0.060(9) -0.009(7) -0.018(7) -0.014(7) C24 0.055(10) 0.063(9) 0.044(7) -0.016(6) 0.002(7) -0.027(8) C25 0.044(8) 0.040(6) 0.035(6) 0.000(5) 0.011(6) -0.011(6) C26 0.024(7) 0.032(6) 0.048(7) 0.011(5) -0.005(5) 0.011(5) C27 0.031(7) 0.024(5) 0.035(6) 0.004(4) 0.008(5) 0.006(5) C28 0.062(10) 0.040(7) 0.036(6) -0.018(5) 0.015(6) 0.011(6) C29 0.046(8) 0.027(6) 0.051(7) -0.006(5) 0.010(6) 0.004(5) C30 0.050(10) 0.027(7) 0.128(16) -0.002(8) 0.007(10) 0.017(7) C31 0.121(19) 0.041(8) 0.070(11) -0.023(7) -0.019(11) 0.022(10) C32 0.076(13) 0.023(7) 0.137(19) 0.003(8) 0.019(13) -0.009(7) C41 0.018(6) 0.031(6) 0.058(8) -0.012(5) -0.001(6) 0.007(5) C42 0.061(10) 0.046(7) 0.052(8) -0.025(6) -0.001(7) -0.004(7) C43 0.055(10) 0.063(10) 0.063(10) -0.019(7) -0.009(8) -0.005(8) C44 0.064(11) 0.061(9) 0.046(7) -0.013(7) -0.006(7) 0.006(8) C45 0.054(9) 0.028(6) 0.040(6) -0.014(5) 0.012(6) 0.011(6) C46 0.018(6) 0.033(6) 0.048(7) -0.004(5) 0.000(5) -0.001(5) C47 0.027(6) 0.027(5) 0.037(6) -0.010(5) 0.018(5) -0.004(5) C48 0.057(10) 0.062(9) 0.030(6) 0.004(6) 0.011(6) 0.004(7) C49 0.040(8) 0.042(7) 0.044(7) 0.010(5) 0.025(6) -0.009(6) C50 0.079(13) 0.059(9) 0.070(10) -0.001(8) 0.046(10) -0.032(9) C51 0.092(15) 0.064(10) 0.073(11) -0.026(9) 0.059(11) -0.001(10) C52 0.099(17) 0.104(16) 0.056(10) 0.027(10) 0.026(11) -0.001(13) Cr' 0.0197(10) 0.0211(8) 0.0262(8) -0.0021(6) 0.0078(7) -0.0024(7) O1' 0.024(5) 0.026(4) 0.044(4) -0.004(3) -0.002(4) -0.002(3) O2' 0.020(4) 0.031(4) 0.040(4) 0.001(3) 0.012(4) 0.002(3) O3' 0.023(5) 0.038(4) 0.042(5) -0.010(4) 0.013(4) -0.010(3) N1' 0.032(6) 0.026(5) 0.026(5) -0.002(3) 0.011(4) -0.005(4) N2' 0.025(5) 0.030(5) 0.026(4) -0.004(3) 0.000(4) 0.002(4) N3' 0.033(6) 0.027(5) 0.024(4) -0.005(3) 0.002(4) -0.001(4) C1' 0.027(6) 0.031(6) 0.026(5) -0.004(4) 0.006(5) -0.005(5) C2' 0.049(9) 0.046(7) 0.048(7) -0.002(6) 0.029(7) 0.011(6) C3' 0.056(10) 0.057(9) 0.054(8) -0.015(7) 0.032(8) 0.016(7) C4' 0.056(9) 0.053(8) 0.038(7) -0.024(6) 0.031(7) -0.012(7) C5' 0.040(7) 0.032(6) 0.025(5) -0.002(4) 0.018(5) -0.005(5) C6' 0.024(6) 0.027(5) 0.039(6) 0.004(5) 0.004(5) 0.002(4) C7' 0.025(6) 0.033(6) 0.020(5) 0.003(4) -0.002(4) -0.003(5) C8' 0.051(9) 0.075(10) 0.028(6) -0.014(6) 0.005(6) -0.006(7) C9' 0.035(7) 0.044(7) 0.027(6) 0.011(5) -0.004(5) -0.004(6) C10' 0.066(11) 0.056(9) 0.053(8) 0.013(7) -0.019(8) -0.027(8) C11' 0.056(10) 0.093(12) 0.031(6) 0.012(7) 0.011(7) -0.008(9) C12' 0.063(11) 0.053(9) 0.069(10) 0.007(7) -0.028(9) 0.012(8) C21' 0.026(7) 0.046(7) 0.036(6) 0.006(5) 0.009(5) 0.001(5) C22' 0.041(8) 0.065(9) 0.039(7) 0.005(6) 0.036(6) 0.014(7) C23' 0.033(8) 0.068(9) 0.061(9) -0.009(7) 0.028(7) 0.020(7) C24' 0.066(11) 0.045(7) 0.051(8) -0.010(6) 0.015(7) 0.029(7) C25' 0.040(8) 0.040(6) 0.024(5) -0.001(5) -0.008(5) 0.008(5) C26' 0.031(7) 0.044(7) 0.033(6) 0.007(5) 0.012(5) -0.014(6) C27' 0.025(6) 0.026(5) 0.045(6) 0.004(5) 0.014(5) 0.001(5) C28' 0.064(10) 0.032(6) 0.048(7) -0.020(5) -0.008(7) -0.002(6) C29' 0.046(9) 0.033(6) 0.064(8) -0.007(6) 0.026(7) -0.017(6) C30' 0.073(12) 0.037(7) 0.093(13) 0.020(8) -0.003(10) 0.009(8) C31' 0.105(15) 0.045(9) 0.069(10) -0.022(8) 0.014(11) -0.006(10) C32' 0.057(11) 0.054(9) 0.113(16) 0.005(10) 0.014(11) -0.025(8) C41' 0.049(8) 0.048(7) 0.023(5) -0.011(5) 0.004(5) 0.008(6) C42' 0.072(11) 0.041(7) 0.043(7) 0.002(5) 0.000(7) 0.026(7) C43' 0.084(12) 0.023(6) 0.067(9) 0.005(6) -0.005(9) -0.006(7) C44' 0.062(10) 0.028(7) 0.068(9) 0.008(6) 0.006(8) 0.000(6) C45' 0.034(7) 0.031(6) 0.041(6) 0.007(5) 0.007(5) -0.010(5) C46' 0.035(7) 0.052(8) 0.033(6) -0.011(5) 0.000(5) 0.011(6) C47' 0.034(8) 0.051(8) 0.036(6) 0.005(5) 0.014(5) 0.002(6) C48' 0.030(7) 0.042(7) 0.071(9) 0.001(6) 0.007(7) -0.014(6) C49' 0.028(8) 0.098(13) 0.040(7) -0.010(7) 0.001(6) -0.005(8) C50' 0.076(12) 0.110(13) 0.115(13) -0.001(11) -0.012(11) -0.013(10) C51' 0.069(11) 0.108(12) 0.117(13) -0.053(11) -0.022(10) -0.022(10) C52' 0.061(11) 0.107(12) 0.098(12) 0.003(10) 0.012(10) -0.029(9) _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 O2 1.899(7) . ? Cr O3 1.914(8) . ? Cr O1 1.921(8) . ? Cr N2 2.149(10) . ? Cr N3 2.160(11) . ? Cr N1 2.161(9) . ? O1 C7 1.322(15) . ? O2 C27 1.279(15) . ? O3 C47 1.294(14) . ? N1 C1 1.34(2) . ? N1 C5 1.37(2) . ? N2 C25 1.37(2) . ? N2 C21 1.39(2) . ? N3 C41 1.36(2) . ? N3 C45 1.38(2) . ? C1 C2 1.44(2) . ? C1 C6 1.45(2) . ? C2 C3 1.36(2) . ? C3 C4 1.39(2) . ? C4 C5 1.38(2) . ? C5 C8 1.45(2) . ? C6 C7 1.35(2) . ? C7 C9 1.56(2) . ? C9 C10 1.50(3) . ? C9 C11 1.51(3) . ? C9 C12 1.50(4) . ? C21 C22 1.41(2) . ? C21 C26 1.41(2) . ? C22 C23 1.39(2) . ? C23 C24 1.40(2) . ? C24 C25 1.36(2) . ? C25 C28 1.52(2) . ? C26 C27 1.36(2) . ? C27 C29 1.54(2) . ? C29 C30 1.50(2) . ? C29 C31 1.53(2) . ? C29 C32 1.55(2) . ? C41 C46 1.40(2) . ? C41 C42 1.46(2) . ? C42 C43 1.38(2) . ? C43 C44 1.32(2) . ? C44 C45 1.39(2) . ? C45 C48 1.48(2) . ? C46 C47 1.37(2) . ? C47 C49 1.54(2) . ? C49 C52 1.53(3) . ? C49 C51 1.53(2) . ? C49 C50 1.54(2) . ? Cr' O2' 1.904(8) . ? Cr' O1' 1.937(9) . ? Cr' O3' 1.945(9) . ? Cr' N2' 2.144(9) . ? Cr' N3' 2.160(10) . ? Cr' N1' 2.164(9) . ? O1' C7' 1.294(14) . ? O2' C27' 1.305(15) . ? O3' C47' 1.33(2) . ? N1' C1' 1.32(2) . ? N1' C5' 1.38(2) . ? N2' C25' 1.36(2) . ? N2' C21' 1.37(2) . ? N3' C41' 1.32(2) . ? N3' C45' 1.39(2) . ? C1' C2' 1.43(2) . ? C1' C6' 1.47(2) . ? C2' C3' 1.37(2) . ? C3' C4' 1.40(2) . ? C4' C5' 1.40(2) . ? C5' C8' 1.50(2) . ? C6' C7' 1.35(2) . ? C7' C9' 1.556(15) . ? C9' C10' 1.50(2) . ? C9' C11' 1.53(2) . ? C9' C12' 1.54(2) . ? C21' C22' 1.41(2) . ? C21' C26' 1.45(2) . ? C22' C23' 1.38(2) . ? C23' C24' 1.38(2) . ? C24' C25' 1.39(2) . ? C25' C28' 1.50(2) . ? C26' C27' 1.36(2) . ? C27' C29' 1.53(2) . ? C29' C31' 1.52(2) . ? C29' C30' 1.54(2) . ? C29' C32' 1.55(2) . ? C41' C46' 1.42(2) . ? C41' C42' 1.44(2) . ? C42' C43' 1.40(3) . ? C43' C44' 1.38(2) . ? C44' C45' 1.36(2) . ? C45' C48' 1.50(2) . ? C46' C47' 1.35(2) . ? C47' C49' 1.52(2) . ? C49' C51' 1.46(3) . ? C49' C52' 1.51(3) . ? C49' C50' 1.51(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cr O3 88.7(3) . . ? O2 Cr O1 88.0(3) . . ? O3 Cr O1 173.9(4) . . ? O2 Cr N2 87.1(4) . . ? O3 Cr N2 88.3(4) . . ? O1 Cr N2 86.4(4) . . ? O2 Cr N3 83.4(4) . . ? O3 Cr N3 89.4(4) . . ? O1 Cr N3 95.3(4) . . ? N2 Cr N3 170.3(4) . . ? O2 Cr N1 176.1(4) . . ? O3 Cr N1 94.2(3) . . ? O1 Cr N1 89.4(3) . . ? N2 Cr N1 95.6(4) . . ? N3 Cr N1 93.9(4) . . ? C7 O1 Cr 126.8(7) . . ? C27 O2 Cr 126.1(7) . . ? C47 O3 Cr 122.6(7) . . ? C1 N1 C5 119.8(10) . . ? C1 N1 Cr 115.8(8) . . ? C5 N1 Cr 123.7(8) . . ? C25 N2 C21 116.4(11) . . ? C25 N2 Cr 126.4(9) . . ? C21 N2 Cr 117.1(8) . . ? C41 N3 C45 120.6(12) . . ? C41 N3 Cr 114.4(9) . . ? C45 N3 Cr 124.3(9) . . ? N1 C1 C2 120.2(12) . . ? N1 C1 C6 126.1(10) . . ? C2 C1 C6 113.7(12) . . ? C3 C2 C1 119.7(13) . . ? C2 C3 C4 118.6(11) . . ? C5 C4 C3 121.0(14) . . ? N1 C5 C4 120.0(13) . . ? N1 C5 C8 121.4(10) . . ? C4 C5 C8 118.7(12) . . ? C7 C6 C1 126.2(12) . . ? O1 C7 C6 123.3(11) . . ? O1 C7 C9 115.0(10) . . ? C6 C7 C9 121.6(11) . . ? C10 C9 C11 109.3(22) . . ? C10 C9 C12 114.6(24) . . ? C11 C9 C12 104.7(20) . . ? C10 C9 C7 109.6(18) . . ? C11 C9 C7 110.9(15) . . ? C12 C9 C7 107.7(17) . . ? N2 C21 C22 120.2(11) . . ? N2 C21 C26 121.7(11) . . ? C22 C21 C26 118.1(12) . . ? C23 C22 C21 120.8(13) . . ? C22 C23 C24 118.0(13) . . ? C25 C24 C23 119.2(14) . . ? C24 C25 N2 124.4(14) . . ? C24 C25 C28 116.0(13) . . ? N2 C25 C28 119.5(12) . . ? C27 C26 C21 128.4(11) . . ? O2 C27 C26 121.9(10) . . ? O2 C27 C29 113.7(11) . . ? C26 C27 C29 124.4(11) . . ? C30 C29 C31 108.5(14) . . ? C30 C29 C27 114.0(12) . . ? C31 C29 C27 108.2(11) . . ? C30 C29 C32 110.7(13) . . ? C31 C29 C32 108.2(16) . . ? C27 C29 C32 107.0(11) . . ? N3 C41 C46 126.4(12) . . ? N3 C41 C42 118.0(13) . . ? C46 C41 C42 115.5(12) . . ? C43 C42 C41 120.2(15) . . ? C44 C43 C42 119.1(15) . . ? C43 C44 C45 122.8(16) . . ? N3 C45 C44 119.4(13) . . ? N3 C45 C48 121.2(12) . . ? C44 C45 C48 119.3(13) . . ? C47 C46 C41 127.2(11) . . ? O3 C47 C46 122.8(11) . . ? O3 C47 C49 114.6(10) . . ? C46 C47 C49 122.6(11) . . ? C52 C49 C51 112.1(16) . . ? C52 C49 C47 106.2(12) . . ? C51 C49 C47 107.3(11) . . ? C52 C49 C50 108.7(14) . . ? C51 C49 C50 108.8(13) . . ? C47 C49 C50 113.7(12) . . ? O2' Cr' O1' 88.6(4) . . ? O2' Cr' O3' 88.3(4) . . ? O1' Cr' O3' 173.9(4) . . ? O2' Cr' N2' 88.2(3) . . ? O1' Cr' N2' 86.7(4) . . ? O3' Cr' N2' 88.0(3) . . ? O2' Cr' N3' 175.3(4) . . ? O1' Cr' N3' 95.2(4) . . ? O3' Cr' N3' 88.2(4) . . ? N2' Cr' N3' 94.9(3) . . ? O2' Cr' N1' 83.7(3) . . ? O1' Cr' N1' 88.8(4) . . ? O3' Cr' N1' 96.0(4) . . ? N2' Cr' N1' 170.9(4) . . ? N3' Cr' N1' 93.4(3) . . ? C7' O1' Cr' 121.3(7) . . ? C27' O2' Cr' 124.3(7) . . ? C47' O3' Cr' 126.8(8) . . ? C1' N1' C5' 119.0(10) . . ? C1' N1' Cr' 117.4(7) . . ? C5' N1' Cr' 123.4(8) . . ? C25' N2' C21' 118.6(10) . . ? C25' N2' Cr' 125.0(8) . . ? C21' N2' Cr' 116.0(8) . . ? C41' N3' C45' 118.8(10) . . ? C41' N3' Cr' 116.5(9) . . ? C45' N3' Cr' 123.9(8) . . ? N1' C1' C2' 122.1(11) . . ? N1' C1' C6' 124.6(10) . . ? C2' C1' C6' 113.3(11) . . ? C3' C2' C1' 119.4(14) . . ? C2' C3' C4' 118.7(12) . . ? C5' C4' C3' 119.1(13) . . ? N1' C5' C4' 121.6(13) . . ? N1' C5' C8' 122.4(10) . . ? C4' C5' C8' 116.0(12) . . ? C7' C6' C1' 125.1(10) . . ? O1' C7' C6' 125.5(10) . . ? O1' C7' C9' 112.7(10) . . ? C6' C7' C9' 121.7(11) . . ? C10' C9' C11' 109.5(13) . . ? C10' C9' C12' 110.0(13) . . ? C11' C9' C12' 109.2(12) . . ? C10' C9' C7' 108.9(10) . . ? C11' C9' C7' 106.6(11) . . ? C12' C9' C7' 112.5(11) . . ? N2' C21' C22' 120.5(12) . . ? N2' C21' C26' 124.0(11) . . ? C22' C21' C26' 115.4(12) . . ? C23' C22' C21' 120.2(13) . . ? C22' C23' C24' 118.6(11) . . ? C23' C24' C25' 120.3(13) . . ? N2' C25' C24' 121.3(13) . . ? N2' C25' C28' 120.9(11) . . ? C24' C25' C28' 117.7(12) . . ? C27' C26' C21' 126.0(11) . . ? O2' C27' C26' 123.2(10) . . ? O2' C27' C29' 114.5(10) . . ? C26' C27' C29' 122.2(11) . . ? C31' C29' C27' 108.6(12) . . ? C31' C29' C30' 109.1(15) . . ? C27' C29' C30' 106.8(13) . . ? C31' C29' C32' 108.3(16) . . ? C27' C29' C32' 113.5(13) . . ? C30' C29' C32' 110.5(14) . . ? N3' C41' C46' 125.0(12) . . ? N3' C41' C42' 121.3(14) . . ? C46' C41' C42' 113.5(13) . . ? C43' C42' C41' 118.2(14) . . ? C44' C43' C42' 118.7(12) . . ? C45' C44' C43' 121.1(15) . . ? C44' C45' N3' 121.4(13) . . ? C44' C45' C48' 118.7(12) . . ? N3' C45' C48' 119.9(10) . . ? C47' C46' C41' 128.2(12) . . ? O3' C47' C46' 121.7(13) . . ? O3' C47' C49' 115.4(13) . . ? C46' C47' C49' 122.9(14) . . ? C51' C49' C52' 114.2(19) . . ? C51' C49' C50' 110.7(18) . . ? C52' C49' C50' 102.8(17) . . ? C51' C49' C47' 109.6(14) . . ? C52' C49' C47' 109.3(13) . . ? C50' C49' C47' 110.0(16) . . ? _refine_diff_density_max 0.994 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.111 #===END data_Compound_6 _database_code_CSD 216351 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H48 N3 O3 Cr' _chemical_formula_weight 622.77 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.419(2) _cell_length_b 19.285(4) _cell_length_c 16.146(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.642(14) _cell_angle_gamma 90.00 _cell_volume 3524.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 11.13 _cell_measurement_theta_max 27.98 _exptl_crystal_description 'platy prisms' _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method ? _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 2.951 _exptl_absorpt_correction_type 'Face-indexed numerical' _exptl_absorpt_correction_T_min 0.4425 _exptl_absorpt_correction_T_max 0.7469 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5208 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 59.99 _reflns_number_total 5177 _reflns_number_observed 3100 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+1.9167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5173 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_obs 0.0652 _refine_ls_wR_factor_all 0.1791 _refine_ls_wR_factor_obs 0.1424 _refine_ls_goodness_of_fit_all 1.024 _refine_ls_goodness_of_fit_obs 1.093 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.093 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.49441(7) 0.22385(5) 0.18475(5) 0.0465(3) Uani 1 d . . O1 O 0.5616(3) 0.3118(2) 0.1616(2) 0.0541(9) Uani 1 d . . N1 N 0.5073(4) 0.1935(3) 0.0618(3) 0.0533(11) Uani 1 d . . O2 O 0.4707(3) 0.2558(2) 0.2924(2) 0.0579(10) Uani 1 d . . N2 N 0.6625(4) 0.1900(3) 0.2329(3) 0.0524(11) Uani 1 d . . O3 O 0.4316(3) 0.1342(2) 0.2089(2) 0.0557(10) Uani 1 d . . N3 N 0.3241(4) 0.2561(3) 0.1459(3) 0.0534(12) Uani 1 d . . C1 C 0.5735(5) 0.2272(3) 0.0108(3) 0.0565(14) Uani 1 d . . C2 C 0.5805(6) 0.2005(4) -0.0702(4) 0.071(2) Uani 1 d . . H2A H 0.6279(6) 0.2229(4) -0.1054(4) 0.086 Uiso 1 calc R . C3 C 0.5193(6) 0.1433(4) -0.0968(4) 0.077(2) Uani 1 d . . H3A H 0.5242(6) 0.1264(4) -0.1509(4) 0.093 Uiso 1 calc R . C4 C 0.4492(6) 0.1085(4) -0.0465(4) 0.070(2) Uani 1 d . . C5 C 0.4455(5) 0.1360(3) 0.0317(4) 0.064(2) Uani 1 d . . H5A H 0.3975(5) 0.1138(3) 0.0667(4) 0.077 Uiso 1 calc R . C6 C 0.6370(5) 0.2897(3) 0.0356(4) 0.061(2) Uani 1 d . . H6A H 0.6906(5) 0.3055(3) 0.0003(4) 0.074 Uiso 1 calc R . C7 C 0.6277(4) 0.3283(3) 0.1046(3) 0.0547(14) Uani 1 d . . C8 C 0.3815(7) 0.0441(4) -0.0728(5) 0.093(2) Uani 1 d . . H8A H 0.4354(7) 0.0088(4) -0.0877(5) 0.139 Uiso 1 d R . H8B H 0.3233(7) 0.0542(4) -0.1207(5) 0.139 Uiso 1 d R . H8C H 0.3418(7) 0.0275(4) -0.0271(5) 0.139 Uiso 1 d R . C9 C 0.6941(6) 0.3971(4) 0.1226(4) 0.067(2) Uani 1 d . . C10 C 0.7751(6) 0.4152(4) 0.0584(5) 0.088(2) Uani 1 d . . H10A H 0.8338(6) 0.3790(4) 0.0572(5) 0.132 Uiso 1 calc R . H10B H 0.8143(6) 0.4589(4) 0.0732(5) 0.132 Uiso 1 calc R . H10C H 0.7289(6) 0.4192(4) 0.0036(5) 0.132 Uiso 1 calc R . C11 C 0.6028(9) 0.4539(4) 0.1239(7) 0.127(4) Uani 1 d . . H11A H 0.5508(9) 0.4428(4) 0.1648(7) 0.191 Uiso 1 calc R . H11B H 0.5569(9) 0.4579(4) 0.0691(7) 0.191 Uiso 1 calc R . H11C H 0.6424(9) 0.4976(4) 0.1387(7) 0.191 Uiso 1 calc R . C12 C 0.7707(9) 0.3909(6) 0.2069(5) 0.142(5) Uani 1 d . . H12A H 0.8283(9) 0.3542(6) 0.2044(5) 0.213 Uiso 1 calc R . H12B H 0.7213(9) 0.3801(6) 0.2496(5) 0.213 Uiso 1 calc R . H12C H 0.8114(9) 0.4344(6) 0.2203(5) 0.213 Uiso 1 calc R . C21 C 0.7192(4) 0.2147(3) 0.3061(3) 0.0549(14) Uani 1 d . . C22 C 0.8365(5) 0.1921(4) 0.3324(4) 0.068(2) Uani 1 d . . H22A H 0.8775(5) 0.2104(4) 0.3819(4) 0.082 Uiso 1 calc R . C23 C 0.8914(5) 0.1453(4) 0.2885(4) 0.072(2) Uani 1 d . . H23A H 0.9688(5) 0.1306(4) 0.3077(4) 0.086 Uiso 1 calc R . C24 C 0.8316(5) 0.1192(3) 0.2150(4) 0.062(2) Uani 1 d . . C25 C 0.7186(4) 0.1427(3) 0.1903(4) 0.0578(15) Uani 1 d . . H25A H 0.6777(4) 0.1248(3) 0.1406(4) 0.069 Uiso 1 calc R . C26 C 0.6652(4) 0.2623(3) 0.3576(3) 0.058(2) Uani 1 d . . H26A H 0.7152(4) 0.2837(3) 0.4011(3) 0.069 Uiso 1 calc R . C27 C 0.5505(4) 0.2796(3) 0.3500(3) 0.0536(13) Uani 1 d . . C28 C 0.8892(6) 0.0688(4) 0.1606(5) 0.086(2) Uani 1 d . . H28A H 0.9012(6) 0.0245(4) 0.1891(5) 0.129 Uiso 1 d R . H28B H 0.9648(6) 0.0872(4) 0.1499(5) 0.129 Uiso 1 d R . H28C H 0.8384(6) 0.0623(4) 0.1081(5) 0.129 Uiso 1 d R . C29 C 0.4979(5) 0.3280(4) 0.4117(4) 0.064(2) Uani 1 d . . C30 C 0.5893(6) 0.3586(4) 0.4780(4) 0.090(2) Uani 1 d . . H30A H 0.6318(6) 0.3215(4) 0.5095(4) 0.135 Uiso 1 calc R . H30B H 0.5503(6) 0.3873(4) 0.5154(4) 0.135 Uiso 1 calc R . H30C H 0.6443(6) 0.3867(4) 0.4516(4) 0.135 Uiso 1 calc R . C31 C 0.4324(8) 0.3855(4) 0.3633(5) 0.102(3) Uani 1 d . . H31A H 0.3737(8) 0.3661(4) 0.3206(5) 0.153 Uiso 1 calc R . H31B H 0.4876(8) 0.4136(4) 0.3370(5) 0.153 Uiso 1 calc R . H31C H 0.3936(8) 0.4142(4) 0.4008(5) 0.153 Uiso 1 calc R . C32 C 0.4090(6) 0.2845(5) 0.4541(4) 0.092(2) Uani 1 d . . H32A H 0.4505(6) 0.2470(5) 0.4856(4) 0.138 Uiso 1 calc R . H32B H 0.3496(6) 0.2653(5) 0.4117(4) 0.138 Uiso 1 calc R . H32C H 0.3712(6) 0.3138(5) 0.4915(4) 0.138 Uiso 1 calc R . C41 C 0.2312(4) 0.2309(4) 0.1823(4) 0.060(2) Uani 1 d . . C42 C 0.1216(5) 0.2663(4) 0.1676(5) 0.076(2) Uani 1 d . . H42A H 0.0576(5) 0.2521(4) 0.1947(5) 0.091 Uiso 1 calc R . C43 C 0.1101(6) 0.3211(4) 0.1138(5) 0.084(2) Uani 1 d . . H43A H 0.0375(6) 0.3447(4) 0.1050(5) 0.101 Uiso 1 calc R . C44 C 0.1994(6) 0.3430(4) 0.0721(4) 0.072(2) Uani 1 d . . C45 C 0.3074(5) 0.3100(3) 0.0927(3) 0.062(2) Uani 1 d . . H45A H 0.3724(5) 0.3263(3) 0.0683(3) 0.074 Uiso 1 calc R . C46 C 0.2401(4) 0.1687(4) 0.2305(4) 0.062(2) Uani 1 d . . H46A H 0.1764(4) 0.1580(4) 0.2596(4) 0.075 Uiso 1 calc R . C47 C 0.3330(4) 0.1227(3) 0.2385(3) 0.0559(14) Uani 1 d . . C48 C 0.1873(7) 0.3985(4) 0.0065(5) 0.096(3) Uani 1 d . . H48A H 0.1676(7) 0.3776(4) -0.0482(5) 0.144 Uiso 1 d R . H48B H 0.2613(7) 0.4236(4) 0.0085(5) 0.144 Uiso 1 d R . H48C H 0.1251(7) 0.4304(4) 0.0167(5) 0.144 Uiso 1 d R . C49 C 0.3295(5) 0.0529(4) 0.2828(4) 0.066(2) Uani 1 d . . C50 C 0.2112(5) 0.0370(5) 0.3124(5) 0.091(2) Uani 1 d . . H50A H 0.1922(5) 0.0732(5) 0.3502(5) 0.136 Uiso 1 calc R . H50B H 0.2159(5) -0.0073(5) 0.3412(5) 0.136 Uiso 1 calc R . H50C H 0.1501(5) 0.0349(5) 0.2646(5) 0.136 Uiso 1 calc R . C51 C 0.3587(8) -0.0039(4) 0.2236(6) 0.116(3) Uani 1 d . . H51A H 0.4341(8) 0.0061(4) 0.2047(6) 0.174 Uiso 1 calc R . H51B H 0.2975(8) -0.0059(4) 0.1759(6) 0.174 Uiso 1 calc R . H51C H 0.3633(8) -0.0481(4) 0.2525(6) 0.174 Uiso 1 calc R . C52 C 0.4254(6) 0.0561(5) 0.3583(5) 0.104(3) Uani 1 d . . H52A H 0.4065(6) 0.0924(5) 0.3959(5) 0.157 Uiso 1 calc R . H52B H 0.5010(6) 0.0660(5) 0.3397(5) 0.157 Uiso 1 calc R . H52C H 0.4296(6) 0.0119(5) 0.3872(5) 0.157 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0366(4) 0.0595(6) 0.0423(5) 0.0007(5) 0.0010(3) 0.0039(4) O1 0.056(2) 0.060(2) 0.047(2) -0.003(2) 0.009(2) -0.002(2) N1 0.048(2) 0.061(3) 0.049(3) -0.001(2) -0.002(2) 0.010(2) O2 0.045(2) 0.079(3) 0.049(2) 0.002(2) 0.0038(15) 0.006(2) N2 0.045(2) 0.056(3) 0.058(3) 0.000(2) 0.012(2) -0.001(2) O3 0.038(2) 0.067(3) 0.062(2) 0.010(2) 0.006(2) 0.001(2) N3 0.049(2) 0.061(3) 0.046(3) -0.001(2) -0.006(2) 0.007(2) C1 0.057(3) 0.069(4) 0.043(3) -0.004(3) 0.003(2) 0.015(3) C2 0.076(4) 0.085(5) 0.054(4) -0.004(4) 0.012(3) 0.012(3) C3 0.080(4) 0.091(6) 0.058(4) -0.014(4) -0.003(3) 0.022(4) C4 0.074(4) 0.071(5) 0.060(4) -0.014(4) -0.012(3) 0.013(3) C5 0.060(3) 0.067(4) 0.061(4) 0.000(3) -0.007(3) 0.007(3) C6 0.057(3) 0.075(5) 0.053(3) 0.006(3) 0.012(2) 0.007(3) C7 0.047(3) 0.064(4) 0.052(3) 0.011(3) 0.001(2) 0.009(2) C8 0.099(5) 0.087(6) 0.085(5) -0.021(5) -0.015(4) 0.013(4) C9 0.075(4) 0.066(4) 0.062(4) 0.008(3) 0.015(3) -0.013(3) C10 0.093(5) 0.089(6) 0.084(5) 0.021(4) 0.020(4) -0.020(4) C11 0.154(9) 0.063(6) 0.178(10) -0.020(6) 0.069(8) -0.006(6) C12 0.156(9) 0.176(11) 0.082(6) 0.031(6) -0.028(6) -0.105(8) C21 0.037(2) 0.064(4) 0.061(3) 0.024(3) -0.002(2) -0.005(2) C22 0.041(3) 0.089(5) 0.070(4) 0.011(4) -0.008(3) -0.004(3) C23 0.043(3) 0.083(5) 0.088(5) 0.010(4) 0.006(3) 0.008(3) C24 0.050(3) 0.063(4) 0.073(4) 0.013(3) 0.012(3) 0.010(3) C25 0.047(3) 0.065(4) 0.061(4) 0.002(3) 0.006(2) 0.002(3) C26 0.049(3) 0.075(4) 0.047(3) 0.008(3) -0.003(2) -0.011(3) C27 0.051(3) 0.060(4) 0.051(3) 0.003(3) 0.009(2) -0.010(3) C28 0.068(4) 0.101(6) 0.091(5) 0.003(4) 0.015(3) 0.023(4) C29 0.062(3) 0.075(5) 0.056(4) -0.001(3) 0.008(3) -0.001(3) C30 0.088(5) 0.106(6) 0.078(5) -0.029(5) 0.021(4) -0.022(4) C31 0.123(7) 0.079(6) 0.103(6) -0.020(5) 0.007(5) 0.023(5) C32 0.072(4) 0.129(7) 0.080(5) -0.016(5) 0.029(3) -0.011(4) C41 0.040(2) 0.074(4) 0.065(3) -0.018(3) -0.001(2) 0.008(3) C42 0.046(3) 0.076(5) 0.101(5) -0.010(4) -0.005(3) 0.014(3) C43 0.053(3) 0.093(6) 0.101(5) -0.015(5) -0.016(3) 0.026(4) C44 0.075(4) 0.065(4) 0.066(4) -0.012(3) -0.019(3) 0.022(3) C45 0.063(3) 0.070(4) 0.048(3) -0.012(3) -0.009(2) 0.008(3) C46 0.038(3) 0.078(4) 0.070(4) 0.000(3) 0.004(2) 0.005(3) C47 0.043(3) 0.071(4) 0.052(3) -0.003(3) 0.001(2) 0.000(2) C48 0.112(6) 0.072(5) 0.094(6) -0.005(4) -0.025(4) 0.033(4) C49 0.050(3) 0.074(4) 0.074(4) 0.018(3) 0.011(3) -0.006(3) C50 0.056(3) 0.121(7) 0.095(5) 0.027(5) 0.010(3) -0.014(4) C51 0.135(8) 0.069(6) 0.158(9) 0.007(6) 0.067(7) -0.001(5) C52 0.057(4) 0.149(8) 0.104(6) 0.063(6) -0.004(4) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr O2 1.898(4) . ? Cr O1 1.919(4) . ? Cr O3 1.931(4) . ? Cr N3 2.059(4) . ? Cr N2 2.078(4) . ? Cr N1 2.093(5) . ? O1 C7 1.304(6) . ? N1 C1 1.355(7) . ? N1 C5 1.369(8) . ? O2 C27 1.296(6) . ? N2 C25 1.353(7) . ? N2 C21 1.356(7) . ? O3 C47 1.299(6) . ? N3 C45 1.345(8) . ? N3 C41 1.369(7) . ? C1 C2 1.418(8) . ? C1 C6 1.437(9) . ? C2 C3 1.347(10) . ? C3 C4 1.386(10) . ? C4 C5 1.375(8) . ? C4 C8 1.495(10) . ? C6 C7 1.356(8) . ? C7 C9 1.537(9) . ? C9 C11 1.515(11) . ? C9 C10 1.520(8) . ? C9 C12 1.521(10) . ? C21 C22 1.419(7) . ? C21 C26 1.433(8) . ? C22 C23 1.352(9) . ? C23 C24 1.383(9) . ? C24 C25 1.375(7) . ? C24 C28 1.518(9) . ? C26 C27 1.340(7) . ? C27 C29 1.543(8) . ? C29 C31 1.500(10) . ? C29 C30 1.512(9) . ? C29 C32 1.544(9) . ? C41 C42 1.418(8) . ? C41 C46 1.427(9) . ? C42 C43 1.364(10) . ? C43 C44 1.362(10) . ? C44 C45 1.388(8) . ? C44 C48 1.500(10) . ? C46 C47 1.375(8) . ? C47 C49 1.528(9) . ? C49 C51 1.519(10) . ? C49 C50 1.523(8) . ? C49 C52 1.527(9) . ? 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 O2 Cr O1 90.0(2) . . ? O2 Cr O3 90.2(2) . . ? O1 Cr O3 178.2(2) . . ? O2 Cr N3 86.4(2) . . ? O1 Cr N3 93.4(2) . . ? O3 Cr N3 88.4(2) . . ? O2 Cr N2 89.8(2) . . ? O1 Cr N2 88.7(2) . . ? O3 Cr N2 89.6(2) . . ? N3 Cr N2 175.7(2) . . ? O2 Cr N1 175.0(2) . . ? O1 Cr N1 89.0(2) . . ? O3 Cr N1 90.9(2) . . ? N3 Cr N1 88.8(2) . . ? N2 Cr N1 95.1(2) . . ? C7 O1 Cr 129.5(4) . . ? C1 N1 C5 118.4(5) . . ? C1 N1 Cr 123.9(4) . . ? C5 N1 Cr 117.7(4) . . ? C27 O2 Cr 126.8(3) . . ? C25 N2 C21 118.4(5) . . ? C25 N2 Cr 119.9(4) . . ? C21 N2 Cr 121.7(4) . . ? C47 O3 Cr 126.2(4) . . ? C45 N3 C41 119.7(5) . . ? C45 N3 Cr 118.4(4) . . ? C41 N3 Cr 121.1(4) . . ? N1 C1 C2 119.4(6) . . ? N1 C1 C6 122.3(5) . . ? C2 C1 C6 118.2(6) . . ? C3 C2 C1 120.1(7) . . ? C2 C3 C4 121.6(6) . . ? C5 C4 C3 116.3(7) . . ? C5 C4 C8 120.2(7) . . ? C3 C4 C8 123.5(7) . . ? N1 C5 C4 124.1(6) . . ? C7 C6 C1 126.7(5) . . ? O1 C7 C6 124.3(6) . . ? O1 C7 C9 113.2(5) . . ? C6 C7 C9 122.5(5) . . ? C11 C9 C10 109.0(6) . . ? C11 C9 C12 111.1(8) . . ? C10 C9 C12 107.4(6) . . ? C11 C9 C7 107.7(6) . . ? C10 C9 C7 113.5(6) . . ? C12 C9 C7 108.2(6) . . ? N2 C21 C22 118.4(6) . . ? N2 C21 C26 122.6(4) . . ? C22 C21 C26 119.0(5) . . ? C23 C22 C21 122.2(6) . . ? C22 C23 C24 118.8(5) . . ? C25 C24 C23 117.8(6) . . ? C25 C24 C28 120.4(6) . . ? C23 C24 C28 121.8(5) . . ? N2 C25 C24 124.4(6) . . ? C27 C26 C21 126.6(5) . . ? O2 C27 C26 124.2(5) . . ? O2 C27 C29 112.3(4) . . ? C26 C27 C29 123.4(5) . . ? C31 C29 C30 109.2(7) . . ? C31 C29 C27 108.7(5) . . ? C30 C29 C27 113.7(5) . . ? C31 C29 C32 108.8(6) . . ? C30 C29 C32 109.3(5) . . ? C27 C29 C32 107.1(6) . . ? N3 C41 C42 118.4(6) . . ? N3 C41 C46 122.0(5) . . ? C42 C41 C46 119.5(6) . . ? C43 C42 C41 119.1(7) . . ? C44 C43 C42 122.7(6) . . ? C43 C44 C45 116.1(7) . . ? C43 C44 C48 124.5(6) . . ? C45 C44 C48 119.5(7) . . ? N3 C45 C44 123.6(6) . . ? C47 C46 C41 126.3(5) . . ? O3 C47 C46 123.5(6) . . ? O3 C47 C49 113.6(5) . . ? C46 C47 C49 123.0(5) . . ? C51 C49 C50 109.3(6) . . ? C51 C49 C52 109.7(7) . . ? C50 C49 C52 109.2(5) . . ? C51 C49 C47 108.6(5) . . ? C50 C49 C47 113.8(5) . . ? C52 C49 C47 106.1(6) . . ? _refine_diff_density_max 0.249 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.051 #===END data_Compound_7 _database_code_CSD 216352 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H53 N5 O2 Cl2 Cr2' _chemical_formula_weight 810.77 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 16.147(2) _cell_length_b 11.9358(15) _cell_length_c 21.325(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.896(15) _cell_angle_gamma 90.00 _cell_volume 4104.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 4.69 _cell_measurement_theta_max 12.49 _exptl_crystal_description blocks _exptl_crystal_colour 'Blue/green dichroic' _exptl_crystal_size_max 0.93 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_min 0.67 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method ? _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 38.79 _diffrn_reflns_number 7419 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.1155 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7147 _reflns_number_observed 3907 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1009 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6138 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_obs 0.0620 _refine_ls_wR_factor_all 0.1488 _refine_ls_wR_factor_obs 0.1164 _refine_ls_goodness_of_fit_all 0.991 _refine_ls_goodness_of_fit_obs 1.109 _refine_ls_restrained_S_all 1.023 _refine_ls_restrained_S_obs 1.109 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr 0.75021(6) 0.14614(6) 0.24426(4) 0.0309(2) Uani 1 d . . Cr2 Cr 0.74328(6) 0.37329(7) 0.19362(4) 0.0366(2) Uani 1 d . . Cl1 Cl 0.67355(11) 0.31996(14) 0.30895(7) 0.0542(4) Uani 1 d . . Cl2 Cl 0.80349(12) 0.54255(11) 0.23075(8) 0.0574(5) Uani 1 d . . O1 O 0.6914(2) 0.2226(3) 0.1705(2) 0.0335(8) Uani 1 d . . O2 O 0.8321(2) 0.2644(3) 0.2271(2) 0.0288(8) Uani 1 d . . N1 N 0.6779(3) -0.0046(4) 0.2283(2) 0.0366(11) Uani 1 d . . N2 N 0.6553(4) 0.4581(4) 0.1296(2) 0.0487(14) Uani 1 d . . N3 N 0.8269(3) 0.1043(3) 0.3253(2) 0.0347(10) Uani 1 d . . N4 N 1.0428(3) 0.3552(4) 0.3525(2) 0.0424(11) Uani 1 d . . C1 C 0.7080(4) -0.1110(4) 0.2321(3) 0.0422(14) Uani 1 d . . C2 C 0.6587(5) -0.2040(5) 0.2169(3) 0.056(2) Uani 1 d . . H2A H 0.6809(5) -0.2759(5) 0.2188(3) 0.067 Uiso 1 calc R . C3 C 0.5762(5) -0.1869(5) 0.1988(3) 0.059(2) Uani 1 d . . H3A H 0.5417(5) -0.2477(5) 0.1895(3) 0.071 Uiso 1 calc R . C4 C 0.5456(4) -0.0813(6) 0.1948(3) 0.057(2) Uani 1 d . . H4A H 0.4901(4) -0.0694(6) 0.1831(3) 0.068 Uiso 1 calc R . C5 C 0.5978(4) 0.0095(5) 0.2082(3) 0.0440(14) Uani 1 d . . C6 C 0.5662(4) 0.1282(5) 0.2015(3) 0.0454(14) Uani 1 d . . H6A H 0.5727(4) 0.1636(5) 0.2424(3) 0.054 Uiso 1 calc R . H6B H 0.5071(4) 0.1244(5) 0.1908(3) 0.054 Uiso 1 calc R . C7 C 0.6058(4) 0.2073(5) 0.1529(3) 0.0406(13) Uani 1 d . . C8 C 0.5573(4) 0.3176(5) 0.1659(3) 0.051(2) Uani 1 d . . H8A H 0.4988(4) 0.3017(5) 0.1579(3) 0.061 Uiso 1 calc R . H8B H 0.5653(4) 0.3337(5) 0.2104(3) 0.061 Uiso 1 calc R . C9 C 0.5760(5) 0.4235(6) 0.1312(3) 0.054(2) Uani 1 d . . C10 C 0.5106(5) 0.4827(7) 0.1027(4) 0.074(2) Uani 1 d . . H10A H 0.4562(5) 0.4581(7) 0.1050(4) 0.089 Uiso 1 calc R . C11 C 0.5291(7) 0.5803(7) 0.0704(5) 0.096(3) Uani 1 d . . H11A H 0.4865(7) 0.6256(7) 0.0539(5) 0.115 Uiso 1 calc R . C12 C 0.6092(7) 0.6090(7) 0.0631(4) 0.084(3) Uani 1 d . . H12A H 0.6213(7) 0.6696(7) 0.0377(4) 0.101 Uiso 1 calc R . C13 C 0.6733(5) 0.5492(5) 0.0931(3) 0.060(2) Uani 1 d . . C14 C 0.7963(4) -0.1293(5) 0.2523(3) 0.056(2) Uani 1 d . . H14A H 0.8086(4) -0.2080(5) 0.2512(3) 0.083 Uiso 1 d R . H14B H 0.8064(4) -0.1016(5) 0.2942(3) 0.083 Uiso 1 d R . H14C H 0.8312(4) -0.0902(5) 0.2244(3) 0.083 Uiso 1 d R . C15 C 0.7601(5) 0.5791(6) 0.0822(3) 0.072(2) Uani 1 d . . H15A H 0.7785(5) 0.6359(6) 0.1116(3) 0.108 Uiso 1 d R . H15B H 0.7637(5) 0.6068(6) 0.0402(3) 0.108 Uiso 1 d R . H15C H 0.7945(5) 0.5139(6) 0.0878(3) 0.108 Uiso 1 d R . C16 C 0.5985(4) 0.1656(5) 0.0825(3) 0.050(2) Uani 1 d . . C17 C 0.6451(5) 0.0557(5) 0.0740(3) 0.055(2) Uani 1 d . . H17A H 0.6231(5) -0.0007(5) 0.1006(3) 0.082 Uiso 1 calc R . H17B H 0.7029(5) 0.0666(5) 0.0852(3) 0.082 Uiso 1 calc R . H17C H 0.6387(5) 0.0322(5) 0.0310(3) 0.082 Uiso 1 calc R . C18 C 0.5079(5) 0.1486(8) 0.0603(4) 0.078(2) Uani 1 d . . H18A H 0.4823(5) 0.0962(8) 0.0876(4) 0.117 Uiso 1 calc R . H18B H 0.5052(5) 0.1199(8) 0.0182(4) 0.117 Uiso 1 calc R . H18C H 0.4791(5) 0.2189(8) 0.0613(4) 0.117 Uiso 1 calc R . C19 C 0.6377(5) 0.2488(6) 0.0388(3) 0.064(2) Uani 1 d . . H19A H 0.6948(5) 0.2602(6) 0.0522(3) 0.096 Uiso 1 calc R . H19B H 0.6086(5) 0.3188(6) 0.0398(3) 0.096 Uiso 1 calc R . H19C H 0.6347(5) 0.2198(6) -0.0033(3) 0.096 Uiso 1 calc R . C21 C 0.7978(4) 0.0840(5) 0.3823(3) 0.0440(14) Uani 1 d . . C22 C 0.8513(5) 0.0772(6) 0.4353(3) 0.061(2) Uani 1 d . . H22A H 0.8302(5) 0.0653(6) 0.4745(3) 0.073 Uiso 1 calc R . C23 C 0.9357(5) 0.0880(5) 0.4297(3) 0.059(2) Uani 1 d . . H23A H 0.9720(5) 0.0820(5) 0.4648(3) 0.071 Uiso 1 calc R . C24 C 0.9649(4) 0.1077(4) 0.3722(3) 0.0442(15) Uani 1 d . . H24A H 1.0216(4) 0.1155(4) 0.3676(3) 0.053 Uiso 1 calc R . C25 C 0.9097(4) 0.1163(4) 0.3200(2) 0.0337(12) Uani 1 d . . C26 C 0.9425(3) 0.1359(4) 0.2562(2) 0.0356(12) Uani 1 d . . H26A H 0.9240(3) 0.0745(4) 0.2292(2) 0.043 Uiso 1 calc R . H26B H 1.0026(3) 0.1321(4) 0.2603(2) 0.043 Uiso 1 calc R . C27 C 0.9182(3) 0.2482(4) 0.2220(2) 0.0294(11) Uani 1 d . . C28 C 0.9670(4) 0.3465(4) 0.2521(2) 0.0347(12) Uani 1 d . . H28A H 1.0242(4) 0.3402(4) 0.2405(2) 0.042 Uiso 1 calc R . H28B H 0.9450(4) 0.4153(4) 0.2338(2) 0.042 Uiso 1 calc R . C29 C 0.9671(4) 0.3574(4) 0.3226(2) 0.0346(12) Uani 1 d . . C30 C 0.8950(4) 0.3727(4) 0.3547(3) 0.0408(13) Uani 1 d . . H30A H 0.8438(4) 0.3776(4) 0.3329(3) 0.049 Uiso 1 calc R . C31 C 0.9008(4) 0.3805(5) 0.4197(3) 0.050(2) Uani 1 d . . H31A H 0.8534(4) 0.3878(5) 0.4424(3) 0.060 Uiso 1 calc R . C32 C 0.9786(5) 0.3772(5) 0.4498(3) 0.056(2) Uani 1 d . . H32A H 0.9841(5) 0.3824(5) 0.4934(3) 0.067 Uiso 1 calc R . C33 C 1.0473(4) 0.3662(5) 0.4155(3) 0.0471(15) Uani 1 d . . C34 C 0.7063(5) 0.0675(6) 0.3865(3) 0.063(2) Uani 1 d . . H34A H 0.6941(5) 0.0514(6) 0.4292(3) 0.094 Uiso 1 d R . H34B H 0.6884(5) 0.0061(6) 0.3601(3) 0.094 Uiso 1 d R . H34C H 0.6777(5) 0.1345(6) 0.3730(3) 0.094 Uiso 1 d R . C35 C 1.1327(5) 0.3630(6) 0.4465(3) 0.069(2) Uani 1 d . . H35A H 1.1381(5) 0.2979(6) 0.4728(3) 0.104 Uiso 1 d R . H35B H 1.1417(5) 0.4291(6) 0.4715(3) 0.104 Uiso 1 d R . H35C H 1.1730(5) 0.3599(6) 0.4150(3) 0.104 Uiso 1 d R . C36 C 0.9393(4) 0.2345(4) 0.1508(2) 0.0359(12) Uani 1 d . . C37 C 0.8822(4) 0.1483(5) 0.1182(3) 0.050(2) Uani 1 d . . H37A H 0.8890(4) 0.0773(5) 0.1390(3) 0.074 Uiso 1 calc R . H37B H 0.8961(4) 0.1409(5) 0.0752(3) 0.074 Uiso 1 calc R . H37C H 0.8257(4) 0.1725(5) 0.1200(3) 0.074 Uiso 1 calc R . C38 C 0.9257(6) 0.3446(6) 0.1159(3) 0.068(2) Uani 1 d . . H38A H 0.9607(6) 0.4013(6) 0.1351(3) 0.102 Uiso 1 calc R . H38B H 0.8687(6) 0.3667(6) 0.1176(3) 0.102 Uiso 1 calc R . H38C H 0.9392(6) 0.3351(6) 0.0728(3) 0.102 Uiso 1 calc R . C39 C 1.0294(4) 0.1954(7) 0.1436(3) 0.063(2) Uani 1 d . . H39A H 1.0385(4) 0.1259(7) 0.1656(3) 0.094 Uiso 1 calc R . H39B H 1.0670(4) 0.2511(7) 0.1609(3) 0.094 Uiso 1 calc R . H39C H 1.0389(4) 0.1850(7) 0.0999(3) 0.094 Uiso 1 calc R . N40 N 0.3008(10) 0.2843(9) 0.0836(7) 0.185(6) Uani 1 d . . C41 C 0.2879(7) 0.1976(8) 0.0986(5) 0.091(3) Uani 1 d . . C42 C 0.2719(8) 0.0872(9) 0.1162(6) 0.121(4) Uani 1 d . . H42A H 0.2142(8) 0.0795(9) 0.1243(6) 0.182 Uiso 1 d R . H42B H 0.3050(8) 0.0689(9) 0.1534(6) 0.182 Uiso 1 d R . H42C H 0.2854(8) 0.0375(9) 0.0828(6) 0.182 Uiso 1 d 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 0.0271(5) 0.0288(4) 0.0360(4) 0.0040(3) -0.0049(4) -0.0021(4) Cr2 0.0385(6) 0.0262(4) 0.0439(5) 0.0010(3) -0.0101(4) 0.0048(4) Cl1 0.0433(10) 0.0661(9) 0.0530(8) -0.0121(7) 0.0008(7) 0.0101(8) Cl2 0.0728(12) 0.0297(6) 0.0676(10) -0.0036(6) -0.0180(9) 0.0022(7) O1 0.026(2) 0.036(2) 0.036(2) -0.0006(14) -0.009(2) 0.004(2) O2 0.025(2) 0.0243(15) 0.037(2) 0.0011(13) -0.002(2) 0.0000(15) N1 0.026(3) 0.038(2) 0.045(2) 0.003(2) -0.005(2) -0.007(2) N2 0.058(4) 0.040(2) 0.047(3) 0.003(2) -0.014(3) 0.017(3) N3 0.038(3) 0.029(2) 0.036(2) 0.005(2) 0.001(2) 0.003(2) N4 0.046(3) 0.032(2) 0.048(3) -0.005(2) -0.007(2) -0.006(2) C1 0.039(4) 0.035(3) 0.053(3) 0.002(2) 0.004(3) -0.007(3) C2 0.061(5) 0.041(3) 0.066(4) -0.008(3) 0.004(4) -0.009(3) C3 0.061(5) 0.047(3) 0.069(4) -0.004(3) -0.002(4) -0.021(4) C4 0.037(4) 0.064(4) 0.069(4) 0.003(3) -0.003(3) -0.012(3) C5 0.029(3) 0.049(3) 0.054(3) 0.004(3) 0.001(3) -0.007(3) C6 0.024(3) 0.056(3) 0.056(3) -0.004(3) 0.001(3) 0.001(3) C7 0.031(3) 0.040(3) 0.050(3) -0.001(2) -0.005(3) 0.007(3) C8 0.037(4) 0.051(3) 0.063(4) -0.002(3) -0.014(3) 0.017(3) C9 0.047(4) 0.058(4) 0.054(4) -0.003(3) -0.014(3) 0.018(3) C10 0.062(5) 0.071(5) 0.088(5) 0.005(4) -0.019(4) 0.033(4) C11 0.110(9) 0.067(5) 0.106(7) 0.025(5) -0.040(7) 0.032(6) C12 0.104(8) 0.063(5) 0.081(5) 0.023(4) -0.025(5) 0.020(5) C13 0.086(6) 0.043(3) 0.049(3) 0.012(3) -0.017(4) 0.008(4) C14 0.045(4) 0.036(3) 0.085(4) -0.002(3) -0.005(3) 0.000(3) C15 0.096(7) 0.051(4) 0.068(4) 0.026(3) 0.001(4) 0.001(4) C16 0.043(4) 0.059(4) 0.047(3) -0.005(3) -0.016(3) 0.006(3) C17 0.066(5) 0.054(3) 0.044(3) -0.010(3) -0.001(3) -0.003(4) C18 0.049(5) 0.107(6) 0.075(5) -0.021(5) -0.028(4) -0.002(5) C19 0.085(6) 0.063(4) 0.041(3) 0.003(3) -0.016(4) 0.008(4) C21 0.059(4) 0.037(3) 0.037(3) 0.002(2) 0.005(3) -0.003(3) C22 0.090(6) 0.059(4) 0.034(3) 0.016(3) 0.006(4) -0.002(4) C23 0.080(6) 0.051(3) 0.046(4) 0.009(3) -0.018(4) 0.002(4) C24 0.044(4) 0.036(3) 0.051(3) 0.008(2) -0.019(3) 0.005(3) C25 0.041(4) 0.022(2) 0.036(3) 0.006(2) -0.007(2) 0.001(2) C26 0.026(3) 0.034(2) 0.046(3) -0.007(2) -0.005(2) 0.002(3) C27 0.028(3) 0.028(2) 0.031(2) -0.001(2) -0.002(2) -0.003(2) C28 0.036(3) 0.033(2) 0.036(3) -0.003(2) 0.006(2) -0.008(2) C29 0.040(3) 0.025(2) 0.038(3) -0.003(2) -0.006(3) -0.003(2) C30 0.043(4) 0.035(3) 0.045(3) -0.004(2) 0.001(3) 0.001(3) C31 0.054(4) 0.049(3) 0.048(3) -0.009(3) 0.007(3) 0.004(3) C32 0.079(5) 0.050(3) 0.038(3) -0.002(3) -0.010(3) 0.001(4) C33 0.058(4) 0.037(3) 0.045(3) -0.002(2) -0.009(3) 0.002(3) C34 0.062(5) 0.070(4) 0.058(4) 0.008(3) 0.019(4) -0.010(4) C35 0.072(5) 0.067(4) 0.066(4) -0.003(4) -0.032(4) 0.004(4) C36 0.032(3) 0.042(3) 0.033(2) -0.005(2) -0.003(2) -0.002(3) C37 0.057(4) 0.054(3) 0.037(3) -0.015(3) -0.001(3) -0.009(3) C38 0.107(7) 0.056(4) 0.040(3) 0.010(3) 0.007(4) -0.009(4) C39 0.044(4) 0.102(5) 0.044(3) -0.019(4) 0.014(3) -0.001(4) N40 0.249(17) 0.086(7) 0.226(14) 0.013(8) 0.078(13) -0.007(9) C41 0.102(8) 0.072(5) 0.101(7) 0.013(5) 0.015(6) 0.003(6) C42 0.140(11) 0.097(7) 0.125(9) 0.028(6) 0.004(8) -0.029(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 Cr1 O2 1.981(3) . ? Cr1 O1 2.014(3) . ? Cr1 N3 2.134(4) . ? Cr1 N1 2.163(4) . ? Cr1 Cl1 2.813(2) . ? Cr1 Cr2 2.9185(12) . ? Cr2 O1 2.035(4) . ? Cr2 O2 2.037(3) . ? Cr2 N2 2.171(5) . ? Cr2 Cl2 2.361(2) . ? Cr2 Cl1 2.829(2) . ? O1 C7 1.426(7) . ? O2 C27 1.414(6) . ? N1 C5 1.353(8) . ? N1 C1 1.360(7) . ? N2 C9 1.348(9) . ? N2 C13 1.376(8) . ? N3 C21 1.346(7) . ? N3 C25 1.356(7) . ? N4 C33 1.348(7) . ? N4 C29 1.350(7) . ? C1 C2 1.394(8) . ? C1 C14 1.486(8) . ? C2 C3 1.384(10) . ? C3 C4 1.355(10) . ? C4 C5 1.393(9) . ? C5 C6 1.510(8) . ? C6 C7 1.562(9) . ? C7 C8 1.563(8) . ? C7 C16 1.582(8) . ? C8 C9 1.503(9) . ? C9 C10 1.385(9) . ? C10 C11 1.393(12) . ? C11 C12 1.354(13) . ? C12 C13 1.388(10) . ? C13 C15 1.476(11) . ? C16 C19 1.522(10) . ? C16 C18 1.528(9) . ? C16 C17 1.528(9) . ? C21 C22 1.390(9) . ? C21 C34 1.498(10) . ? C22 C23 1.381(11) . ? C23 C24 1.357(9) . ? C24 C25 1.394(7) . ? C25 C26 1.502(8) . ? C26 C27 1.568(7) . ? C27 C28 1.535(6) . ? C27 C36 1.580(7) . ? C28 C29 1.510(7) . ? C29 C30 1.391(8) . ? C30 C31 1.388(8) . ? C31 C32 1.383(9) . ? C32 C33 1.366(10) . ? C33 C35 1.499(9) . ? C36 C38 1.521(8) . ? C36 C37 1.525(7) . ? C36 C39 1.544(9) . ? N40 C41 1.105(13) . ? C41 C42 1.398(13) . ? 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 O2 Cr1 O1 79.93(14) . . ? O2 Cr1 N3 87.2(2) . . ? O1 Cr1 N3 165.9(2) . . ? O2 Cr1 N1 157.5(2) . . ? O1 Cr1 N1 91.4(2) . . ? N3 Cr1 N1 102.7(2) . . ? O2 Cr1 Cl1 83.08(11) . . ? O1 Cr1 Cl1 81.23(11) . . ? N3 Cr1 Cl1 91.54(12) . . ? N1 Cr1 Cl1 116.35(14) . . ? O2 Cr1 Cr2 44.18(10) . . ? O1 Cr1 Cr2 44.16(10) . . ? N3 Cr1 Cr2 121.80(12) . . ? N1 Cr1 Cr2 134.78(12) . . ? Cl1 Cr1 Cr2 59.12(4) . . ? O1 Cr2 O2 78.15(13) . . ? O1 Cr2 N2 90.7(2) . . ? O2 Cr2 N2 160.8(2) . . ? O1 Cr2 Cl2 174.44(11) . . ? O2 Cr2 Cl2 99.07(10) . . ? N2 Cr2 Cl2 93.29(14) . . ? O1 Cr2 Cl1 80.50(11) . . ? O2 Cr2 Cl1 81.73(11) . . ? N2 Cr2 Cl1 112.0(2) . . ? Cl2 Cr2 Cl1 94.37(6) . . ? O1 Cr2 Cr1 43.60(9) . . ? O2 Cr2 Cr1 42.67(10) . . ? N2 Cr2 Cr1 132.66(15) . . ? Cl2 Cr2 Cr1 131.55(5) . . ? Cl1 Cr2 Cr1 58.58(4) . . ? Cr1 Cl1 Cr2 62.30(4) . . ? C7 O1 Cr1 124.0(3) . . ? C7 O1 Cr2 123.9(3) . . ? Cr1 O1 Cr2 92.24(13) . . ? C27 O2 Cr1 125.8(3) . . ? C27 O2 Cr2 137.6(3) . . ? Cr1 O2 Cr2 93.14(15) . . ? C5 N1 C1 117.9(5) . . ? C5 N1 Cr1 116.5(4) . . ? C1 N1 Cr1 125.4(4) . . ? C9 N2 C13 119.0(6) . . ? C9 N2 Cr2 115.7(4) . . ? C13 N2 Cr2 125.0(5) . . ? C21 N3 C25 119.1(5) . . ? C21 N3 Cr1 123.9(4) . . ? C25 N3 Cr1 116.2(3) . . ? C33 N4 C29 118.1(5) . . ? N1 C1 C2 122.1(6) . . ? N1 C1 C14 119.3(5) . . ? C2 C1 C14 118.6(6) . . ? C3 C2 C1 118.5(6) . . ? C4 C3 C2 119.8(6) . . ? C3 C4 C5 119.8(6) . . ? N1 C5 C4 121.8(6) . . ? N1 C5 C6 117.4(5) . . ? C4 C5 C6 120.8(6) . . ? C5 C6 C7 118.9(5) . . ? O1 C7 C6 109.1(4) . . ? O1 C7 C8 109.5(5) . . ? C6 C7 C8 99.6(5) . . ? O1 C7 C16 108.3(5) . . ? C6 C7 C16 115.2(5) . . ? C8 C7 C16 114.8(5) . . ? C9 C8 C7 120.4(6) . . ? N2 C9 C10 122.5(7) . . ? N2 C9 C8 119.0(5) . . ? C10 C9 C8 118.6(7) . . ? C9 C10 C11 117.8(9) . . ? C12 C11 C10 119.9(8) . . ? C11 C12 C13 120.7(8) . . ? N2 C13 C12 119.5(8) . . ? N2 C13 C15 120.6(6) . . ? C12 C13 C15 119.7(7) . . ? C19 C16 C18 108.6(6) . . ? C19 C16 C17 105.3(6) . . ? C18 C16 C17 108.6(6) . . ? C19 C16 C7 111.3(5) . . ? C18 C16 C7 111.1(6) . . ? C17 C16 C7 111.6(5) . . ? N3 C21 C22 120.9(6) . . ? N3 C21 C34 117.9(5) . . ? C22 C21 C34 121.2(6) . . ? C23 C22 C21 120.0(6) . . ? C24 C23 C22 118.9(6) . . ? C23 C24 C25 119.8(7) . . ? N3 C25 C24 121.2(5) . . ? N3 C25 C26 119.2(4) . . ? C24 C25 C26 119.6(5) . . ? C25 C26 C27 117.6(4) . . ? O2 C27 C28 110.5(4) . . ? O2 C27 C26 107.8(4) . . ? C28 C27 C26 110.3(4) . . ? O2 C27 C36 110.4(4) . . ? C28 C27 C36 110.5(4) . . ? C26 C27 C36 107.3(4) . . ? C29 C28 C27 117.2(4) . . ? N4 C29 C30 122.0(5) . . ? N4 C29 C28 115.1(5) . . ? C30 C29 C28 122.8(5) . . ? C31 C30 C29 118.9(6) . . ? C32 C31 C30 118.4(6) . . ? C33 C32 C31 119.8(5) . . ? N4 C33 C32 122.6(6) . . ? N4 C33 C35 116.1(6) . . ? C32 C33 C35 121.4(6) . . ? C38 C36 C37 106.9(5) . . ? C38 C36 C39 109.0(6) . . ? C37 C36 C39 107.6(5) . . ? C38 C36 C27 110.4(5) . . ? C37 C36 C27 110.7(5) . . ? C39 C36 C27 112.1(4) . . ? N40 C41 C42 178.6(14) . . ? _refine_diff_density_max 0.357 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.070 #===END