# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 186/1346
 
data_VG9741 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C46 H64 N2 O2 Cr' 
_chemical_formula_weight          728.99 
_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    I2/a 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y, -z' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y, z' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x, -y+1/2, z+1/2' 
  
_cell_length_a                    13.645(5) 
_cell_length_b                    18.382(4) 
_cell_length_c                    17.243(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  102.73(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      4218.8(25) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     203(2) 
_cell_measurement_reflns_used     21 
_cell_measurement_theta_min       4.92 
_cell_measurement_theta_max       12.54 
  
_exptl_crystal_description        blocks 
_exptl_crystal_colour             Red 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.43 
_exptl_crystal_size_min           0.37 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.148 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1576 
_exptl_absorpt_coefficient_mu     0.308 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       203(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         9.17 
_diffrn_reflns_number             3778 
_diffrn_reflns_av_R_equivalents   0.0343 
_diffrn_reflns_av_sigmaI/netI     0.0906 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.89 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3669 
_reflns_number_observed           2158 
_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^)+(0.0626P)^2^+0.2976P] 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          3669 
_refine_ls_number_parameters      235 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.1238 
_refine_ls_R_factor_obs           0.0603 
_refine_ls_wR_factor_all          0.1580 
_refine_ls_wR_factor_obs          0.1253 
_refine_ls_goodness_of_fit_all    1.041 
_refine_ls_goodness_of_fit_obs    1.097 
_refine_ls_restrained_S_all       1.041 
_refine_ls_restrained_S_obs       1.097 
_refine_ls_shift/esd_max          0.001 
_refine_ls_shift/esd_mean         0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Cr Cr 0.2500 0.04531(5) 0.5000 0.0440(3) Uani 1 d S . 
N N 0.3609(2) 0.1259(2) 0.5305(2) 0.0312(7) Uani 1 d D . 
H H 0.3470(35) 0.1482(24) 0.5733(17) 0.052(15) Uiso 1 d D . 
O O 0.3452(2) -0.02770(13) 0.5458(2) 0.0379(7) Uani 1 d . . 
C1 C 0.4617(3) 0.0974(2) 0.5631(3) 0.0484(12) Uani 1 d . . 
H1A H 0.5073(3) 0.1381(2) 0.5812(3) 0.058 Uiso 1 calc R . 
H1B H 0.4858(3) 0.0720(2) 0.5209(3) 0.058 Uiso 1 calc R . 
C2 C 0.4647(3) 0.0463(2) 0.6308(2) 0.0329(8) Uani 1 d . . 
C3 C 0.4085(3) -0.0186(2) 0.6161(2) 0.0305(8) Uani 1 d . . 
C4 C 0.4197(3) -0.0720(2) 0.6767(2) 0.0318(8) Uani 1 d . . 
C5 C 0.4841(3) -0.0555(2) 0.7492(2) 0.0325(8) Uani 1 d . . 
H5A H 0.4926(3) -0.0908(2) 0.7895(2) 0.039 Uiso 1 calc R . 
C6 C 0.5369(3) 0.0098(2) 0.7662(2) 0.0329(8) Uani 1 d . . 
C7 C 0.5261(3) 0.0604(2) 0.7060(2) 0.0311(8) Uani 1 d . . 
H7A H 0.5604(3) 0.1050(2) 0.7153(2) 0.037 Uiso 1 calc R . 
C8 C 0.3604(3) -0.1436(2) 0.6620(3) 0.0336(9) Uani 1 d . . 
C9 C 0.2472(3) -0.1263(2) 0.6486(3) 0.0490(12) Uani 1 d . . 
H9A H 0.2343(3) -0.1008(2) 0.6945(3) 0.073 Uiso 1 calc R . 
H9B H 0.2091(3) -0.1713(2) 0.6410(3) 0.073 Uiso 1 calc R . 
H9C H 0.2271(3) -0.0960(2) 0.6017(3) 0.073 Uiso 1 calc R . 
C10 C 0.3803(3) -0.1840(2) 0.5892(3) 0.0405(10) Uani 1 d . . 
H10A H 0.3640(3) -0.1525(2) 0.5430(3) 0.061 Uiso 1 calc R . 
H10B H 0.3390(3) -0.2274(2) 0.5797(3) 0.061 Uiso 1 calc R . 
H10C H 0.4506(3) -0.1976(2) 0.5987(3) 0.061 Uiso 1 calc R . 
C11 C 0.3872(4) -0.1955(2) 0.7332(3) 0.0491(12) Uani 1 d . . 
H11A H 0.3753(4) -0.1714(2) 0.7804(3) 0.074 Uiso 1 calc R . 
H11B H 0.4575(4) -0.2090(2) 0.7417(3) 0.074 Uiso 1 calc R . 
H11C H 0.3458(4) -0.2388(2) 0.7227(3) 0.074 Uiso 1 calc R . 
C12 C 0.6052(3) 0.0225(2) 0.8488(2) 0.0400(10) Uani 1 d . . 
C13 C 0.6971(4) -0.0271(3) 0.8589(3) 0.0550(13) Uani 1 d . . 
H13A H 0.7332(4) -0.0165(3) 0.8176(3) 0.083 Uiso 1 calc R . 
H13B H 0.6755(4) -0.0775(3) 0.8548(3) 0.083 Uiso 1 calc R . 
H13C H 0.7409(4) -0.0188(3) 0.9106(3) 0.083 Uiso 1 calc R . 
C14 C 0.5487(4) 0.0055(3) 0.9140(3) 0.0582(13) Uani 1 d . . 
H14A H 0.4904(4) 0.0369(3) 0.9079(3) 0.087 Uiso 1 calc R . 
H14B H 0.5927(4) 0.0138(3) 0.9657(3) 0.087 Uiso 1 calc R . 
H14C H 0.5273(4) -0.0449(3) 0.9098(3) 0.087 Uiso 1 calc R . 
C15 C 0.6404(4) 0.1018(3) 0.8610(3) 0.0609(15) Uani 1 d . . 
H15A H 0.6768(4) 0.1150(3) 0.8206(3) 0.091 Uiso 1 calc R . 
H15B H 0.6842(4) 0.1072(3) 0.9132(3) 0.091 Uiso 1 calc R . 
H15C H 0.5825(4) 0.1334(3) 0.8568(3) 0.091 Uiso 1 calc R . 
C16 C 0.3594(3) 0.1805(2) 0.4702(2) 0.0301(8) Uani 1 d . . 
C17 C 0.3797(3) 0.2532(2) 0.4916(3) 0.0470(12) Uani 1 d . . 
C18 C 0.3778(4) 0.3027(3) 0.4301(4) 0.072(2) Uani 1 d . . 
H18A H 0.3905(4) 0.3521(3) 0.4425(4) 0.086 Uiso 1 calc R . 
C19 C 0.3581(4) 0.2814(4) 0.3525(4) 0.079(2) Uani 1 d . . 
H19A H 0.3583(4) 0.3159(4) 0.3122(4) 0.095 Uiso 1 calc R . 
C20 C 0.3377(4) 0.2089(4) 0.3328(3) 0.066(2) Uani 1 d . . 
H20A H 0.3236(4) 0.1948(4) 0.2791(3) 0.079 Uiso 1 calc R . 
C21 C 0.3379(3) 0.1574(2) 0.3912(2) 0.0374(9) Uani 1 d . . 
C22 C 0.4008(5) 0.2783(3) 0.5769(4) 0.081(2) Uani 1 d . . 
H22A H 0.4165(5) 0.3298(3) 0.5794(4) 0.121 Uiso 1 d R . 
H22B H 0.4575(5) 0.2513(3) 0.6076(4) 0.121 Uiso 1 d R . 
H22C H 0.3421(5) 0.2698(3) 0.5988(4) 0.121 Uiso 1 d R . 
C23 C 0.3153(4) 0.0796(3) 0.3722(4) 0.072(2) Uani 1 d . . 
H23A H 0.2431(4) 0.0728(3) 0.3566(4) 0.109 Uiso 1 d R . 
H23B H 0.3422(4) 0.0501(3) 0.4186(4) 0.109 Uiso 1 d R . 
H23C H 0.3457(4) 0.0649(3) 0.3288(4) 0.109 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 0.0331(5) 0.0219(4) 0.0614(7) 0.000 -0.0230(4) 0.000 
N 0.027(2) 0.029(2) 0.035(2) 0.0052(14) 0.0010(13) 0.0019(12) 
O 0.0357(15) 0.0279(14) 0.041(2) 0.0053(11) -0.0111(12) 0.0000(10) 
C1 0.032(2) 0.046(2) 0.057(3) 0.020(2) -0.012(2) -0.009(2) 
C2 0.026(2) 0.032(2) 0.036(2) 0.011(2) -0.0031(15) -0.002(2) 
C3 0.021(2) 0.029(2) 0.038(2) 0.006(2) -0.0013(15) 0.0019(13) 
C4 0.023(2) 0.030(2) 0.042(2) 0.005(2) 0.0058(15) 0.0023(14) 
C5 0.032(2) 0.031(2) 0.033(2) 0.005(2) 0.0051(15) 0.0051(15) 
C6 0.032(2) 0.034(2) 0.031(2) 0.003(2) 0.004(2) 0.004(2) 
C7 0.025(2) 0.027(2) 0.038(2) 0.003(2) 0.0002(15) -0.0020(13) 
C8 0.029(2) 0.028(2) 0.043(2) 0.007(2) 0.007(2) -0.0014(14) 
C9 0.031(2) 0.041(2) 0.074(3) 0.001(2) 0.012(2) -0.005(2) 
C10 0.038(2) 0.030(2) 0.051(3) 0.004(2) 0.003(2) 0.000(2) 
C11 0.056(3) 0.032(2) 0.055(3) 0.013(2) 0.004(2) -0.006(2) 
C12 0.049(2) 0.037(2) 0.029(2) 0.004(2) -0.002(2) 0.002(2) 
C13 0.047(3) 0.072(3) 0.037(2) -0.002(2) -0.011(2) 0.005(2) 
C14 0.085(4) 0.053(3) 0.037(3) 0.000(2) 0.014(2) -0.002(3) 
C15 0.087(4) 0.048(3) 0.039(3) -0.006(2) -0.006(3) -0.017(3) 
C16 0.027(2) 0.027(2) 0.033(2) 0.006(2) -0.0004(15) -0.0042(13) 
C17 0.037(2) 0.031(2) 0.064(3) 0.003(2) -0.010(2) -0.003(2) 
C18 0.051(3) 0.039(3) 0.115(5) 0.032(3) -0.006(3) -0.006(2) 
C19 0.046(3) 0.085(4) 0.100(5) 0.064(4) 0.005(3) 0.001(3) 
C20 0.041(3) 0.118(5) 0.037(3) 0.032(3) 0.004(2) 0.017(3) 
C21 0.022(2) 0.055(2) 0.033(2) 0.001(2) 0.0007(15) 0.008(2) 
C22 0.083(4) 0.050(3) 0.088(5) -0.034(3) -0.025(3) 0.006(3) 
C23 0.051(3) 0.069(3) 0.083(4) -0.046(3) -0.018(3) 0.015(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 O 1.913(3) 2_556 ? 
Cr O 1.913(3) . ? 
Cr N 2.100(3) . ? 
Cr N 2.100(3) 2_556 ? 
N C16 1.444(5) . ? 
N C1 1.463(5) . ? 
O C3 1.336(4) . ? 
C1 C2 1.492(6) . ? 
C2 C7 1.404(5) . ? 
C2 C3 1.410(5) . ? 
C3 C4 1.417(5) . ? 
C4 C5 1.394(5) . ? 
C4 C8 1.538(5) . ? 
C5 C6 1.397(5) . ? 
C6 C7 1.378(5) . ? 
C6 C12 1.539(5) . ? 
C8 C10 1.533(6) . ? 
C8 C11 1.535(5) . ? 
C8 C9 1.543(5) . ? 
C12 C14 1.529(7) . ? 
C12 C13 1.530(6) . ? 
C12 C15 1.534(6) . ? 
C16 C21 1.396(6) . ? 
C16 C17 1.398(5) . ? 
C17 C18 1.393(7) . ? 
C17 C22 1.508(8) . ? 
C18 C19 1.364(10) . ? 
C19 C20 1.387(9) . ? 
C20 C21 1.382(7) . ? 
C21 C23 1.484(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 
O Cr O 90.9(2) 2_556 . ? 
O Cr N 169.93(14) 2_556 . ? 
O Cr N 90.28(11) . . ? 
O Cr N 90.28(11) 2_556 2_556 ? 
O Cr N 169.93(14) . 2_556 ? 
N Cr N 90.3(2) . 2_556 ? 
C16 N C1 112.9(3) . . ? 
C16 N Cr 114.5(2) . . ? 
C1 N Cr 114.1(2) . . ? 
C3 O Cr 122.1(2) . . ? 
N C1 C2 112.8(4) . . ? 
C7 C2 C3 120.8(3) . . ? 
C7 C2 C1 120.9(3) . . ? 
C3 C2 C1 118.1(3) . . ? 
O C3 C2 119.1(3) . . ? 
O C3 C4 121.7(3) . . ? 
C2 C3 C4 119.2(3) . . ? 
C5 C4 C3 117.0(3) . . ? 
C5 C4 C8 122.6(3) . . ? 
C3 C4 C8 120.3(3) . . ? 
C4 C5 C6 124.7(4) . . ? 
C7 C6 C5 117.2(3) . . ? 
C7 C6 C12 122.5(3) . . ? 
C5 C6 C12 120.3(3) . . ? 
C6 C7 C2 120.9(3) . . ? 
C10 C8 C11 107.5(3) . . ? 
C10 C8 C4 111.5(3) . . ? 
C11 C8 C4 112.1(3) . . ? 
C10 C8 C9 109.2(3) . . ? 
C11 C8 C9 107.6(4) . . ? 
C4 C8 C9 108.8(3) . . ? 
C14 C12 C13 109.1(4) . . ? 
C14 C12 C15 106.7(4) . . ? 
C13 C12 C15 109.1(4) . . ? 
C14 C12 C6 110.4(4) . . ? 
C13 C12 C6 109.1(3) . . ? 
C15 C12 C6 112.3(3) . . ? 
C21 C16 C17 122.4(4) . . ? 
C21 C16 N 117.3(3) . . ? 
C17 C16 N 120.3(4) . . ? 
C18 C17 C16 117.0(5) . . ? 
C18 C17 C22 120.7(5) . . ? 
C16 C17 C22 122.2(4) . . ? 
C19 C18 C17 121.7(5) . . ? 
C18 C19 C20 120.1(5) . . ? 
C21 C20 C19 120.9(5) . . ? 
C20 C21 C16 117.9(5) . . ? 
C20 C21 C23 122.3(5) . . ? 
C16 C21 C23 119.9(4) . . ? 
  
_refine_diff_density_max    0.330 
_refine_diff_density_min   -0.345 
_refine_diff_density_rms    0.056 
  
 
data_VG9821 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C27 H38 N3 O Cl2 Cr' 
_chemical_formula_weight          543.50 
_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' 
 'Cl'  'Cl'   0.3639   0.7018 
 '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                    9.5664(14) 
_cell_length_b                    13.048(2) 
_cell_length_c                    23.432(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.832(13) 
_cell_angle_gamma                 90.00 
_cell_volume                      2909.7(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     27 
_cell_measurement_theta_min       5.76 
_cell_measurement_theta_max       22.44 
  
_exptl_crystal_description        plates 
_exptl_crystal_colour             Green 
_exptl_crystal_size_max           0.27 
_exptl_crystal_size_mid           0.27 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.241 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1148 
_exptl_absorpt_coefficient_mu     5.094 
_exptl_absorpt_correction_type    Ellipsoidal 
_exptl_absorpt_correction_T_min   0.3736 
_exptl_absorpt_correction_T_max   0.5922 
  
_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             4755 
_diffrn_reflns_av_R_equivalents   0.0601 
_diffrn_reflns_av_sigmaI/netI     0.0760 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          3.79 
_diffrn_reflns_theta_max          63.96 
_reflns_number_total              4438 
_reflns_number_observed           3139 
_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 372 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^)+(0.0689P)^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        0.00057(11) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          4066 
_refine_ls_number_parameters      324 
_refine_ls_number_restraints      31 
_refine_ls_R_factor_all           0.0910 
_refine_ls_R_factor_obs           0.0565 
_refine_ls_wR_factor_all          0.1464 
_refine_ls_wR_factor_obs          0.1267 
_refine_ls_goodness_of_fit_all    1.018 
_refine_ls_goodness_of_fit_obs    1.087 
_refine_ls_restrained_S_all       1.046 
_refine_ls_restrained_S_obs       1.089 
_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 0.50620(8) 0.07116(5) 0.20124(3) 0.0322(2) Uani 1 d . . 
Cl1 Cl 0.30975(14) 0.04737(9) 0.24952(6) 0.0528(3) Uani 1 d . . 
Cl2 Cl 0.71566(13) 0.10262(9) 0.16148(5) 0.0480(3) Uani 1 d . . 
O1 O 0.4924(3) -0.0596(2) 0.16900(13) 0.0388(7) Uani 1 d . . 
N1 N 0.3966(4) 0.1135(2) 0.12138(15) 0.0318(8) Uani 1 d D . 
H1 H 0.4613(39) 0.0795(35) 0.1034(19) 0.039(13) Uiso 1 d D . 
N2 N 0.5235(5) 0.2179(3) 0.2383(2) 0.0437(9) Uani 1 d . . 
N3 N 0.6230(5) 0.0085(3) 0.2736(2) 0.0453(10) Uani 1 d . . 
C1 C 0.3850(5) -0.1080(3) 0.1391(2) 0.0297(9) Uani 1 d . . 
C2 C 0.3884(4) -0.2174(3) 0.1368(2) 0.0268(8) Uani 1 d . . 
C3 C 0.2772(5) -0.2668(3) 0.1056(2) 0.0328(9) Uani 1 d . . 
H3A H 0.2789(5) -0.3380(3) 0.1039(2) 0.039 Uiso 1 calc R . 
C4 C 0.1631(5) -0.2162(3) 0.0765(2) 0.0342(9) Uani 1 d . . 
C5 C 0.1650(5) -0.1099(3) 0.0778(2) 0.0343(9) Uani 1 d . . 
H5A H 0.0925(5) -0.0738(3) 0.0573(2) 0.041 Uiso 1 calc R . 
C6 C 0.2733(5) -0.0554(3) 0.1091(2) 0.0324(9) Uani 1 d . . 
C7 C 0.2598(5) 0.0597(3) 0.1097(2) 0.0436(11) Uani 1 d . . 
H7A H 0.2148(5) 0.0821(3) 0.0729(2) 0.052 Uiso 1 calc R . 
H7B H 0.1995(5) 0.0790(3) 0.1388(2) 0.052 Uiso 1 calc R . 
C8 C 0.3944(5) 0.2170(3) 0.0967(2) 0.0332(9) Uani 1 d . . 
C9 C 0.3143(5) 0.2958(3) 0.1178(2) 0.0379(10) Uani 1 d . . 
C10 C 0.3170(6) 0.3912(3) 0.0914(2) 0.0519(14) Uani 1 d . . 
H10A H 0.2673(6) 0.4453(3) 0.1055(2) 0.062 Uiso 1 calc R . 
C11 C 0.3917(7) 0.4074(3) 0.0450(2) 0.0566(15) Uani 1 d . . 
H11A H 0.3912(7) 0.4718(3) 0.0279(2) 0.068 Uiso 1 calc R . 
C12 C 0.4671(6) 0.3289(4) 0.0237(2) 0.0512(13) Uani 1 d . . 
H12A H 0.5176(6) 0.3409(4) -0.0075(2) 0.061 Uiso 1 calc R . 
C13 C 0.4687(5) 0.2317(3) 0.0482(2) 0.0404(11) Uani 1 d . . 
C14 C 0.5122(5) -0.2763(3) 0.1678(2) 0.0337(9) Uani 1 d . . 
C15 C 0.6504(5) -0.2444(4) 0.1450(3) 0.0520(13) Uani 1 d . . 
H15A H 0.6444(5) -0.2563(4) 0.1044(3) 0.078 Uiso 1 calc R . 
H15B H 0.7262(5) -0.2840(4) 0.1638(3) 0.078 Uiso 1 calc R . 
H15C H 0.6673(5) -0.1730(4) 0.1527(3) 0.078 Uiso 1 calc R . 
C16 C 0.5156(7) -0.2590(4) 0.2325(2) 0.0518(14) Uani 1 d . . 
H16A H 0.5932(7) -0.2960(4) 0.2519(2) 0.078 Uiso 1 calc R . 
H16B H 0.4294(7) -0.2831(4) 0.2455(2) 0.078 Uiso 1 calc R . 
H16C H 0.5263(7) -0.1872(4) 0.2407(2) 0.078 Uiso 1 calc R . 
C17 C 0.4970(6) -0.3928(3) 0.1583(2) 0.0523(14) Uani 1 d . . 
H17A H 0.4944(6) -0.4077(3) 0.1181(2) 0.078 Uiso 1 calc R . 
H17B H 0.4116(6) -0.4160(3) 0.1723(2) 0.078 Uiso 1 calc R . 
H17C H 0.5756(6) -0.4272(3) 0.1786(2) 0.078 Uiso 1 calc R . 
C18 C 0.0439(5) -0.2765(4) 0.0424(2) 0.0501(13) Uani 1 d D . 
C19 C 0.1008(10) -0.3343(8) -0.0055(4) 0.099(4) Uani 0.85 d PD 1 
H19A H 0.1797(10) -0.3749(8) 0.0096(4) 0.148 Uiso 0.85 calc PR 1 
H19B H 0.1301(10) -0.2867(8) -0.0332(4) 0.148 Uiso 0.85 calc PR 1 
H19C H 0.0290(10) -0.3783(8) -0.0236(4) 0.148 Uiso 0.85 calc PR 1 
C20 C -0.0123(7) -0.3595(5) 0.0826(4) 0.068(2) Uani 0.85 d PD 1 
H20A H 0.0633(7) -0.4042(5) 0.0967(4) 0.101 Uiso 0.85 calc PR 1 
H20B H -0.0849(7) -0.3988(5) 0.0615(4) 0.101 Uiso 0.85 calc PR 1 
H20C H -0.0496(7) -0.3265(5) 0.1144(4) 0.101 Uiso 0.85 calc PR 1 
C21 C -0.0796(8) -0.2111(5) 0.0227(4) 0.077(3) Uani 0.85 d PD 1 
H21A H -0.1115(8) -0.1761(5) 0.0550(4) 0.115 Uiso 0.85 calc PR 1 
H21B H -0.1539(8) -0.2533(5) 0.0050(4) 0.115 Uiso 0.85 calc PR 1 
H21C H -0.0529(8) -0.1617(5) -0.0046(4) 0.115 Uiso 0.85 calc PR 1 
C19' C 0.0595(79) -0.2440(45) -0.0212(15) 0.124(23) Uiso 0.15 d PD 2 
H19D H 0.0469(79) -0.1713(45) -0.0251(15) 0.185 Uiso 0.15 calc PR 2 
H19E H -0.0103(79) -0.2786(45) -0.0466(15) 0.185 Uiso 0.15 calc PR 2 
H19F H 0.1514(79) -0.2623(45) -0.0309(15) 0.185 Uiso 0.15 calc PR 2 
C20' C 0.0655(60) -0.3916(18) 0.0439(22) 0.088(14) Uiso 0.15 d PD 2 
H20D H 0.1611(60) -0.4070(18) 0.0381(22) 0.132 Uiso 0.15 calc PR 2 
H20E H 0.0037(60) -0.4230(18) 0.0141(22) 0.132 Uiso 0.15 calc PR 2 
H20F H 0.0452(60) -0.4177(18) 0.0805(22) 0.132 Uiso 0.15 calc PR 2 
C21' C -0.1075(48) -0.2524(57) 0.0515(38) 0.240(73) Uiso 0.15 d PD 2 
H21D H -0.1214(48) -0.1796(57) 0.0506(38) 0.360 Uiso 0.15 calc PR 2 
H21E H -0.1277(48) -0.2786(57) 0.0881(38) 0.360 Uiso 0.15 calc PR 2 
H21F H -0.1692(48) -0.2839(57) 0.0217(38) 0.360 Uiso 0.15 calc PR 2 
C22 C 0.2220(6) 0.2825(4) 0.1652(2) 0.0490(12) Uani 1 d . . 
H22A H 0.2589(6) 0.2288(4) 0.1904(2) 0.073 Uiso 1 d R . 
H22B H 0.1288(6) 0.2647(4) 0.1492(2) 0.073 Uiso 1 d R . 
H22C H 0.2192(6) 0.3453(4) 0.1864(2) 0.073 Uiso 1 d R . 
C23 C 0.5427(7) 0.1460(4) 0.0207(2) 0.0570(14) Uani 1 d . . 
H23A H 0.4766(7) 0.0926(4) 0.0094(2) 0.085 Uiso 1 d R . 
H23B H 0.6159(7) 0.1192(4) 0.0476(2) 0.085 Uiso 1 d R . 
H23C H 0.5828(7) 0.1715(4) -0.0124(2) 0.085 Uiso 1 d R . 
C24 C 0.5211(6) 0.2949(3) 0.2603(2) 0.0419(11) Uani 1 d . . 
C25 C 0.5136(7) 0.3930(4) 0.2887(3) 0.063(2) Uani 1 d . . 
H25A H 0.4497(7) 0.4370(4) 0.2659(3) 0.094 Uiso 1 d R . 
H25B H 0.6052(7) 0.4238(4) 0.2932(3) 0.094 Uiso 1 d R . 
H25C H 0.4810(7) 0.3832(4) 0.3257(3) 0.094 Uiso 1 d R . 
C26 C 0.6746(6) -0.0409(4) 0.3092(2) 0.0458(12) Uani 1 d . . 
C27 C 0.7409(8) -0.1063(5) 0.3546(3) 0.076(2) Uani 1 d . . 
H27A H 0.7287(8) -0.0767(5) 0.3913(3) 0.113 Uiso 1 d R . 
H27B H 0.8394(8) -0.1124(5) 0.3505(3) 0.113 Uiso 1 d R . 
H27C H 0.6984(8) -0.1730(5) 0.3520(3) 0.113 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 0.0344(4) 0.0237(3) 0.0360(4) 0.0008(3) -0.0096(3) -0.0032(3) 
Cl1 0.0491(7) 0.0504(6) 0.0593(7) 0.0134(5) 0.0076(6) 0.0001(5) 
Cl2 0.0372(6) 0.0475(6) 0.0576(7) -0.0001(5) -0.0037(5) -0.0071(5) 
O1 0.035(2) 0.0264(13) 0.050(2) 0.0000(12) -0.0181(14) -0.0018(13) 
N1 0.038(2) 0.021(2) 0.034(2) 0.0071(13) -0.004(2) 0.0011(15) 
N2 0.050(2) 0.034(2) 0.045(2) -0.001(2) -0.007(2) 0.000(2) 
N3 0.049(3) 0.038(2) 0.046(2) 0.000(2) -0.011(2) -0.007(2) 
C1 0.027(2) 0.024(2) 0.036(2) -0.0011(15) -0.008(2) -0.003(2) 
C2 0.029(2) 0.018(2) 0.032(2) 0.0017(14) -0.007(2) -0.001(2) 
C3 0.033(2) 0.025(2) 0.039(2) -0.004(2) -0.002(2) 0.001(2) 
C4 0.028(2) 0.032(2) 0.040(2) -0.004(2) -0.011(2) -0.003(2) 
C5 0.031(2) 0.030(2) 0.039(2) 0.004(2) -0.012(2) 0.000(2) 
C6 0.035(2) 0.023(2) 0.037(2) 0.0010(15) -0.008(2) -0.001(2) 
C7 0.044(3) 0.024(2) 0.058(3) 0.003(2) -0.018(2) -0.001(2) 
C8 0.038(2) 0.019(2) 0.040(2) 0.0041(15) -0.009(2) -0.005(2) 
C9 0.042(3) 0.029(2) 0.040(2) 0.002(2) -0.007(2) 0.000(2) 
C10 0.059(3) 0.023(2) 0.069(3) 0.001(2) -0.013(3) -0.002(2) 
C11 0.078(4) 0.028(2) 0.061(3) 0.012(2) -0.008(3) -0.010(2) 
C12 0.065(4) 0.043(2) 0.046(3) 0.009(2) 0.004(2) -0.013(2) 
C13 0.047(3) 0.034(2) 0.038(2) 0.000(2) -0.001(2) -0.005(2) 
C14 0.031(2) 0.026(2) 0.042(2) 0.000(2) -0.006(2) 0.005(2) 
C15 0.029(3) 0.049(3) 0.076(3) 0.000(2) -0.003(2) 0.006(2) 
C16 0.074(4) 0.040(2) 0.037(2) 0.003(2) -0.014(2) 0.008(2) 
C17 0.054(3) 0.028(2) 0.071(3) -0.005(2) -0.014(3) 0.008(2) 
C18 0.039(3) 0.042(2) 0.065(3) -0.013(2) -0.015(2) -0.007(2) 
C19 0.074(6) 0.132(8) 0.088(6) -0.078(6) -0.004(5) -0.025(6) 
C20 0.039(4) 0.054(4) 0.104(6) 0.012(4) -0.018(4) -0.017(3) 
C21 0.048(4) 0.049(3) 0.122(7) 0.002(4) -0.046(5) -0.004(3) 
C22 0.050(3) 0.037(2) 0.059(3) -0.006(2) 0.002(2) 0.009(2) 
C23 0.077(4) 0.049(3) 0.047(3) -0.002(2) 0.011(3) 0.004(3) 
C24 0.053(3) 0.032(2) 0.039(2) -0.004(2) -0.004(2) 0.001(2) 
C25 0.074(4) 0.042(3) 0.071(4) -0.019(2) 0.000(3) 0.009(3) 
C26 0.056(3) 0.041(2) 0.037(2) 0.004(2) -0.012(2) -0.014(2) 
C27 0.090(5) 0.068(4) 0.063(4) 0.027(3) -0.021(4) -0.010(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 O1 1.865(3) . ? 
Cr N3 2.100(4) . ? 
Cr N2 2.102(4) . ? 
Cr N1 2.123(3) . ? 
Cr Cl1 2.311(2) . ? 
Cr Cl2 2.330(2) . ? 
O1 C1 1.341(5) . ? 
N1 C8 1.468(5) . ? 
N1 C7 1.486(6) . ? 
N2 C24 1.131(6) . ? 
N3 C26 1.128(6) . ? 
C1 C6 1.397(6) . ? 
C1 C2 1.429(5) . ? 
C2 C3 1.388(6) . ? 
C2 C14 1.531(5) . ? 
C3 C4 1.393(6) . ? 
C4 C5 1.388(6) . ? 
C4 C18 1.540(6) . ? 
C5 C6 1.401(6) . ? 
C6 C7 1.508(5) . ? 
C8 C9 1.402(7) . ? 
C8 C13 1.414(7) . ? 
C9 C10 1.391(6) . ? 
C9 C22 1.498(7) . ? 
C10 C11 1.378(9) . ? 
C11 C12 1.376(8) . ? 
C12 C13 1.393(7) . ? 
C13 C23 1.503(7) . ? 
C14 C16 1.530(6) . ? 
C14 C15 1.533(7) . ? 
C14 C17 1.541(6) . ? 
C18 C21 1.492(8) . ? 
C18 C19 1.500(9) . ? 
C18 C20' 1.52(2) . ? 
C18 C21' 1.52(2) . ? 
C18 C20 1.567(8) . ? 
C18 C19' 1.57(2) . ? 
C24 C25 1.446(6) . ? 
C26 C27 1.458(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 
O1 Cr N3 88.91(14) . . ? 
O1 Cr N2 179.33(14) . . ? 
N3 Cr N2 90.43(15) . . ? 
O1 Cr N1 82.69(12) . . ? 
N3 Cr N1 171.10(15) . . ? 
N2 Cr N1 97.96(14) . . ? 
O1 Cr Cl1 92.74(12) . . ? 
N3 Cr Cl1 86.83(14) . . ? 
N2 Cr Cl1 87.35(14) . . ? 
N1 Cr Cl1 96.49(12) . . ? 
O1 Cr Cl2 91.57(12) . . ? 
N3 Cr Cl2 89.02(13) . . ? 
N2 Cr Cl2 88.29(13) . . ? 
N1 Cr Cl2 88.25(12) . . ? 
Cl1 Cr Cl2 173.95(5) . . ? 
C1 O1 Cr 131.4(3) . . ? 
C8 N1 C7 112.7(3) . . ? 
C8 N1 Cr 124.9(2) . . ? 
C7 N1 Cr 112.7(3) . . ? 
C24 N2 Cr 173.5(5) . . ? 
C26 N3 Cr 167.7(4) . . ? 
O1 C1 C6 122.6(3) . . ? 
O1 C1 C2 118.0(3) . . ? 
C6 C1 C2 119.4(4) . . ? 
C3 C2 C1 117.6(4) . . ? 
C3 C2 C14 122.1(3) . . ? 
C1 C2 C14 120.2(3) . . ? 
C2 C3 C4 124.0(4) . . ? 
C5 C4 C3 117.0(4) . . ? 
C5 C4 C18 122.0(4) . . ? 
C3 C4 C18 120.9(4) . . ? 
C4 C5 C6 121.7(4) . . ? 
C1 C6 C5 120.1(3) . . ? 
C1 C6 C7 123.1(4) . . ? 
C5 C6 C7 116.8(4) . . ? 
N1 C7 C6 113.5(4) . . ? 
C9 C8 C13 121.4(4) . . ? 
C9 C8 N1 121.5(4) . . ? 
C13 C8 N1 116.9(4) . . ? 
C10 C9 C8 117.7(5) . . ? 
C10 C9 C22 118.2(5) . . ? 
C8 C9 C22 124.1(4) . . ? 
C11 C10 C9 121.5(5) . . ? 
C12 C11 C10 120.4(4) . . ? 
C11 C12 C13 120.8(5) . . ? 
C12 C13 C8 118.1(5) . . ? 
C12 C13 C23 119.1(5) . . ? 
C8 C13 C23 122.8(4) . . ? 
C16 C14 C2 109.5(4) . . ? 
C16 C14 C15 111.8(4) . . ? 
C2 C14 C15 110.6(4) . . ? 
C16 C14 C17 106.3(4) . . ? 
C2 C14 C17 111.7(3) . . ? 
C15 C14 C17 106.8(4) . . ? 
C21 C18 C19 113.1(6) . . ? 
C20' C18 C21' 109.4(22) . . ? 
C21 C18 C4 112.9(4) . . ? 
C19 C18 C4 109.8(5) . . ? 
C20' C18 C4 113.7(22) . . ? 
C21' C18 C4 119.2(38) . . ? 
C21 C18 C20 105.8(6) . . ? 
C19 C18 C20 106.0(6) . . ? 
C4 C18 C20 108.8(4) . . ? 
C20' C18 C19' 105.3(19) . . ? 
C21' C18 C19' 105.2(21) . . ? 
C4 C18 C19' 102.6(27) . . ? 
N2 C24 C25 178.3(6) . . ? 
N3 C26 C27 179.1(5) . . ? 
  
_refine_diff_density_max    0.438 
_refine_diff_density_min   -0.477 
_refine_diff_density_rms    0.064