 
data_12feb05a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H30 Cl4 N4 O2 U' 
_chemical_formula_weight          690.27 
 
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' 
 'U'  'U'  -9.6767   9.6646 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'P 2(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                    8.5021(2) 
_cell_length_b                    17.4789(3) 
_cell_length_c                    10.3866(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  125.2340(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      1260.75(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     9124
_cell_measurement_theta_min       3.395
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        'thin plate' 
_exptl_crystal_colour             'yellow' 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.818 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              660 
_exptl_absorpt_coefficient_mu     6.878 
_exptl_absorpt_correction_type    'integration' 
_exptl_absorpt_correction_T_min   0.316
_exptl_absorpt_correction_T_max   0.721
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;

loop_
_exptl_crystal_face_index_h 
_exptl_crystal_face_index_k 
_exptl_crystal_face_index_l 
_exptl_crystal_face_perp_dist 
    1    0    0  0.135
   -1    0    0  0.060
    0    0    1  0.095
    0    0   -1  0.085
    0    1    0  0.023
    0   -1    0  0.023
    4    0   -7  0.095
 
_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_type   'NONIUS KappaCCD' 
_diffrn_measurement_method        'CCD' 
_diffrn_detector_area_resol_mean  9 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             18214 
_diffrn_reflns_av_R_equivalents   0.0473 
_diffrn_reflns_av_sigmaI/netI     0.0327 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.42 
_diffrn_reflns_theta_max          27.50 
_reflns_number_total              2895 
_reflns_number_gt                 1967 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'KappaCCD (Nonius B. V., 1998)' 
_computing_cell_refinement        'HKL Scalepack (Otwinowski & Minor, 1997)' 
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL V5.1 (Sheldrick, 1998)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 

_publ_section_references
;
collect:
"Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998.

HKL Scalepack & HKL Denzo:
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet,
Eds., Academic Press.

absorption correction (Numerical):
P. Coppens, in Crystallographic Computing, edited by F. R. Ahmed,
S. R. Hall, C. P. Huber, pp255-270, 1970, Copenhagen: Munksgaard.

maXus: 
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland
"maXus: a computer program for the solution and refinement of crystal
structures from diffraction data", University of Glasgow, Scotland, UK,
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama,
Japan (1998).

Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen,
Germany.
;
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0325P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr. 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2895 
_refine_ls_number_parameters      124 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0474 
_refine_ls_R_factor_gt            0.0247 
_refine_ls_wR_factor_ref          0.0623 
_refine_ls_wR_factor_gt           0.0577 
_refine_ls_goodness_of_fit_ref    0.988 
_refine_ls_restrained_S_all       0.988 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
U1 U 0.0000 0.5000 0.0000 0.04702(8) Uani 1 2 d S . . 
Cl1 Cl 0.23524(16) 0.38125(6) 0.15077(12) 0.0780(3) Uani 1 1 d . . . 
Cl2 Cl -0.16565(17) 0.47573(8) 0.14968(14) 0.0746(3) Uani 1 1 d . . . 
O1 O 0.1720(3) 0.55895(14) 0.1544(2) 0.0612(6) Uani 1 1 d . . . 
N1 N 0.3138(5) 0.4466(2) 0.6030(4) 0.0658(9) Uani 1 1 d . . . 
N2 N 0.3844(5) 0.3542(2) 0.7649(4) 0.0672(9) Uani 1 1 d . . . 
C1 C 0.2999(10) 0.5229(3) 0.5413(7) 0.101(2) Uani 1 1 d . . . 
H1A H 0.2238 0.5211 0.4283 0.152 Uiso 1 1 calc R . . 
H1B H 0.4266 0.5414 0.5808 0.152 Uiso 1 1 calc R . . 
H1C H 0.2403 0.5568 0.5741 0.152 Uiso 1 1 calc R . . 
C2 C 0.2274(6) 0.3841(2) 0.5162(5) 0.0782(12) Uani 1 1 d . . . 
H2 H 0.1505 0.3815 0.4067 0.094 Uiso 1 1 calc R . . 
C3 C 0.2719(6) 0.3255(3) 0.6161(5) 0.0825(13) Uani 1 1 d . . . 
H3 H 0.2329 0.2749 0.5885 0.099 Uiso 1 1 calc R . . 
C4 C 0.4086(5) 0.4270(3) 0.7531(4) 0.0649(10) Uani 1 1 d . . . 
H4 H 0.4816 0.4602 0.8378 0.078 Uiso 1 1 calc R . . 
C5 C 0.4630(7) 0.3123(3) 0.9128(5) 0.0875(14) Uani 1 1 d . . . 
H5A H 0.3692 0.2751 0.8979 0.105 Uiso 1 1 calc R . . 
H5B H 0.4869 0.3479 0.9940 0.105 Uiso 1 1 calc R . . 
C6 C 0.6445(6) 0.2726(3) 0.9649(5) 0.0866(13) Uani 1 1 d . . . 
H6A H 0.7335 0.3089 0.9689 0.104 Uiso 1 1 calc R . . 
H6B H 0.6180 0.2333 0.8889 0.104 Uiso 1 1 calc R . . 
C7 C 0.7386(8) 0.2357(4) 1.1291(7) 0.139(2) Uani 1 1 d . . . 
H7A H 0.7218 0.2702 1.1935 0.167 Uiso 1 1 calc R . . 
H7B H 0.6697 0.1889 1.1164 0.167 Uiso 1 1 calc R . . 
C8 C 0.9264(10) 0.2191(4) 1.2072(8) 0.181(4) Uani 1 1 d . . . 
H8A H 0.9721 0.1982 1.3085 0.272 Uiso 1 1 calc R . . 
H8B H 0.9970 0.2649 1.2208 0.272 Uiso 1 1 calc R . . 
H8C H 0.9447 0.1825 1.1482 0.272 Uiso 1 1 calc R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
U1 0.05058(13) 0.04492(11) 0.04303(12) -0.00424(8) 0.02555(9) -0.00021(9) 
Cl1 0.0814(7) 0.0627(6) 0.0758(7) 0.0098(5) 0.0371(6) 0.0211(6) 
Cl2 0.0701(7) 0.1009(7) 0.0639(7) 0.0010(6) 0.0451(6) 0.0003(6) 
O1 0.0619(16) 0.0590(16) 0.0569(15) -0.0139(12) 0.0309(13) -0.0098(13) 
N1 0.057(2) 0.073(2) 0.054(2) 0.0038(17) 0.0245(18) 0.0040(17) 
N2 0.069(2) 0.077(2) 0.054(2) 0.0055(17) 0.0344(18) 0.0083(18) 
C1 0.107(5) 0.078(3) 0.087(4) 0.009(3) 0.038(4) -0.012(3) 
C2 0.085(3) 0.080(3) 0.050(2) -0.002(2) 0.028(2) -0.004(2) 
C3 0.096(3) 0.070(3) 0.057(3) -0.001(2) 0.031(3) -0.004(2) 
C4 0.052(2) 0.087(3) 0.052(2) -0.008(2) 0.027(2) 0.003(2) 
C5 0.090(3) 0.114(4) 0.057(3) 0.020(3) 0.042(3) 0.011(3) 
C6 0.077(3) 0.099(3) 0.068(3) 0.019(2) 0.032(3) -0.006(3) 
C7 0.094(4) 0.174(6) 0.136(5) 0.097(4) 0.058(4) 0.021(4) 
C8 0.088(4) 0.220(7) 0.149(6) 0.105(5) 0.018(4) -0.025(6) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
U1 O1 1.751(2) 3_565 ? 
U1 O1 1.751(2) . ? 
U1 Cl2 2.6659(11) . ? 
U1 Cl2 2.6659(11) 3_565 ? 
U1 Cl1 2.6733(10) . ? 
U1 Cl1 2.6733(10) 3_565 ? 
N1 C4 1.323(4) . ? 
N1 C2 1.335(5) . ? 
N1 C1 1.455(6) . ? 
N2 C4 1.306(5) . ? 
N2 C3 1.360(4) . ? 
N2 C5 1.469(4) . ? 
C1 H1A 0.9600 . ? 
C1 H1B 0.9600 . ? 
C1 H1C 0.9600 . ? 
C2 C3 1.349(5) . ? 
C2 H2 0.9300 . ? 
C3 H3 0.9300 . ? 
C4 H4 0.9300 . ? 
C5 C6 1.481(5) . ? 
C5 H5A 0.9700 . ? 
C5 H5B 0.9700 . ? 
C6 C7 1.546(5) . ? 
C6 H6A 0.9700 . ? 
C6 H6B 0.9700 . ? 
C7 C8 1.341(6) . ? 
C7 H7A 0.9700 . ? 
C7 H7B 0.9700 . ? 
C8 H8A 0.9600 . ? 
C8 H8B 0.9600 . ? 
C8 H8C 0.9600 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O1 U1 O1 180.00(13) 3_565 . ? 
O1 U1 Cl2 89.85(8) 3_565 . ? 
O1 U1 Cl2 90.15(8) . . ? 
O1 U1 Cl2 90.15(8) 3_565 3_565 ? 
O1 U1 Cl2 89.85(8) . 3_565 ? 
Cl2 U1 Cl2 180.00(6) . 3_565 ? 
O1 U1 Cl1 91.53(8) 3_565 . ? 
O1 U1 Cl1 88.47(8) . . ? 
Cl2 U1 Cl1 90.19(4) . . ? 
Cl2 U1 Cl1 89.81(4) 3_565 . ? 
O1 U1 Cl1 88.47(8) 3_565 3_565 ? 
O1 U1 Cl1 91.53(8) . 3_565 ? 
Cl2 U1 Cl1 89.81(4) . 3_565 ? 
Cl2 U1 Cl1 90.19(4) 3_565 3_565 ? 
Cl1 U1 Cl1 180.0 . 3_565 ? 
C4 N1 C2 107.9(4) . . ? 
C4 N1 C1 126.6(4) . . ? 
C2 N1 C1 125.4(4) . . ? 
C4 N2 C3 107.4(3) . . ? 
C4 N2 C5 125.6(4) . . ? 
C3 N2 C5 127.0(4) . . ? 
N1 C1 H1A 109.5 . . ? 
N1 C1 H1B 109.5 . . ? 
H1A C1 H1B 109.5 . . ? 
N1 C1 H1C 109.5 . . ? 
H1A C1 H1C 109.5 . . ? 
H1B C1 H1C 109.5 . . ? 
N1 C2 C3 107.6(4) . . ? 
N1 C2 H2 126.2 . . ? 
C3 C2 H2 126.2 . . ? 
C2 C3 N2 107.1(4) . . ? 
C2 C3 H3 126.4 . . ? 
N2 C3 H3 126.4 . . ? 
N2 C4 N1 109.9(4) . . ? 
N2 C4 H4 125.0 . . ? 
N1 C4 H4 125.0 . . ? 
N2 C5 C6 111.4(3) . . ? 
N2 C5 H5A 109.3 . . ? 
C6 C5 H5A 109.3 . . ? 
N2 C5 H5B 109.3 . . ? 
C6 C5 H5B 109.3 . . ? 
H5A C5 H5B 108.0 . . ? 
C5 C6 C7 111.4(4) . . ? 
C5 C6 H6A 109.3 . . ? 
C7 C6 H6A 109.3 . . ? 
C5 C6 H6B 109.3 . . ? 
C7 C6 H6B 109.3 . . ? 
H6A C6 H6B 108.0 . . ? 
C8 C7 C6 115.8(5) . . ? 
C8 C7 H7A 108.3 . . ? 
C6 C7 H7A 108.3 . . ? 
C8 C7 H7B 108.3 . . ? 
C6 C7 H7B 108.3 . . ? 
H7A C7 H7B 107.4 . . ? 
C7 C8 H8A 109.5 . . ? 
C7 C8 H8B 109.5 . . ? 
H8A C8 H8B 109.5 . . ? 
C7 C8 H8C 109.5 . . ? 
H8A C8 H8C 109.5 . . ? 
H8B C8 H8C 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              27.50 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.420 
_refine_diff_density_min   -0.826 
_refine_diff_density_rms    0.091 
