data_OLSN88
_audit_creation_date              2012-02-06
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_chemical_formula_moiety          '0.5(Cl10 O2 U2), 0.5(C48 H40 P2)'
_chemical_formula_sum             'C24 H20 Cl5 O P U'
_chemical_formula_weight          770.69
_chemical_oxdiff_formula          'U1 O1 Cl5 P1 C24 H20'
loop_
  _atom_type_symbol
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 C 0.00347 0.00161 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
 Cl 0.14873 0.16029 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
 H 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
 O 0.01158 0.00611 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
 P 0.10434 0.09671 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
 U -10.21189 10.40537
 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'

_space_group_crystal_system       'tetragonal'
_space_group_IT_number            85
_space_group_name_H-M_alt         'P 4/n'
_space_group_name_Hall            '-P 4a'
loop_
  _space_group_symop_id
  _space_group_symop_operation_xyz
 1 x,y,z
 2 -y+1/2,x,z
 3 y,-x+1/2,z
 4 -x+1/2,-y+1/2,z
 5 -x,-y,-z
 6 y-1/2,-x,-z
 7 -y,x-1/2,-z
 8 x-1/2,y-1/2,-z

_cell_length_a                    13.1905(4)
_cell_length_b                    13.1905(4)
_cell_length_c                    7.5128(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1307.14(8)
_cell_formula_units_Z             2
_cell_measurement_reflns_used     1499
_cell_measurement_theta_max       28.2891
_cell_measurement_theta_min       3.0825
_exptl_absorpt_coefficient_mu     6.799
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_correction_T_min   0.76914
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn     1.9580
_exptl_crystal_F_000              709.7255
_diffrn_reflns_av_R_equivalents   0.0389
_diffrn_reflns_av_unetI/netI      0.0576
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_l_max        4
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_number             2640
_diffrn_reflns_theta_full         28.351280
_diffrn_reflns_theta_max          1.1576
_diffrn_reflns_theta_min          0.9294
_diffrn_detector_area_resol_mean  8.3367
_diffrn_measured_fraction_theta_full 0.879489
_diffrn_measured_fraction_theta_max 0.879489
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -19.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4808  -99.0000   60.0000 82

#__ type_ start__ end____ width___ exp.time_
  2 omega  -38.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4808  -77.0000 -150.0000 36
;
_diffrn_measurement_device_type   'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method        'ω scans'
_diffrn_orient_matrix_UB_11       0.0234125000
_diffrn_orient_matrix_UB_12       0.0472240000
_diffrn_orient_matrix_UB_13       -0.0185215000
_diffrn_orient_matrix_UB_21       0.0481387000
_diffrn_orient_matrix_UB_22       -0.0215145000
_diffrn_orient_matrix_UB_23       0.0186610000
_diffrn_orient_matrix_UB_31       0.0051218000
_diffrn_orient_matrix_UB_32       -0.0140925000
_diffrn_orient_matrix_UB_33       -0.0906765000
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength      0.7107
_diffrn_source                    'Enhance (Mo) X-ray Source'
_diffrn_source_current            n/a
_diffrn_source_voltage            n/a
_reflns_Friedel_coverage          0.0
_reflns_limit_h_max               17
_reflns_limit_h_min               0
_reflns_limit_k_max               17
_reflns_limit_k_min               0
_reflns_limit_l_max               9
_reflns_limit_l_min               0
_reflns_number_gt                 1301
_reflns_number_total              1445
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric  1
_reflns_odcompleteness_theta      26.32
_reflns_threshold_expression      I>=2u(I)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max          2.081476
_refine_diff_density_min          -1.099274
_refine_diff_density_rms          0.248689
_refine_ls_d_res_high             0.748332
_refine_ls_d_res_low              6.595247
_refine_ls_goodness_of_fit_ref    0.831615
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_constraints     0
_refine_ls_number_parameters      94
_refine_ls_number_reflns          1445
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.038250
_refine_ls_R_factor_gt            0.030814
_refine_ls_restrained_S_all       0.831615
_refine_ls_shift/su_max           0.1373
_refine_ls_shift/su_mean          0.0015
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0569P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_ref          0.078294
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_refinement_flags_posn
 U1 U 0.250000 0.250000 0.66716(4) 0.01241(13) Uani 1.000000 S
 P2 P 0.250000 0.750000 0.500000 0.0091(4) Uani 1.000000 S
 C6 C 0.2560(3) 0.6410(3) 0.3563(6) 0.0117(9) Uani 1.000000 .
 C7 C 0.2677(5) 0.4852(4) 0.1128(8) 0.0243(12) Uani 1.000000 .
 C8 C 0.1833(4) 0.6341(4) 0.2197(7) 0.0179(10) Uani 1.000000 .
 C9 C 0.3335(4) 0.5709(4) 0.3696(7) 0.0151(10) Uani 1.000000 .
 C10 C 0.1900(4) 0.5544(4) 0.0989(7) 0.0219(11) Uani 1.000000 .
 C11 C 0.3390(4) 0.4921(4) 0.2471(8) 0.0213(11) Uani 1.000000 .
 Cl1 Cl 0.250000 0.250000 0.3425(3) 0.0178(5) Uani 1.000000 S
 Cl2 Cl 0.36134(10) 0.09198(10) 0.66944(16) 0.0240(3) Uani 1.000000 .
 O3 O 0.250000 0.250000 0.9088(10) 0.0171(14) Uani 1.000000 S
 H10 H 0.147(4) 0.559(4) 0.007(6) 0.009(12) Uiso 1.000000 .
 H11 H 0.382(3) 0.448(4) 0.247(6) 0.000(11) Uiso 1.000000 .
 H9 H 0.381(4) 0.581(4) 0.452(8) 0.021(14) Uiso 1.000000 .
 H8 H 0.133(4) 0.685(4) 0.210(7) 0.020(14) Uiso 1.000000 .
 H7 H 0.274(4) 0.436(5) 0.049(8) 0.023(15) Uiso 1.000000 .

loop_
  _atom_site_aniso_label
  _atom_site_aniso_U_11
  _atom_site_aniso_U_22
  _atom_site_aniso_U_33
  _atom_site_aniso_U_12
  _atom_site_aniso_U_13
  _atom_site_aniso_U_23
 U1 0.01144(15) 0.01144(15) 0.0144(2) -0.000000 -0.000000 0.000000
 P2 0.0093(6) 0.0093(6) 0.0088(10) -0.000000 -0.000000 0.000000
 C6 0.014(2) 0.010(2) 0.010(2) -0.0032(17) 0.0032(18) -0.0022(18)
 C7 0.041(3) 0.013(2) 0.020(3) -0.008(2) 0.007(2) -0.002(2)
 C8 0.021(3) 0.014(2) 0.019(2) -0.005(2) -0.003(2) 0.001(2)
 C9 0.017(2) 0.015(2) 0.013(2) -0.0046(19) 0.003(2) -0.0003(19)
 C10 0.035(3) 0.019(3) 0.011(2) -0.005(2) -0.005(2) 0.001(2)
 C11 0.024(3) 0.012(2) 0.027(3) 0.005(2) 0.009(2) -0.000(2)
 Cl1 0.0193(7) 0.0193(7) 0.0149(11) -0.000000 -0.000000 0.000000
 Cl2 0.0281(7) 0.0190(6) 0.0249(7) 0.0125(5) 0.0070(5) 0.0049(5)
 O3 0.0090(19) 0.0090(19) 0.033(4) -0.000000 -0.000000 0.000000

loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
 U1 Cl1 2.439(2) .
 U1 Cl2 2.5499(12) .
 U1 Cl2 2.5499(12) 3
 U1 Cl2 2.5499(12) 2
 U1 Cl2 2.5499(12) 4
 U1 O3 1.816(7) .
 P2 C6 1.800(4) .
 P2 C6 1.800(4) 4_565
 P2 C6 1.800(4) 6_566
 P2 C6 1.800(4) 7_666
 C6 C8 1.407(7) .
 C6 C9 1.382(7) .
 C7 C10 1.377(8) .
 C7 C11 1.383(8) .
 C7 H7 0.82(6) .
 C8 C10 1.391(7) .
 C8 H8 0.95(6) .
 C9 C11 1.390(7) .
 C9 H9 0.89(6) .
 C10 H10 0.90(5) .
 C11 H11 0.81(5) .

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
 Cl2 U1 Cl1 90.38(3) 3 .
 Cl2 U1 Cl1 90.38(3) . .
 Cl2 U1 Cl1 90.38(3) 4 .
 Cl2 U1 Cl1 90.38(3) 2 .
 Cl2 U1 Cl2 89.997(11) . 3
 Cl2 U1 Cl2 179.23(6) 2 3
 Cl2 U1 Cl2 89.997(11) 2 .
 Cl2 U1 Cl2 89.997(12) 4 3
 Cl2 U1 Cl2 179.23(6) 4 .
 Cl2 U1 Cl2 89.997(11) 4 2
 O3 U1 Cl1 180.0 . .
 O3 U1 Cl2 89.62(3) . .
 O3 U1 Cl2 89.62(3) . 3
 O3 U1 Cl2 89.62(3) . 4
 O3 U1 Cl2 89.62(3) . 2
 C6 P2 C6 106.3(3) . 4_565
 C6 P2 C6 111.08(15) 6_566 4_565
 C6 P2 C6 111.08(14) 6_566 .
 C6 P2 C6 111.08(14) 7_666 4_565
 C6 P2 C6 111.08(15) 7_666 .
 C6 P2 C6 106.3(3) 7_666 6_566
 C8 C6 P2 117.3(4) . 4_565
 C9 C6 P2 121.6(4) . 4_565
 C9 C6 C8 120.9(4) . .
 C11 C7 C10 121.1(5) . .
 H7 C7 C10 124(4) . .
 H7 C7 C11 114(4) . .
 C10 C8 C6 118.8(5) . .
 H8 C8 C6 119(3) . .
 H8 C8 C10 122(3) . .
 C11 C9 C6 119.4(5) . .
 H9 C9 C6 118(4) . .
 H9 C9 C11 122(4) . .
 C8 C10 C7 120.0(5) . .
 H10 C10 C7 125(3) . .
 H10 C10 C8 114(3) . .
 C9 C11 C7 119.8(5) . .
 H11 C11 C7 115(3) . .
 H11 C11 C9 125(3) . .

