#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:17:58 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179962 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/56/7025639.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7025639
loop_
_publ_author_name
'Swartz, 2nd, Douglas L'
'Spencer, Liam P.'
'Scott, Brian L.'
'Odom, Aaron L.'
'Boncella, James M.'
_publ_section_title
;
 Exploring the coordination modes of pyrrolyl ligands in bis(imido)
 uranium(VI) complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6841
_journal_page_last               6846
_journal_paper_doi               10.1039/c002440f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C58 H68 Cl4 N4 O2 P2 U'
_chemical_formula_weight         1294.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.5310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.705(2)
_cell_length_b                   19.068(3)
_cell_length_c                   16.984(2)
_cell_measurement_temperature    120(1)
_cell_volume                     5369.6(12)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27712
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.329
_exptl_absorpt_correction_T_max  0.7319
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Eight disordered dichloromethane solvent molecules per cell were squeezed.
;
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0397P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                4828
_reflns_number_total             5550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002440f.txt
_cod_data_source_block           apx615s
_cod_original_cell_volume        5369.4(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7025639
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'
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
U1 U 0.5000 0.322289(10) 0.7500 0.02133(7) Uani 1 2 d S
P1 P 0.62992(6) 0.28376(5) 0.61321(6) 0.0253(2) Uani 1 1 d .
N1 N 0.40495(18) 0.32952(15) 0.65974(19) 0.0265(7) Uani 1 1 d .
N2 N 0.5000 0.4512(2) 0.7500 0.0318(10) Uani 1 2 d S
N3 N 0.5000 0.1925(2) 0.7500 0.0253(10) Uani 1 2 d S
O1 O 0.57984(15) 0.30701(12) 0.66379(15) 0.0279(6) Uani 1 1 d .
C1 C 0.5669(2) 0.25830(19) 0.5094(2) 0.0278(8) Uani 1 1 d .
C2 C 0.5896(3) 0.2087(2) 0.4625(2) 0.0376(10) Uani 1 1 d .
H2 H 0.6392 0.1863 0.4851 0.045 Uiso 1 1 calc R
C3 C 0.5390(3) 0.1923(2) 0.3827(3) 0.0491(12) Uani 1 1 d .
H3 H 0.5544 0.1585 0.3517 0.059 Uiso 1 1 calc R
C4 C 0.4655(3) 0.2256(2) 0.3481(3) 0.0412(10) Uani 1 1 d .
H4 H 0.4318 0.2143 0.2940 0.049 Uiso 1 1 calc R
C5 C 0.4421(2) 0.2751(2) 0.3930(2) 0.0375(10) Uani 1 1 d .
H5 H 0.3926 0.2975 0.3693 0.045 Uiso 1 1 calc R
C6 C 0.4918(2) 0.2916(2) 0.4736(2) 0.0329(9) Uani 1 1 d .
H6 H 0.4756 0.3250 0.5043 0.039 Uiso 1 1 calc R
C7 C 0.6945(2) 0.2114(2) 0.6608(2) 0.0283(8) Uani 1 1 d .
C8 C 0.7675(2) 0.2006(2) 0.6495(2) 0.0322(9) Uani 1 1 d .
H8 H 0.7844 0.2316 0.6168 0.039 Uiso 1 1 calc R
C9 C 0.8149(2) 0.1441(2) 0.6868(2) 0.0373(10) Uani 1 1 d .
H9 H 0.8639 0.1369 0.6793 0.045 Uiso 1 1 calc R
C10 C 0.7900(2) 0.0981(2) 0.7351(3) 0.0373(10) Uani 1 1 d .
H10 H 0.8219 0.0596 0.7595 0.045 Uiso 1 1 calc R
C11 C 0.7181(2) 0.1087(2) 0.7476(3) 0.0411(10) Uani 1 1 d .
H11 H 0.7021 0.0780 0.7813 0.049 Uiso 1 1 calc R
C12 C 0.6692(2) 0.1654(2) 0.7098(3) 0.0356(10) Uani 1 1 d .
H12 H 0.6201 0.1722 0.7173 0.043 Uiso 1 1 calc R
C13 C 0.6947(2) 0.3522(2) 0.6004(2) 0.0270(8) Uani 1 1 d .
C14 C 0.6803(3) 0.3847(2) 0.5243(3) 0.0371(10) Uani 1 1 d .
H14 H 0.6370 0.3706 0.4774 0.045 Uiso 1 1 calc R
C15 C 0.7300(3) 0.4383(2) 0.5172(3) 0.0483(12) Uani 1 1 d .
H15 H 0.7206 0.4595 0.4653 0.058 Uiso 1 1 calc R
C16 C 0.7928(3) 0.4605(2) 0.5858(3) 0.0436(11) Uani 1 1 d .
H16 H 0.8252 0.4973 0.5807 0.052 Uiso 1 1 calc R
C17 C 0.8083(2) 0.4285(2) 0.6627(3) 0.0382(10) Uani 1 1 d .
H17 H 0.8517 0.4431 0.7092 0.046 Uiso 1 1 calc R
C18 C 0.7593(2) 0.3750(2) 0.6701(2) 0.0345(9) Uani 1 1 d .
H18 H 0.7693 0.3537 0.7221 0.041 Uiso 1 1 calc R
C19 C 0.3223(2) 0.3550(2) 0.6123(2) 0.0330(9) Uani 1 1 d .
C20 C 0.3153(2) 0.3665(2) 0.5203(2) 0.0402(10) Uani 1 1 d .
H20A H 0.3512 0.4034 0.5176 0.060 Uiso 1 1 calc R
H20B H 0.2609 0.3792 0.4874 0.060 Uiso 1 1 calc R
H20C H 0.3295 0.3240 0.4985 0.060 Uiso 1 1 calc R
C21 C 0.2615(2) 0.3004(2) 0.6169(3) 0.0392(10) Uani 1 1 d .
H21A H 0.2692 0.2579 0.5903 0.059 Uiso 1 1 calc R
H21B H 0.2078 0.3177 0.5886 0.059 Uiso 1 1 calc R
H21C H 0.2690 0.2910 0.6747 0.059 Uiso 1 1 calc R
C22 C 0.3077(3) 0.4234(2) 0.6500(3) 0.0406(10) Uani 1 1 d .
H22A H 0.3165 0.4167 0.7086 0.061 Uiso 1 1 calc R
H22B H 0.2531 0.4383 0.6214 0.061 Uiso 1 1 calc R
H22C H 0.3441 0.4585 0.6438 0.061 Uiso 1 1 calc R
C23 C 0.4922(2) 0.4944(2) 0.8106(2) 0.0284(8) Uani 1 1 d .
C24 C 0.4954(2) 0.5624(2) 0.7892(2) 0.0327(9) Uani 1 1 d .
H24 H 0.4920 0.6015 0.8206 0.039 Uiso 1 1 calc R
C25 C 0.4770(3) 0.4682(2) 0.8868(2) 0.0435(10) Uani 1 1 d .
H25A H 0.4863 0.5054 0.9272 0.065 Uiso 1 1 calc R
H25B H 0.5128 0.4299 0.9111 0.065 Uiso 1 1 calc R
H25C H 0.4222 0.4525 0.8710 0.065 Uiso 1 1 calc R
C26 C 0.4651(2) 0.1479(2) 0.6811(2) 0.0284(8) Uani 1 1 d .
C27 C 0.4782(2) 0.0796(2) 0.7071(3) 0.0376(10) Uani 1 1 d .
H27 H 0.4610 0.0401 0.6733 0.045 Uiso 1 1 calc R
C28 C 0.4229(2) 0.1733(2) 0.5948(2) 0.0366(9) Uani 1 1 d .
H28A H 0.4328 0.1417 0.5555 0.055 Uiso 1 1 calc R
H28B H 0.4423 0.2192 0.5885 0.055 Uiso 1 1 calc R
H28C H 0.3660 0.1755 0.5842 0.055 Uiso 1 1 calc R
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'
P P 0.1023 0.0942 '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'
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
N1 U1 N1 171.42(17) 2_656 .
N1 U1 O1 87.41(11) 2_656 .
N1 U1 O1 93.64(11) . .
N1 U1 O1 93.64(11) 2_656 2_656
N1 U1 O1 87.41(11) . 2_656
O1 U1 O1 165.95(12) . 2_656
N1 U1 N2 85.71(9) 2_656 .
N1 U1 N2 85.71(9) . .
O1 U1 N2 97.02(6) . .
O1 U1 N2 97.02(6) 2_656 .
N1 U1 N3 94.29(9) 2_656 .
N1 U1 N3 94.29(9) . .
O1 U1 N3 82.98(6) . .
O1 U1 N3 82.98(6) 2_656 .
N2 U1 N3 180.000(1) . .
O1 P1 C1 110.74(16) . .
O1 P1 C7 112.36(16) . .
C1 P1 C7 108.28(17) . .
O1 P1 C13 112.58(16) . .
C1 P1 C13 106.30(17) . .
C7 P1 C13 106.26(18) . .
C19 N1 U1 156.4(3) . .
C23 N2 C23 105.7(4) 2_656 .
C23 N2 U1 127.1(2) 2_656 .
C23 N2 U1 127.1(2) . .
C26 N3 C26 105.5(4) . 2_656
C26 N3 U1 127.3(2) . .
C26 N3 U1 127.3(2) 2_656 .
P1 O1 U1 169.77(15) . .
C2 C1 C6 118.8(4) . .
C2 C1 P1 123.1(3) . .
C6 C1 P1 118.1(3) . .
C3 C2 C1 120.2(4) . .
C2 C3 C4 120.4(4) . .
C5 C4 C3 120.4(4) . .
C4 C5 C6 119.9(4) . .
C5 C6 C1 120.2(4) . .
C8 C7 C12 120.1(4) . .
C8 C7 P1 122.0(3) . .
C12 C7 P1 117.9(3) . .
C9 C8 C7 120.0(4) . .
C10 C9 C8 120.1(4) . .
C9 C10 C11 120.4(4) . .
C10 C11 C12 120.2(4) . .
C7 C12 C11 119.2(4) . .
C14 C13 C18 118.9(4) . .
C14 C13 P1 121.7(3) . .
C18 C13 P1 119.4(3) . .
C13 C14 C15 120.2(4) . .
C16 C15 C14 120.5(4) . .
C15 C16 C17 120.3(4) . .
C18 C17 C16 119.5(4) . .
C17 C18 C13 120.6(4) . .
N1 C19 C22 109.6(3) . .
N1 C19 C21 109.3(3) . .
C22 C19 C21 109.9(3) . .
N1 C19 C20 108.1(3) . .
C22 C19 C20 109.9(3) . .
C21 C19 C20 110.1(3) . .
C24 C23 N2 110.5(3) . .
C24 C23 C25 126.0(4) . .
N2 C23 C25 123.3(3) . .
C23 C24 C24 106.6(2) . 2_656
C27 C26 N3 109.3(3) . .
C27 C26 C28 127.1(4) . .
N3 C26 C28 123.6(3) . .
C26 C27 C27 107.9(2) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 1.842(3) 2_656
U1 N1 1.842(3) .
U1 O1 2.383(2) .
U1 O1 2.383(2) 2_656
U1 N2 2.459(4) .
U1 N3 2.476(4) .
P1 O1 1.502(3) .
P1 C1 1.791(4) .
P1 C7 1.793(4) .
P1 C13 1.800(4) .
N1 C19 1.483(5) .
N2 C23 1.362(4) 2_656
N2 C23 1.362(4) .
N3 C26 1.402(4) .
N3 C26 1.402(4) 2_656
C1 C2 1.385(5) .
C1 C6 1.405(5) .
C2 C3 1.372(6) .
C3 C4 1.380(6) .
C4 C5 1.366(6) .
C5 C6 1.379(5) .
C7 C8 1.387(5) .
C7 C12 1.388(5) .
C8 C9 1.377(6) .
C9 C10 1.375(6) .
C10 C11 1.377(6) .
C11 C12 1.393(5) .
C13 C14 1.375(5) .
C13 C18 1.397(5) .
C14 C15 1.381(6) .
C15 C16 1.365(6) .
C16 C17 1.378(6) .
C17 C18 1.374(5) .
C19 C22 1.514(6) .
C19 C21 1.519(6) .
C19 C20 1.540(5) .
C23 C24 1.355(5) .
C23 C25 1.496(5) .
C24 C24 1.399(8) 2_656
C26 C27 1.370(5) .
C26 C28 1.473(5) .
C27 C27 1.388(8) 2_656
