#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:48:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178964 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/93/4119323.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_4119323
loop_
_publ_author_name
'Liam P. Spencer'
'Ping Yang'
'Stefan G. Minasian'
'Robert E. Jilek'
'Enrique R. Batista'
'Kevin S. Boland'
'James M. Boncella'
'Steven D. Conradson'
'David L. Clark'
'Trevor W. Hayton'
'Stosh A. Kozimor'
'Richard L. Martin'
'Molly M. MacInnes'
'Angela C. Olson'
'Brian L. Scott'
'David K. Shuh'
'Marianne P. Wilkerson'
_publ_section_title
;
 Tetrahalide Complexes of the [U(NR)2]2+ Ion: Synthesis, Theory, and
 Chlorine K-Edge X-ray Absorption Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2279
_journal_page_last               2290
_journal_paper_doi               10.1021/ja310575j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C24 H58 Br4 N4 U'
_chemical_formula_weight         960.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9027(12)
_cell_length_b                   11.4929(9)
_cell_length_c                   19.6962(16)
_cell_measurement_temperature    140(1)
_cell_volume                     3373.5(5)
_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      140(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.961
_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  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36055
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.568
_exptl_absorpt_correction_T_max  0.5975
_exptl_absorpt_correction_T_min  0.2506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       'rectangular slab'
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         4107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0374P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                3000
_reflns_number_total             4107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310575j_si_002_6.cif
_cod_data_source_block           apx949a
_cod_database_code               4119323
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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 0.0000 0.5000 0.0000 0.01331(8) Uani 1 2 d S
Br2 Br -0.09584(4) 0.41379(4) 0.11720(3) 0.02620(14) Uani 1 1 d .
Br1 Br 0.04768(4) 0.70099(4) 0.07682(3) 0.02868(15) Uani 1 1 d .
N1 N 0.1039(3) 0.4282(3) 0.0256(2) 0.0164(9) Uani 1 1 d .
N2 N 0.9413(3) 0.0140(3) 0.1887(2) 0.0196(10) Uani 1 1 d .
C1 C 0.1938(3) 0.3754(4) 0.0332(2) 0.0152(10) Uani 1 1 d .
C2 C 0.1952(4) 0.3053(5) 0.0980(3) 0.0316(14) Uani 1 1 d .
H2A H 0.1811 0.3549 0.1357 0.047 Uiso 1 1 calc R
H2B H 0.2539 0.2724 0.1044 0.047 Uiso 1 1 calc R
H2C H 0.1517 0.2439 0.0951 0.047 Uiso 1 1 calc R
C3 C 0.2626(4) 0.4724(4) 0.0364(4) 0.0332(15) Uani 1 1 d .
H3A H 0.2585 0.5190 -0.0039 0.050 Uiso 1 1 calc R
H3B H 0.3217 0.4395 0.0396 0.050 Uiso 1 1 calc R
H3C H 0.2512 0.5200 0.0755 0.050 Uiso 1 1 calc R
C4 C 0.2127(4) 0.2993(5) -0.0283(3) 0.0272(12) Uani 1 1 d .
H4A H 0.1678 0.2397 -0.0314 0.041 Uiso 1 1 calc R
H4B H 0.2708 0.2641 -0.0236 0.041 Uiso 1 1 calc R
H4C H 0.2115 0.3462 -0.0686 0.041 Uiso 1 1 calc R
C5 C 0.8692(4) -0.0630(5) 0.1590(3) 0.0329(14) Uani 1 1 d .
H5A H 0.8152 -0.0171 0.1533 0.039 Uiso 1 1 calc R
H5B H 0.8884 -0.0881 0.1143 0.039 Uiso 1 1 calc R
C6 C 0.8465(4) -0.1694(5) 0.2004(3) 0.0439(17) Uani 1 1 d .
H6A H 0.8986 -0.2181 0.2042 0.066 Uiso 1 1 calc R
H6B H 0.7991 -0.2117 0.1786 0.066 Uiso 1 1 calc R
H6C H 0.8274 -0.1459 0.2449 0.066 Uiso 1 1 calc R
C7 C 0.9175(4) 0.0574(5) 0.2591(3) 0.0276(13) Uani 1 1 d .
H7A H 0.9096 -0.0093 0.2887 0.033 Uiso 1 1 calc R
H7B H 0.9675 0.1024 0.2765 0.033 Uiso 1 1 calc R
C8 C 0.8338(4) 0.1314(6) 0.2624(3) 0.0423(17) Uani 1 1 d .
H8A H 0.8401 0.1967 0.2324 0.063 Uiso 1 1 calc R
H8B H 0.8253 0.1587 0.3080 0.063 Uiso 1 1 calc R
H8C H 0.7829 0.0857 0.2488 0.063 Uiso 1 1 calc R
C9 C 1.0282(4) -0.0556(5) 0.1940(3) 0.0272(13) Uani 1 1 d .
H9A H 1.0207 -0.1139 0.2292 0.033 Uiso 1 1 calc R
H9B H 1.0373 -0.0964 0.1514 0.033 Uiso 1 1 calc R
C10 C 1.1117(4) 0.0135(5) 0.2095(3) 0.0348(15) Uani 1 1 d .
H10A H 1.1206 0.0711 0.1749 0.052 Uiso 1 1 calc R
H10B H 1.1625 -0.0378 0.2108 0.052 Uiso 1 1 calc R
H10C H 1.1052 0.0512 0.2527 0.052 Uiso 1 1 calc R
C11 C 0.9535(4) 0.1175(4) 0.1419(3) 0.0259(12) Uani 1 1 d .
H11A H 0.8963 0.1572 0.1378 0.031 Uiso 1 1 calc R
H11B H 0.9952 0.1712 0.1631 0.031 Uiso 1 1 calc R
C12 C 0.9873(4) 0.0903(6) 0.0715(3) 0.0353(15) Uani 1 1 d .
H12A H 1.0454 0.0546 0.0745 0.053 Uiso 1 1 calc R
H12B H 0.9917 0.1610 0.0458 0.053 Uiso 1 1 calc R
H12C H 0.9463 0.0381 0.0494 0.053 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'
Br Br -0.2901 2.4595 '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 180.0 5_565 .
N1 U1 Br1 89.53(12) 5_565 .
N1 U1 Br1 90.47(12) . .
N1 U1 Br1 90.47(12) 5_565 5_565
N1 U1 Br1 89.53(12) . 5_565
Br1 U1 Br1 180.0 . 5_565
N1 U1 Br2 92.49(13) 5_565 5_565
N1 U1 Br2 87.51(13) . 5_565
Br1 U1 Br2 91.314(16) . 5_565
Br1 U1 Br2 88.685(16) 5_565 5_565
N1 U1 Br2 87.51(13) 5_565 .
N1 U1 Br2 92.49(13) . .
Br1 U1 Br2 88.686(16) . .
Br1 U1 Br2 91.315(16) 5_565 .
Br2 U1 Br2 180.0 5_565 .
C1 N1 U1 169.1(3) . .
C5 N2 C7 112.4(4) . .
C5 N2 C11 108.1(4) . .
C7 N2 C11 109.0(4) . .
C5 N2 C9 108.8(4) . .
C7 N2 C9 107.9(4) . .
C11 N2 C9 110.5(4) . .
N1 C1 C2 108.5(4) . .
N1 C1 C3 108.4(4) . .
C2 C1 C3 110.4(5) . .
N1 C1 C4 108.9(4) . .
C2 C1 C4 111.3(4) . .
C3 C1 C4 109.3(4) . .
C6 C5 N2 115.2(5) . .
C8 C7 N2 114.7(5) . .
C10 C9 N2 116.0(4) . .
C12 C11 N2 115.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 1.825(4) 5_565
U1 N1 1.825(4) .
U1 Br1 2.8513(5) .
U1 Br1 2.8514(5) 5_565
U1 Br2 2.8897(5) 5_565
U1 Br2 2.8898(5) .
N1 C1 1.480(6) .
N2 C5 1.509(7) .
N2 C7 1.515(6) .
N2 C11 1.516(6) .
N2 C9 1.526(7) .
C1 C2 1.510(6) .
C1 C3 1.516(7) .
C1 C4 1.519(7) .
C5 C6 1.508(8) .
C7 C8 1.511(8) .
C9 C10 1.508(8) .
C11 C12 1.507(7) .
