#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:18:57 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/62/7046243.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_7046243
loop_
_publ_author_name
'Maria, Leonor'
'Santos, Isabel C.'
'Santos, Isabel'
_publ_section_title
;
 Uranium(iii) complexes supported by hydrobis(mercaptoimidazolyl)borates:
 synthesis and oxidation chemistry.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10601
_journal_page_last               10612
_journal_paper_doi               10.1039/c8dt01149d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C28 H32 B2 N8 O2 S4 U'
_chemical_formula_sum            'C28 H32 B2 N8 O2 S4 U'
_chemical_formula_weight         900.51
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-04-10 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                83.5600(10)
_cell_angle_beta                 78.969(2)
_cell_angle_gamma                79.5510(10)
_cell_formula_units_Z            1
_cell_length_a                   7.6236(2)
_cell_length_b                   8.5987(3)
_cell_length_c                   13.1949(4)
_cell_measurement_reflns_used    4671
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.42
_cell_volume                     832.21(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury Macrae et al,2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5635
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    5.168
_exptl_absorpt_correction_T_max  0.9037
_exptl_absorpt_correction_T_min  0.3960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0229
_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)+(0.0181P)²+0.9025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                2828
_reflns_number_total             2835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt01149d2.cif
_cod_data_source_block           comp8_free
_cod_depositor_comments
'Adding full bibliography for 7046238--7046244.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7046243
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.5000 0.5000 0.5000 0.01286(8) Uani 1 2 d S
S1 S 0.84687(13) 0.33497(11) 0.48113(7) 0.0178(2) Uani 1 1 d .
S2 S 0.59569(13) 0.63809(10) 0.30325(7) 0.0161(2) Uani 1 1 d .
O1 O 0.4220(4) 0.3448(3) 0.4515(2) 0.0194(6) Uani 1 1 d .
N1 N 0.8267(4) 0.1613(4) 0.3203(2) 0.0136(7) Uani 1 1 d .
N2 N 0.7800(4) 0.0347(4) 0.4748(2) 0.0168(7) Uani 1 1 d .
N3 N 0.6633(4) 0.3641(4) 0.2008(2) 0.0147(7) Uani 1 1 d .
N4 N 0.3947(5) 0.5040(4) 0.1979(3) 0.0211(7) Uani 1 1 d .
B1 B 0.8552(6) 0.2942(5) 0.2294(3) 0.0144(9) Uani 1 1 d .
H1 H 0.911(6) 0.388(5) 0.257(3) 0.026(12) Uiso 1 1 d .
C1 C 0.8145(5) 0.1743(4) 0.4229(3) 0.0168(8) Uani 1 1 d .
C2 C 0.7952(5) 0.0104(5) 0.3098(3) 0.0192(8) Uani 1 1 d .
H2 H 0.7931 -0.0309 0.2463 0.023 Uiso 1 1 calc R
C3 C 0.7683(5) -0.0680(5) 0.4042(3) 0.0194(8) Uani 1 1 d .
H3 H 0.7456 -0.1740 0.4193 0.023 Uiso 1 1 calc R
C4 C 0.7504(6) 0.0004(5) 0.5870(3) 0.0253(10) Uani 1 1 d .
H4C H 0.6279 0.0496 0.6168 0.038 Uiso 1 1 calc R
H4B H 0.8393 0.0432 0.6159 0.038 Uiso 1 1 calc R
H4A H 0.7644 -0.1147 0.6036 0.038 Uiso 1 1 calc R
C5 C 0.5514(5) 0.4971(4) 0.2321(3) 0.0142(8) Uani 1 1 d .
C6 C 0.5698(6) 0.2882(5) 0.1460(3) 0.0217(9) Uani 1 1 d .
H6 H 0.6147 0.1903 0.1158 0.026 Uiso 1 1 calc R
C7 C 0.4069(6) 0.3749(5) 0.1426(3) 0.0241(9) Uani 1 1 d .
H7 H 0.3166 0.3519 0.1086 0.029 Uiso 1 1 calc R
C8 C 0.2342(6) 0.6261(5) 0.2180(4) 0.0309(10) Uani 1 1 d .
H8B H 0.2331 0.7056 0.1587 0.046 Uiso 1 1 calc R
H8C H 0.2372 0.6773 0.2802 0.046 Uiso 1 1 calc R
H8A H 0.1250 0.5771 0.2285 0.046 Uiso 1 1 calc R
C9 C 0.9909(5) 0.2219(4) 0.1294(3) 0.0164(8) Uani 1 1 d .
C10 C 0.9887(5) 0.3027(5) 0.0318(3) 0.0190(8) Uani 1 1 d .
H10 H 0.8945 0.3896 0.0235 0.023 Uiso 1 1 calc R
C11 C 1.1202(6) 0.2602(5) -0.0540(3) 0.0220(9) Uani 1 1 d .
H11 H 1.1170 0.3197 -0.1189 0.026 Uiso 1 1 calc R
C12 C 1.2539(6) 0.1322(5) -0.0443(3) 0.0217(9) Uani 1 1 d .
H12 H 1.3445 0.1033 -0.1022 0.026 Uiso 1 1 calc R
C13 C 1.2560(6) 0.0455(5) 0.0504(3) 0.0228(9) Uani 1 1 d .
H13 H 1.3461 -0.0453 0.0570 0.027 Uiso 1 1 calc R
C14 C 1.1269(6) 0.0910(5) 0.1356(3) 0.0209(9) Uani 1 1 d .
H14 H 1.1313 0.0308 0.2003 0.025 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'
S S 0.1246 0.1234 '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'
B B 0.0013 0.0007 '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
O1 U1 O1 180.00(16) . 2_666
O1 U1 S1 91.91(9) . .
O1 U1 S1 88.09(9) 2_666 .
O1 U1 S1 88.09(9) . 2_666
O1 U1 S1 91.91(9) 2_666 2_666
S1 U1 S1 180.0 . 2_666
O1 U1 S2 91.78(9) . .
O1 U1 S2 88.22(9) 2_666 .
S1 U1 S2 87.69(3) . .
S1 U1 S2 92.31(3) 2_666 .
O1 U1 S2 88.22(9) . 2_666
O1 U1 S2 91.78(9) 2_666 2_666
S1 U1 S2 92.31(3) . 2_666
S1 U1 S2 87.69(3) 2_666 2_666
S2 U1 S2 180.0 . 2_666
C1 S1 U1 98.29(13) . .
C5 S2 U1 99.47(12) . .
C1 N1 C2 107.1(3) . .
C1 N1 B1 127.4(3) . .
C2 N1 B1 125.4(3) . .
C1 N2 C3 108.7(3) . .
C1 N2 C4 126.1(3) . .
C3 N2 C4 125.2(3) . .
C5 N3 C6 106.9(3) . .
C5 N3 B1 128.0(3) . .
C6 N3 B1 124.8(3) . .
C5 N4 C7 109.1(3) . .
C5 N4 C8 126.0(3) . .
C7 N4 C8 124.9(4) . .
N1 B1 N3 107.2(3) . .
N1 B1 C9 110.9(3) . .
N3 B1 C9 110.1(3) . .
N1 B1 H1 108(2) . .
N3 B1 H1 110(2) . .
C9 B1 H1 111(2) . .
N1 C1 N2 108.3(3) . .
N1 C1 S1 127.4(3) . .
N2 C1 S1 124.2(3) . .
C3 C2 N1 109.0(3) . .
C3 C2 H2 125.5 . .
N1 C2 H2 125.5 . .
C2 C3 N2 106.9(3) . .
C2 C3 H3 126.5 . .
N2 C3 H3 126.5 . .
N2 C4 H4C 109.5 . .
N2 C4 H4B 109.5 . .
H4C C4 H4B 109.5 . .
N2 C4 H4A 109.5 . .
H4C C4 H4A 109.5 . .
H4B C4 H4A 109.5 . .
N4 C5 N3 108.2(3) . .
N4 C5 S2 124.4(3) . .
N3 C5 S2 127.4(3) . .
C7 C6 N3 109.0(4) . .
C7 C6 H6 125.5 . .
N3 C6 H6 125.5 . .
C6 C7 N4 106.8(4) . .
C6 C7 H7 126.6 . .
N4 C7 H7 126.6 . .
N4 C8 H8B 109.5 . .
N4 C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N4 C8 H8A 109.5 . .
H8B C8 H8A 109.5 . .
H8C C8 H8A 109.5 . .
C14 C9 C10 116.3(4) . .
C14 C9 B1 123.7(3) . .
C10 C9 B1 119.7(3) . .
C11 C10 C9 122.1(4) . .
C11 C10 H10 118.9 . .
C9 C10 H10 118.9 . .
C12 C11 C10 119.8(4) . .
C12 C11 H11 120.1 . .
C10 C11 H11 120.1 . .
C11 C12 C13 119.6(4) . .
C11 C12 H12 120.2 . .
C13 C12 H12 120.2 . .
C12 C13 C14 120.1(4) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C13 C14 C9 122.0(4) . .
C13 C14 H14 119.0 . .
C9 C14 H14 119.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.780(3) .
U1 O1 1.780(3) 2_666
U1 S1 2.7450(10) .
U1 S1 2.7450(10) 2_666
U1 S2 2.7531(9) .
U1 S2 2.7531(9) 2_666
S1 C1 1.730(4) .
S2 C5 1.729(4) .
N1 C1 1.355(5) .
N1 C2 1.388(5) .
N1 B1 1.573(5) .
N2 C1 1.357(5) .
N2 C3 1.379(5) .
N2 C4 1.458(5) .
N3 C5 1.350(5) .
N3 C6 1.390(5) .
N3 B1 1.576(5) .
N4 C5 1.345(5) .
N4 C7 1.375(5) .
N4 C8 1.463(5) .
B1 C9 1.620(5) .
B1 H1 1.11(5) .
C2 C3 1.346(5) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 H4C 0.9800 .
C4 H4B 0.9800 .
C4 H4A 0.9800 .
C6 C7 1.334(6) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C8 H8A 0.9800 .
C9 C14 1.392(5) .
C9 C10 1.395(5) .
C10 C11 1.395(5) .
C10 H10 0.9500 .
C11 C12 1.370(6) .
C11 H11 0.9500 .
C12 C13 1.382(6) .
C12 H12 0.9500 .
C13 C14 1.386(6) .
C13 H13 0.9500 .
C14 H14 0.9500 .
