#------------------------------------------------------------------------------
#$Date: 2019-11-23 02:13:56 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/65/4346575.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_4346575
loop_
_publ_author_name
'Kelley, Steven P.'
'Rogers, Robin D.'
_publ_section_title
;
 Isolation of Uranyl Dicyanamide Complexes from N-Donor Ionic Liquids.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10323
_journal_page_last               10334
_journal_paper_doi               10.1021/acs.inorgchem.5b01699
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C4 H14 N6 O18 S2 U2'
_chemical_formula_weight         974.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.0370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9627(2)
_cell_length_b                   10.9246(3)
_cell_length_c                   10.9120(3)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.53
_cell_measurement_theta_min      2.64
_cell_volume                     949.23(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46293
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.717
_diffrn_reflns_theta_min         2.638
_exptl_absorpt_coefficient_mu    17.366
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.3833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.584
_refine_diff_density_min         -2.671
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0087P)²+3.8618P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3735
_reflns_number_total             4081
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01699_si_002.cif
_cod_data_source_block           (UO2(SO4)(biuret)(OH2))2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346575
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.211
_shelx_estimated_absorpt_t_max   0.543
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_adp
U1 U 0.25710(2) 0.53233(2) 0.31205(2) 0.00842(3) Uani 1 1 d .
S1 S -0.16004(9) 0.42107(7) 0.35905(6) 0.00961(11) Uani 1 1 d .
O1 O 0.1253(3) 0.6589(2) 0.2856(2) 0.0169(4) Uani 1 1 d .
O2 O 0.3938(3) 0.4085(2) 0.3415(2) 0.0177(4) Uani 1 1 d .
O3 O 0.0243(3) 0.4193(2) 0.38467(19) 0.0128(4) Uani 1 1 d .
O4 O -0.2485(3) 0.4160(2) 0.47785(19) 0.0177(5) Uani 1 1 d .
O5 O -0.2032(3) 0.3140(2) 0.2853(2) 0.0152(4) Uani 1 1 d .
O6 O -0.2075(3) 0.5339(2) 0.2950(2) 0.0169(4) Uani 1 1 d .
O7 O 0.1505(3) 0.4221(2) 0.13906(19) 0.0159(4) Uani 1 1 d .
O8 O 0.3889(3) 0.5955(3) 0.12637(19) 0.0193(5) Uani 1 1 d .
O9 O 0.5086(3) 0.6587(2) 0.3536(2) 0.0129(4) Uani 1 1 d .
H9B H 0.577(6) 0.622(4) 0.360(4) 0.019 Uiso 1 1 d U
H9A H 0.535(6) 0.714(4) 0.308(4) 0.019 Uiso 1 1 d U
N1 N 0.0901(4) 0.3383(3) -0.0438(2) 0.0169(5) Uani 1 1 d .
H1B H 0.108(6) 0.338(4) -0.111(4) 0.020 Uiso 1 1 d U
H1A H 0.064(6) 0.278(4) -0.002(4) 0.020 Uiso 1 1 d U
N2 N 0.2528(3) 0.5095(3) -0.0385(2) 0.0144(5) Uani 1 1 d .
H2A H 0.240(5) 0.512(4) -0.112(4) 0.017 Uiso 1 1 d U
N3 N 0.4003(5) 0.6880(3) -0.0572(3) 0.0259(7) Uani 1 1 d .
H3B H 0.391(7) 0.681(5) -0.119(5) 0.031 Uiso 1 1 d U
H3A H 0.439(7) 0.734(5) -0.028(5) 0.031 Uiso 1 1 d U
C1 C 0.1653(4) 0.4210(3) 0.0248(3) 0.0114(5) Uani 1 1 d .
C2 C 0.3484(4) 0.5999(3) 0.0160(3) 0.0142(5) Uani 1 1 d .
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'
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 O2 178.09(11) . .
O1 U1 O4 87.36(10) . 3_566
O2 U1 O4 91.40(10) . 3_566
O1 U1 O3 89.87(9) . .
O2 U1 O3 91.27(10) . .
O4 U1 O3 77.08(7) 3_566 .
O1 U1 O8 84.03(10) . .
O2 U1 O8 96.02(10) . .
O4 U1 O8 140.23(8) 3_566 .
O3 U1 O8 141.39(8) . .
O1 U1 O7 93.15(10) . .
O2 U1 O7 88.64(10) . .
O4 U1 O7 151.05(8) 3_566 .
O3 U1 O7 73.97(7) . .
O8 U1 O7 68.38(8) . .
O1 U1 O9 94.26(10) . .
O2 U1 O9 83.99(10) . .
O4 U1 O9 73.30(7) 3_566 .
O3 U1 O9 149.85(7) . .
O8 U1 O9 68.76(8) . .
O7 U1 O9 135.37(7) . .
O5 S1 O6 110.52(14) . .
O5 S1 O4 109.94(14) . .
O6 S1 O4 109.06(15) . .
O5 S1 O3 108.86(13) . .
O6 S1 O3 110.69(13) . .
O4 S1 O3 107.73(13) . .
S1 O3 U1 134.48(13) . .
S1 O4 U1 148.98(14) . 3_566
C1 O7 U1 139.1(2) . .
C2 O8 U1 135.9(2) . .
C1 N2 C2 124.3(2) . .
O7 C1 N1 121.9(3) . .
O7 C1 N2 122.7(3) . .
N1 C1 N2 115.3(3) . .
O8 C2 N3 122.2(3) . .
O8 C2 N2 122.0(3) . .
N3 C2 N2 115.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.760(2) .
U1 O2 1.766(2) .
U1 O4 2.362(2) 3_566
U1 O3 2.365(2) .
U1 O8 2.384(2) .
U1 O7 2.394(2) .
U1 O9 2.474(2) .
S1 O5 1.461(2) .
S1 O6 1.467(2) .
S1 O4 1.477(2) .
S1 O3 1.494(2) .
O4 U1 2.362(2) 3_566
O7 C1 1.253(3) .
O8 C2 1.247(3) .
N1 C1 1.317(4) .
N2 C1 1.377(4) .
N2 C2 1.381(4) .
N3 C2 1.318(4) .
