#------------------------------------------------------------------------------
#$Date: 2019-11-23 02:13:56 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/65/4346572.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_4346572
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            'C16 H22 N14 O16 U2'
_chemical_formula_weight         1142.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.4520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7642(3)
_cell_length_b                   14.3103(4)
_cell_length_c                   10.9061(3)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.84
_cell_measurement_theta_min      2.45
_cell_volume                     1574.07(8)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36317
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.883
_diffrn_reflns_theta_min         2.449
_exptl_absorpt_coefficient_mu    10.367
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0176P)²+1.4802P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5905
_reflns_number_total             6854
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01699_si_002.cif
_cod_data_source_block           '[C2mim]2[(UO2)(NO3)2N(CN)2)2]'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4346572
_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   0.209
_shelx_estimated_absorpt_t_max   0.456
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_posn
_atom_site_refinement_flags_adp
U1 U 0.29173(2) 0.25554(2) 0.97023(2) 0.01248(2) Uani 1 1 d . .
O1 O 0.39001(16) 0.28004(12) 1.13375(15) 0.0200(3) Uani 1 1 d . .
O2 O 0.19044(17) 0.23277(11) 0.80637(15) 0.0212(3) Uani 1 1 d . .
O3 O 0.09477(17) 0.20070(10) 1.02592(16) 0.0215(3) Uani 1 1 d . .
O4 O 0.10796(16) 0.34868(10) 0.99934(16) 0.0201(3) Uani 1 1 d . .
O5 O -0.06063(17) 0.29224(13) 1.04161(18) 0.0270(3) Uani 1 1 d . .
O6 O 0.28239(16) 0.42691(10) 0.92545(17) 0.0213(3) Uani 1 1 d . .
O7 O 0.44195(17) 0.35300(11) 0.89383(16) 0.0212(3) Uani 1 1 d . .
O8 O 0.42036(19) 0.50279(12) 0.85526(18) 0.0275(3) Uani 1 1 d . .
N1 N 0.8621(2) 0.44211(14) 0.76713(19) 0.0259(4) Uani 1 1 d . .
N3 N 0.7559(2) 0.30979(16) 0.7346(2) 0.0260(4) Uani 1 1 d . .
N4 N 0.4800(2) 0.17102(13) 0.9411(2) 0.0238(4) Uani 1 1 d . .
N5 N 0.67292(19) 0.08049(12) 0.93971(19) 0.0202(3) Uani 1 1 d . .
N6 N 0.7047(2) -0.08849(13) 0.9701(2) 0.0262(4) Uani 1 1 d . .
N7 N 0.04357(18) 0.28043(13) 1.02349(17) 0.0183(3) Uani 1 1 d . .
N8 N 0.38333(19) 0.43111(12) 0.88999(17) 0.0183(3) Uani 1 1 d . .
C2 C 0.8627(2) 0.35479(15) 0.7282(2) 0.0205(4) Uani 1 1 d . .
H2 H 0.9288 0.3279 0.6999 0.025 Uiso 1 1 calc R U
C4 C 0.6844(3) 0.3719(2) 0.7792(3) 0.0380(6) Uani 1 1 d . .
H4 H 0.6035 0.3592 0.7926 0.046 Uiso 1 1 calc R U
C5 C 0.7488(3) 0.4533(2) 0.8003(3) 0.0366(6) Uani 1 1 d . .
H5 H 0.7225 0.5089 0.8322 0.044 Uiso 1 1 calc R U
C6 C 0.9645(3) 0.51239(17) 0.7791(3) 0.0314(5) Uani 1 1 d . .
H6A H 1.0328 0.5087 0.8677 0.038 Uiso 1 1 calc R U
H6B H 0.9242 0.5754 0.7686 0.038 Uiso 1 1 calc R U
C7 C 1.0290(3) 0.49873(19) 0.6788(3) 0.0333(5) Uani 1 1 d . .
H7A H 1.0765 0.4390 0.6943 0.050 Uiso 1 1 calc R U
H7B H 1.0918 0.5497 0.6853 0.050 Uiso 1 1 calc R U
H7C H 0.9610 0.4986 0.5911 0.050 Uiso 1 1 calc R U
C8 C 0.7234(3) 0.21082(18) 0.6981(3) 0.0334(6) Uani 1 1 d . .
H8A H 0.7819 0.1870 0.6537 0.050 Uiso 1 1 calc R U
H8B H 0.6310 0.2061 0.6393 0.050 Uiso 1 1 calc R U
H8C H 0.7358 0.1739 0.7772 0.050 Uiso 1 1 calc R U
C9 C 0.5676(2) 0.12438(13) 0.94044(19) 0.0177(3) Uani 1 1 d . .
C10 C 0.6835(2) -0.00920(14) 0.9555(2) 0.0178(3) 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'
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 178.72(7) . .
O1 U1 N6 88.71(8) . 3_657
O2 U1 N6 92.01(7) . 3_657
O1 U1 N4 89.89(7) . .
O2 U1 N4 91.36(8) . .
N6 U1 N4 67.88(7) 3_657 .
O1 U1 O7 89.82(7) . .
O2 U1 O7 90.47(7) . .
N6 U1 O7 132.63(6) 3_657 .
N4 U1 O7 64.77(6) . .
O1 U1 O6 88.36(7) . .
O2 U1 O6 90.85(7) . .
N6 U1 O6 175.35(6) 3_657 .
N4 U1 O6 115.72(6) . .
O7 U1 O6 50.97(5) . .
O1 U1 O4 89.27(7) . .
O2 U1 O4 89.47(7) . .
N6 U1 O4 115.00(6) 3_657 .
N4 U1 O4 176.98(6) . .
O7 U1 O4 112.32(5) . .
O6 U1 O4 61.35(5) . .
O1 U1 O3 94.36(6) . .
O2 U1 O3 85.00(7) . .
N6 U1 O3 64.77(6) 3_657 .
N4 U1 O3 132.31(6) . .
O7 U1 O3 162.29(5) . .
O6 U1 O3 111.87(5) . .
O4 U1 O3 50.67(5) . .
C2 N1 C5 107.2(2) . .
C2 N1 C6 126.2(2) . .
C5 N1 C6 126.6(2) . .
C2 N3 C4 107.8(2) . .
C2 N3 C8 124.9(2) . .
C4 N3 C8 127.3(2) . .
C9 N4 U1 171.29(17) . .
C10 N5 C9 121.01(19) . .
C10 N6 U1 165.35(18) . 3_657
O5 N7 O3 122.83(19) . .
O5 N7 O4 121.64(18) . .
O3 N7 O4 115.52(17) . .
O5 N7 U1 177.86(15) . .
O3 N7 U1 58.41(10) . .
O4 N7 U1 57.13(10) . .
O8 N8 O6 122.97(19) . .
O8 N8 O7 122.68(19) . .
O6 N8 O7 114.34(16) . .
O8 N8 U1 179.09(14) . .
O6 N8 U1 57.32(9) . .
O7 N8 U1 57.03(9) . .
N1 C2 N3 109.7(2) . .
C5 C4 N3 107.7(2) . .
C4 C5 N1 107.6(2) . .
N1 C6 C7 111.8(2) . .
N4 C9 N5 173.7(2) . .
N6 C10 N5 173.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.7618(15) .
U1 O2 1.7683(16) .
U1 N6 2.4742(19) 3_657
U1 N4 2.4743(19) .
U1 O7 2.4891(16) .
U1 O6 2.4958(15) .
U1 O4 2.4959(15) .
U1 O3 2.5258(16) .
O3 N7 1.263(2) .
O4 N7 1.277(2) .
O5 N7 1.217(2) .
O6 N8 1.276(2) .
O7 N8 1.277(2) .
O8 N8 1.208(2) .
N1 C2 1.321(3) .
N1 C5 1.397(4) .
N1 C6 1.464(4) .
N3 C2 1.340(3) .
N3 C4 1.372(4) .
N3 C8 1.480(4) .
N4 C9 1.157(3) .
N5 C10 1.295(3) .
N5 C9 1.298(3) .
N6 C10 1.157(3) .
N6 U1 2.4742(19) 3_657
C4 C5 1.334(5) .
C6 C7 1.500(4) .
