#------------------------------------------------------------------------------
#$Date: 2022-06-28 19:22:54 +0300 (Tue, 28 Jun 2022) $
#$Revision: 276345 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/65/4346574.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_4346574
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            'C17 H21 N7 O9 U2'
_chemical_formula_weight         943.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                102.123(5)
_cell_angle_beta                 96.577(6)
_cell_angle_gamma                103.460(5)
_cell_formula_units_Z            2
_cell_length_a                   10.0087(8)
_cell_length_b                   10.6432(8)
_cell_length_c                   12.4241(10)
_cell_measurement_reflns_used    2921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.31
_cell_volume                     1239.69(18)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.970
_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  0.0769
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16262
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.584
_diffrn_reflns_theta_min         2.029
_exptl_absorpt_coefficient_mu    13.106
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.606
_refine_diff_density_min         -1.824
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0337
_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)+(0.0214P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3060
_reflns_number_total             4509
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01699_si_002.cif
_cod_data_source_block
'[(C2CN)(C4CN)Im]2n[{(UO2)4(O)2(OAc)4(N(CN)2)2}n]'
_cod_original_cell_volume        1239.69(17)
_cod_database_code               4346574
_shelx_shelxl_version_number     2014/7
_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   0.461
_shelx_estimated_absorpt_t_max   0.695
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
U1 U 0.25560(4) 0.00386(3) 0.28531(3) 0.02077(12) Uani 1 1 d . .
U2 U 0.41451(4) -0.18192(3) 0.48427(3) 0.02029(11) Uani 1 1 d . .
O1 O 0.3484(7) -0.0263(6) 0.1750(5) 0.0317(17) Uani 1 1 d . .
O2 O 0.1479(6) 0.0307(6) 0.3863(5) 0.0265(16) Uani 1 1 d . .
O3 O 0.5350(7) -0.2331(6) 0.4006(6) 0.0301(17) Uani 1 1 d . .
O4 O 0.2848(7) -0.1433(6) 0.5641(5) 0.0289(16) Uani 1 1 d . .
O5 O 0.4238(7) -0.0020(5) 0.4105(5) 0.0259(16) Uani 1 1 d . .
O6 O 0.2315(7) -0.2185(6) 0.3047(5) 0.0291(17) Uani 1 1 d . .
O7 O 0.2436(7) -0.3954(6) 0.3632(5) 0.0307(17) Uani 1 1 d . .
O8 O 0.4004(7) -0.3798(6) 0.5692(6) 0.0351(18) Uani 1 1 d . .
O9 O 0.5870(7) -0.2198(6) 0.6445(5) 0.0328(18) Uani 1 1 d . .
N1 N -0.2776(8) -0.1852(7) 0.2439(6) 0.0247(19) Uani 1 1 d . .
N3 N -0.1485(8) -0.2629(7) 0.3522(6) 0.0246(19) Uani 1 1 d . .
N4 N -0.3906(13) 0.3692(9) 0.0242(9) 0.063(3) Uani 1 1 d . .
N5 N 0.0617(11) -0.3884(8) 0.6667(7) 0.042(2) Uani 1 1 d . .
N6 N 0.0401(9) -0.1381(7) 0.1494(7) 0.030(2) Uani 1 1 d . .
N7 N -0.1215(11) -0.2493(7) -0.0255(7) 0.044(3) Uani 1 1 d . .
N8 N -0.1551(10) -0.1534(8) -0.1851(8) 0.041(2) Uani 1 1 d . .
C2 C -0.1921(10) -0.1573(9) 0.3393(8) 0.025(2) Uani 1 1 d . .
H2A H -0.1652 -0.0732 0.3919 0.029 Uiso 1 1 calc R U
C4 C -0.2126(11) -0.3650(9) 0.2579(8) 0.030(2) Uani 1 1 d . .
H4A H -0.2020 -0.4531 0.2433 0.036 Uiso 1 1 calc R U
C5 C -0.2920(11) -0.3168(8) 0.1914(9) 0.029(2) Uani 1 1 d . .
H5A H -0.3478 -0.3643 0.1211 0.035 Uiso 1 1 calc R U
C6 C -0.3534(10) -0.0956(9) 0.2077(8) 0.025(2) Uani 1 1 d . .
H6A H -0.3914 -0.0519 0.2711 0.030 Uiso 1 1 calc R U
H6B H -0.4328 -0.1478 0.1477 0.030 Uiso 1 1 calc R U
C7 C -0.2590(11) 0.0111(10) 0.1644(9) 0.035(3) Uani 1 1 d . .
H7A H -0.1749 0.0577 0.2216 0.041 Uiso 1 1 calc R U
H7B H -0.2286 -0.0317 0.0962 0.041 Uiso 1 1 calc R U
C8 C -0.3365(12) 0.1117(9) 0.1378(9) 0.035(3) Uani 1 1 d . .
H8A H -0.4260 0.0637 0.0875 0.042 Uiso 1 1 calc R U
H8B H -0.3575 0.1614 0.2078 0.042 Uiso 1 1 calc R U
C9 C -0.2515(12) 0.2089(9) 0.0828(9) 0.035(3) Uani 1 1 d . .
H9A H -0.1646 0.2607 0.1352 0.042 Uiso 1 1 calc R U
H9B H -0.2252 0.1586 0.0157 0.042 Uiso 1 1 calc R U
C10 C -0.3270(13) 0.3005(11) 0.0503(9) 0.042(3) Uani 1 1 d . .
C11 C -0.0517(11) -0.2706(9) 0.4470(8) 0.031(3) Uani 1 1 d . .
H11A H -0.0017 -0.1792 0.4908 0.037 Uiso 1 1 calc R U
H11B H 0.0183 -0.3149 0.4186 0.037 Uiso 1 1 calc R U
C12 C -0.1262(11) -0.3467(9) 0.5227(8) 0.029(2) Uani 1 1 d . .
H12A H -0.1837 -0.2945 0.5622 0.035 Uiso 1 1 calc R U
H12B H -0.1888 -0.4325 0.4774 0.035 Uiso 1 1 calc R U
C13 C -0.0226(12) -0.3720(9) 0.6052(9) 0.028(2) Uani 1 1 d . .
C14 C 0.2065(10) -0.3447(9) 0.2863(8) 0.025(2) Uani 1 1 d . .
C15 C 0.1338(13) -0.4302(9) 0.1741(8) 0.042(3) Uani 1 1 d . .
H15A H 0.0568 -0.3961 0.1471 0.063 Uiso 1 1 calc R U
H15B H 0.0971 -0.5218 0.1798 0.063 Uiso 1 1 calc R U
H15C H 0.1999 -0.4286 0.1216 0.063 Uiso 1 1 calc R U
C16 C 0.5062(11) -0.3391(9) 0.6400(8) 0.028(2) Uani 1 1 d . .
C17 C 0.5508(11) -0.4148(9) 0.7162(9) 0.033(3) Uani 1 1 d . .
H17A H 0.4867 -0.5042 0.6980 0.050 Uiso 1 1 calc R U
H17B H 0.5503 -0.3691 0.7933 0.050 Uiso 1 1 calc R U
H17C H 0.6453 -0.4219 0.7084 0.050 Uiso 1 1 calc R U
C18 C -0.0345(11) -0.1849(8) 0.0651(8) 0.025(2) Uani 1 1 d . .
C19 C -0.1334(11) -0.1927(8) -0.1073(8) 0.026(2) 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 174.5(3) . .
O1 U1 O5 93.3(3) . .
O2 U1 O5 92.0(3) . .
O1 U1 O9 89.7(3) . 2_656
O2 U1 O9 93.4(3) . 2_656
O5 U1 O9 69.7(2) . 2_656
O1 U1 O6 90.4(3) . .
O2 U1 O6 90.2(3) . .
O5 U1 O6 69.6(2) . .
O9 U1 O6 139.3(2) 2_656 .
O1 U1 N6 86.7(3) . .
O2 U1 N6 88.2(3) . .
O5 U1 N6 143.6(2) . .
O9 U1 N6 146.7(2) 2_656 .
O6 U1 N6 73.9(2) . .
O1 U1 N8 87.6(3) . 2
O2 U1 N8 88.9(3) . 2
O5 U1 N8 144.5(2) . 2
O9 U1 N8 74.8(2) 2_656 2
O6 U1 N8 145.9(2) . 2
N6 U1 N8 71.9(3) . 2
O1 U1 U2 99.6(2) . .
O2 U1 U2 84.4(2) . .
O5 U1 U2 29.83(14) . .
O9 U1 U2 98.95(16) 2_656 .
O6 U1 U2 41.10(15) . .
N6 U1 U2 114.35(18) . .
N8 U1 U2 170.6(2) 2 .
O1 U1 U2 95.6(2) . 2_656
O2 U1 U2 89.7(2) . 2_656
O5 U1 U2 28.78(14) . 2_656
O9 U1 U2 41.25(16) 2_656 2_656
O6 U1 U2 98.31(15) . 2_656
N6 U1 U2 171.96(18) . 2_656
N8 U1 U2 115.81(19) 2 2_656
U2 U1 U2 57.702(11) . 2_656
O3 U2 O4 175.6(3) . .
O3 U2 O5 93.2(3) . 2_656
O4 U2 O5 91.0(3) . 2_656
O3 U2 O5 90.8(3) . .
O4 U2 O5 92.0(3) . .
O5 U2 O5 67.9(2) 2_656 .
O3 U2 O8 90.6(3) . .
O4 U2 O8 86.7(3) . .
O5 U2 O8 112.0(2) 2_656 .
O5 U2 O8 178.6(2) . .
O3 U2 O7 83.8(3) . .
O4 U2 O7 91.9(2) . .
O5 U2 O7 176.7(2) 2_656 .
O5 U2 O7 113.5(2) . .
O8 U2 O7 66.8(2) . .
O3 U2 O6 90.6(3) . .
O4 U2 O6 87.4(3) . .
O5 U2 O6 131.81(19) 2_656 .
O5 U2 O6 64.1(2) . .
O8 U2 O6 116.0(2) . .
O7 U2 O6 49.84(19) . .
O3 U2 O9 82.2(3) . .
O4 U2 O9 98.6(3) . .
O5 U2 O9 63.82(19) 2_656 .
O5 U2 O9 130.57(19) . .
O8 U2 O9 49.6(2) . .
O7 U2 O9 114.24(19) . .
O6 U2 O9 163.47(18) . .
O3 U2 C14 83.0(3) . .
O4 U2 C14 93.6(3) . .
O5 U2 C14 156.1(2) 2_656 .
O5 U2 C14 88.6(2) . .
O8 U2 C14 91.7(2) . .
O7 U2 C14 24.9(2) . .
O6 U2 C14 25.5(2) . .
O9 U2 C14 138.1(2) . .
O3 U2 C16 86.9(3) . .
O4 U2 C16 92.0(3) . .
O5 U2 C16 89.0(2) 2_656 .
O5 U2 C16 156.6(2) . .
O8 U2 C16 23.5(2) . .
O7 U2 C16 89.5(2) . .
O6 U2 C16 139.2(2) . .
O9 U2 C16 26.1(2) . .
C14 U2 C16 114.2(3) . .
O3 U2 U2 92.40(19) . 2_656
O4 U2 U2 91.80(18) . 2_656
O5 U2 U2 34.06(14) 2_656 2_656
O5 U2 U2 33.81(15) . 2_656
O8 U2 U2 146.02(16) . 2_656
O7 U2 U2 147.19(15) . 2_656
O6 U2 U2 97.82(13) . 2_656
O9 U2 U2 97.36(12) . 2_656
C14 U2 U2 122.27(19) . 2_656
C16 U2 U2 122.97(19) . 2_656
O3 U2 U1 97.3(2) . .
O4 U2 U1 83.5(2) . .
O5 U2 U1 95.12(15) 2_656 .
O5 U2 U1 28.40(15) . .
O8 U2 U1 151.32(16) . .
O7 U2 U1 86.67(15) . .
O6 U2 U1 36.85(12) . .
O9 U2 U1 158.79(12) . .
C14 U2 U1 62.23(19) . .
C16 U2 U1 173.9(2) . .
U2 U2 U1 61.432(11) 2_656 .
U1 O5 U2 123.6(3) . 2_656
U1 O5 U2 121.8(3) . .
U2 O5 U2 112.1(2) 2_656 .
C14 O6 U1 164.3(6) . .
C14 O6 U2 92.3(5) . .
U1 O6 U2 102.0(2) . .
C14 O7 U2 95.9(5) . .
C16 O8 U2 100.8(6) . .
C16 O9 U1 161.5(6) . 2_656
C16 O9 U2 92.6(5) . .
U1 O9 U2 102.2(2) 2_656 .
C2 N1 C5 107.7(8) . .
C2 N1 C6 125.0(8) . .
C5 N1 C6 127.0(8) . .
C2 N3 C4 106.5(8) . .
C2 N3 C11 126.9(8) . .
C4 N3 C11 126.6(8) . .
C18 N6 U1 158.4(8) . .
C18 N7 C19 119.3(8) . .
C19 N8 U1 151.6(8) . 2
N1 C2 N3 110.7(8) . .
C5 C4 N3 107.7(8) . .
C4 C5 N1 107.4(8) . .
N1 C6 C7 111.4(8) . .
C8 C7 C6 110.5(9) . .
C9 C8 C7 111.5(9) . .
C10 C9 C8 112.4(9) . .
N4 C10 C9 177.6(13) . .
N3 C11 C12 112.0(8) . .
C13 C12 C11 109.8(8) . .
N5 C13 C12 176.9(11) . .
O7 C14 O6 119.3(8) . .
O7 C14 C15 120.9(8) . .
O6 C14 C15 119.8(9) . .
O7 C14 U2 59.2(5) . .
O6 C14 U2 62.2(5) . .
C15 C14 U2 165.4(7) . .
O8 C16 O9 116.9(9) . .
O8 C16 C17 124.6(9) . .
O9 C16 C17 118.5(9) . .
O8 C16 U2 55.6(5) . .
O9 C16 U2 61.3(5) . .
C17 C16 U2 179.7(7) . .
N6 C18 N7 173.6(10) . .
N8 C19 N7 173.0(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.758(7) .
U1 O2 1.766(6) .
U1 O5 2.179(6) .
U1 O9 2.383(6) 2_656
U1 O6 2.388(6) .
U1 N6 2.522(8) .
U1 N8 2.527(8) 2
U1 U2 3.8943(5) .
U1 U2 3.9155(6) 2_656
U2 O3 1.785(7) .
U2 O4 1.792(7) .
U2 O5 2.264(6) 2_656
U2 O5 2.278(6) .
U2 O8 2.529(6) .
U2 O7 2.553(6) .
U2 O6 2.618(6) .
U2 O9 2.642(7) .
U2 C14 2.957(9) .
U2 C16 3.009(10) .
U2 U2 3.7686(7) 2_656
O5 U2 2.264(6) 2_656
O6 C14 1.273(10) .
O7 C14 1.253(11) .
O8 C16 1.223(11) .
O9 C16 1.324(11) .
O9 U1 2.383(6) 2_656
N1 C2 1.314(12) .
N1 C5 1.382(11) .
N1 C6 1.458(11) .
N3 C2 1.330(11) .
N3 C4 1.390(12) .
N3 C11 1.465(12) .
N4 C10 1.147(14) .
N5 C13 1.141(12) .
N6 C18 1.154(11) .
N7 C18 1.292(12) .
N7 C19 1.294(12) .
N8 C19 1.149(12) .
N8 U1 2.527(8) 2
C4 C5 1.340(13) .
C6 C7 1.531(13) .
C7 C8 1.528(13) .
C8 C9 1.510(13) .
C9 C10 1.457(15) .
C11 C12 1.515(13) .
C12 C13 1.484(15) .
C14 C15 1.493(13) .
C16 C17 1.462(13) .
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-06-28T19:21:00+03:00
;
 Removed the '_chemical_name_systematic' data item that had an incorrect value.
;
