#------------------------------------------------------------------------------
#$Date: 2020-05-05 15:46:15 +0300 (Tue, 05 May 2020) $
#$Revision: 251570 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/61/7126197.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_7126197
loop_
_publ_author_name
'Kelley, Steven P.'
'Smetana, Volodymyr'
'Emerson, Stephen D.'
'Mudring, Anja-Verena'
'Rogers, Robin D.'
_publ_section_title
;
 Benchtop access to anhydrous actinide N-donor coordination complexes
 using ionic liquids.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4232
_journal_page_last               4235
_journal_paper_doi               10.1039/c9cc09852f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C16 H25 N13 O15 Th'
_chemical_formula_weight         871.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8468(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7287(13)
_cell_length_b                   12.9810(10)
_cell_length_c                   14.2585(12)
_cell_measurement_reflns_used    9522
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      4.24
_cell_volume                     2876.6(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      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13530
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.122
_diffrn_reflns_theta_min         4.276
_exptl_absorpt_coefficient_mu    5.276
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Polyhedral
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0167
_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)+(0.0245P)²+2.3435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3344
_reflns_number_total             3485
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc09852f2.cif
_cod_data_source_block           Th(NO3)5(mim)2mimHim
_cod_depositor_comments
'Adding full bibliography for 7126194--7126200.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7126197
_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   0.467
_shelx_estimated_absorpt_t_max   0.620
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th Th 0.5000 0.19208(2) 0.2500 0.01061(4) Uani 1 2 d S T P . .
O4 O 0.41775(10) 0.27636(12) 0.10059(10) 0.0172(3) Uani 1 1 d . . . . .
O3 O 0.54351(10) 0.21841(12) 0.08417(10) 0.0159(3) Uani 1 1 d . . . . .
O5 O 0.46401(12) 0.29436(13) -0.03512(12) 0.0242(4) Uani 1 1 d . . . . .
O6 O 0.42792(10) 0.06351(12) 0.12231(10) 0.0164(3) Uani 1 1 d . . . . .
O7 O 0.55846(10) 0.02631(11) 0.18348(10) 0.0158(3) Uani 1 1 d . . . . .
O8 O 0.48716(11) -0.07717(13) 0.07974(11) 0.0244(3) Uani 1 1 d . . . . .
O1 O 0.55783(10) 0.37390(12) 0.21797(11) 0.0174(3) Uani 1 1 d . . . . .
O2 O 0.5000 0.51997(17) 0.2500 0.0301(6) Uani 1 2 d S T P . .
N7 N 0.33144(12) 0.18786(13) 0.24559(13) 0.0151(4) Uani 1 1 d . . . . .
N9 N 0.19859(12) 0.22736(16) 0.26481(13) 0.0186(4) Uani 1 1 d . . . . .
N14 N 0.47460(12) 0.26386(14) 0.04645(12) 0.0159(3) Uani 1 1 d . . . . .
N15 N 0.49093(12) 0.00121(14) 0.12639(12) 0.0149(3) Uani 1 1 d . . . . .
N13 N 0.5000 0.4267(2) 0.2500 0.0175(5) Uani 1 2 d S T P . .
N1 N 0.75208(12) 0.51457(14) -0.03887(12) 0.0168(4) Uani 1 1 d . . . . .
N3 N 0.73706(14) 0.35107(16) -0.01153(15) 0.0245(4) Uani 1 1 d . . . . .
H3 H 0.749(5) 0.298(4) -0.011(5) 0.037 Uiso 0.5 1 d . U P . .
C8 C 0.28135(14) 0.25781(17) 0.27664(15) 0.0172(4) Uani 1 1 d . . . . .
H8A H 0.3013 0.3218 0.3040 0.021 Uiso 1 1 calc R U . . .
C10 C 0.19451(15) 0.13198(19) 0.22361(17) 0.0236(5) Uani 1 1 d . . . . .
H10A H 0.1446 0.0908 0.2066 0.028 Uiso 1 1 calc R U . . .
C11 C 0.27624(15) 0.10806(19) 0.21194(17) 0.0226(5) Uani 1 1 d . . . . .
H11A H 0.2932 0.0460 0.1848 0.027 Uiso 1 1 calc R U . . .
C12 C 0.12580(17) 0.2855(2) 0.2898(2) 0.0299(6) Uani 1 1 d . . . . .
H12A H 0.1469 0.3478 0.3246 0.045 Uiso 1 1 calc R U . . .
H12B H 0.0944 0.2428 0.3297 0.045 Uiso 1 1 calc R U . . .
H12C H 0.0873 0.3049 0.2318 0.045 Uiso 1 1 calc R U . . .
C2 C 0.78964(15) 0.42192(18) -0.03559(15) 0.0198(4) Uani 1 1 d . . . . .
H2A H 0.8461 0.4091 -0.0487 0.024 Uiso 1 1 calc R U . . .
C4 C 0.66293(17) 0.4007(2) 0.0019(2) 0.0341(6) Uani 1 1 d . . . . .
H4A H 0.6136 0.3689 0.0202 0.041 Uiso 1 1 calc R U . . .
C5 C 0.67162(16) 0.5021(2) -0.0150(2) 0.0289(5) Uani 1 1 d . . . . .
H5A H 0.6301 0.5545 -0.0112 0.035 Uiso 1 1 calc R U . . .
C6 C 0.78977(16) 0.61276(19) -0.06030(18) 0.0259(5) Uani 1 1 d . . . . .
H6A H 0.8434 0.6003 -0.0856 0.039 Uiso 1 1 calc R U . . .
H6B H 0.8020 0.6540 -0.0022 0.039 Uiso 1 1 calc R U . . .
H6C H 0.7493 0.6500 -0.1075 0.039 Uiso 1 1 calc R U . . .
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'
Th Th -7.2400 8.8979 '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
_geom_angle_publ_flag
O4 Th O4 129.44(7) 2_655 . ?
O4 Th O7 102.34(5) 2_655 2_655 ?
O4 Th O7 119.96(5) . 2_655 ?
O4 Th O7 119.96(5) 2_655 . ?
O4 Th O7 102.34(5) . . ?
O7 Th O7 66.80(7) 2_655 . ?
O4 Th O3 122.26(5) 2_655 . ?
O4 Th O3 49.71(5) . . ?
O7 Th O3 127.37(5) 2_655 . ?
O7 Th O3 67.29(5) . . ?
O4 Th O3 49.71(5) 2_655 2_655 ?
O4 Th O3 122.26(5) . 2_655 ?
O7 Th O3 67.29(5) 2_655 2_655 ?
O7 Th O3 127.37(5) . 2_655 ?
O3 Th O3 164.80(7) . 2_655 ?
O4 Th O1 67.17(5) 2_655 . ?
O4 Th O1 67.11(5) . . ?
O7 Th O1 168.12(5) 2_655 . ?
O7 Th O1 122.68(5) . . ?
O3 Th O1 64.49(5) . . ?
O3 Th O1 100.96(5) 2_655 . ?
O4 Th O1 67.11(5) 2_655 2_655 ?
O4 Th O1 67.17(5) . 2_655 ?
O7 Th O1 122.69(5) 2_655 2_655 ?
O7 Th O1 168.12(5) . 2_655 ?
O3 Th O1 100.96(5) . 2_655 ?
O3 Th O1 64.48(5) 2_655 2_655 ?
O1 Th O1 49.13(6) . 2_655 ?
O4 Th O6 65.25(5) 2_655 2_655 ?
O4 Th O6 165.30(5) . 2_655 ?
O7 Th O6 49.29(5) 2_655 2_655 ?
O7 Th O6 65.14(5) . 2_655 ?
O3 Th O6 125.30(5) . 2_655 ?
O3 Th O6 65.93(5) 2_655 2_655 ?
O1 Th O6 125.49(5) . 2_655 ?
O1 Th O6 126.01(5) 2_655 2_655 ?
O4 Th O6 165.30(5) 2_655 . ?
O4 Th O6 65.25(5) . . ?
O7 Th O6 65.14(5) 2_655 . ?
O7 Th O6 49.29(5) . . ?
O3 Th O6 65.93(5) . . ?
O3 Th O6 125.30(5) 2_655 . ?
O1 Th O6 126.01(5) . . ?
O1 Th O6 125.49(5) 2_655 . ?
O6 Th O6 100.06(7) 2_655 . ?
O4 Th N7 67.20(5) 2_655 2_655 ?
O4 Th N7 113.90(5) . 2_655 ?
O7 Th N7 112.79(5) 2_655 2_655 ?
O7 Th N7 65.05(5) . 2_655 ?
O3 Th N7 67.57(5) . 2_655 ?
O3 Th N7 112.77(5) 2_655 2_655 ?
O1 Th N7 69.24(5) . 2_655 ?
O1 Th N7 113.09(5) 2_655 2_655 ?
O6 Th N7 69.02(5) 2_655 2_655 ?
O6 Th N7 109.35(5) . 2_655 ?
O4 Th N7 113.90(5) 2_655 . ?
O4 Th N7 67.20(5) . . ?
O7 Th N7 65.05(5) 2_655 . ?
O7 Th N7 112.79(5) . . ?
O3 Th N7 112.77(5) . . ?
O3 Th N7 67.57(5) 2_655 . ?
O1 Th N7 113.09(5) . . ?
O1 Th N7 69.24(5) 2_655 . ?
O6 Th N7 109.35(5) 2_655 . ?
O6 Th N7 69.02(5) . . ?
N7 Th N7 177.63(7) 2_655 . ?
N14 O4 Th 97.90(11) . . ?
N14 O3 Th 96.86(11) . . ?
N15 O6 Th 97.09(11) . . ?
N15 O7 Th 97.97(11) . . ?
N13 O1 Th 97.86(13) . . ?
C8 N7 C11 104.76(19) . . ?
C8 N7 Th 128.68(14) . . ?
C11 N7 Th 126.53(14) . . ?
C8 N9 C10 107.48(18) . . ?
C8 N9 C12 126.7(2) . . ?
C10 N9 C12 125.8(2) . . ?
O5 N14 O3 122.39(18) . . ?
O5 N14 O4 122.06(19) . . ?
O3 N14 O4 115.54(16) . . ?
O5 N14 Th 178.94(15) . . ?
O3 N14 Th 58.26(9) . . ?
O4 N14 Th 57.28(9) . . ?
O8 N15 O6 122.42(18) . . ?
O8 N15 O7 121.98(18) . . ?
O6 N15 O7 115.60(16) . . ?
O8 N15 Th 177.72(14) . . ?
O6 N15 Th 58.27(9) . . ?
O7 N15 Th 57.36(9) . . ?
O2 N13 O1 122.42(12) . 2_655 ?
O2 N13 O1 122.42(12) . . ?
O1 N13 O1 115.2(2) 2_655 . ?
O2 N13 Th 180.0 . . ?
O1 N13 Th 57.58(12) 2_655 . ?
O1 N13 Th 57.58(12) . . ?
C2 N1 C5 107.77(19) . . ?
C2 N1 C6 127.00(19) . . ?
C5 N1 C6 125.2(2) . . ?
C2 N3 C4 106.9(2) . . ?
N7 C8 N9 111.8(2) . . ?
C11 C10 N9 106.1(2) . . ?
C10 C11 N7 109.9(2) . . ?
N3 C2 N1 110.2(2) . . ?
C5 C4 N3 108.7(2) . . ?
C4 C5 N1 106.4(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th O4 2.5614(15) 2_655 ?
Th O4 2.5614(15) . ?
Th O7 2.5776(15) 2_655 ?
Th O7 2.5776(15) . ?
Th O3 2.5833(14) . ?
Th O3 2.5834(14) 2_655 ?
Th O1 2.5951(15) . ?
Th O1 2.5951(15) 2_655 ?
Th O6 2.5981(15) 2_655 ?
Th O6 2.5981(15) . ?
Th N7 2.6428(19) 2_655 ?
Th N7 2.6428(19) . ?
O4 N14 1.278(2) . ?
O3 N14 1.278(2) . ?
O5 N14 1.215(2) . ?
O6 N15 1.273(2) . ?
O7 N15 1.277(2) . ?
O8 N15 1.212(2) . ?
O1 N13 1.278(2) . ?
O2 N13 1.211(3) . ?
N7 C8 1.322(3) . ?
N7 C11 1.389(3) . ?
N9 C8 1.346(3) . ?
N9 C10 1.368(3) . ?
N9 C12 1.460(3) . ?
N13 O1 1.278(2) 2_655 ?
N1 C2 1.338(3) . ?
N1 C5 1.370(3) . ?
N1 C6 1.458(3) . ?
N3 C2 1.317(3) . ?
N3 C4 1.371(3) . ?
C10 C11 1.357(3) . ?
C4 C5 1.350(4) . ?
