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#$Date: 2024-04-05 02:05:43 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/80/7248086.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_7248086
loop_
_publ_author_name
'Shore, Madeline C.'
'Nicholas, Aaron D.'
'Vasiliu, Monica'
'Edwards, Kyle C.'
'de Melo, Gabriel F.'
'Bertke, Jeffery A.'
'Dixon, David A.'
'Knope, Karah E.'
_publ_section_title
;
 Structural chemistry of penta- and hexanitrato thorium(iv) complexes
 isolated using N--H donors
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1380
_journal_page_last               1398
_journal_paper_doi               10.1039/D3CE01319G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'N6 O18 Th, 2(C8 H7 N2)'
_chemical_formula_sum            'C16 H14 N10 O18 Th'
_chemical_formula_weight         866.41
_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   geom
_atom_sites_solution_primary     intrinsic
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-06 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.5800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3201(9)
_cell_length_b                   10.8154(5)
_cell_length_c                   13.1377(6)
_cell_measurement_reflns_used    9741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.19
_cell_volume                     2586.4(2)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2018-3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38370
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.385
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    5.873
_exptl_absorpt_correction_T_max  0.39375
_exptl_absorpt_correction_T_min  0.15933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0208
_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)+(0.0119P)²+13.7052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1763
_reflns_number_total             2384
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01319g2.cif
_cod_data_source_block           15_a
_cod_depositor_comments
'Adding full bibliography for 7248080--7248089.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7248086
_shelx_shelxl_version_number     2018/3
_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   0.681
_shelx_estimated_absorpt_t_max   0.746
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
Th1 Th 0.500000 0.74989(3) 0.750000 0.00775(6) Uani 1 2 d S T P . .
N1 N 0.33945(18) 0.7921(3) 0.7025(3) 0.0132(8) Uani 1 1 d . . . . .
O1 O 0.36471(13) 0.7373(3) 0.63612(19) 0.0123(6) Uani 1 1 d . . . . .
O2 O 0.38744(15) 0.8466(2) 0.7820(2) 0.0120(6) Uani 1 1 d . . . . .
O3 O 0.27464(14) 0.7912(3) 0.6916(2) 0.0191(7) Uani 1 1 d . . . . .
N11 N 0.52582(18) 0.5210(3) 0.6350(3) 0.0117(7) Uani 1 1 d . . . . .
O11 O 0.46314(15) 0.5467(3) 0.6410(2) 0.0117(7) Uani 1 1 d . . . . .
O12 O 0.57594(14) 0.6026(2) 0.6729(2) 0.0112(6) Uani 1 1 d . . . . .
O13 O 0.53855(15) 0.4237(2) 0.5974(2) 0.0134(6) Uani 1 1 d . . . . .
N21 N 0.54729(17) 0.8958(3) 0.9545(3) 0.0130(8) Uani 1 1 d . . . . .
O21 O 0.54168(16) 0.9439(3) 0.8626(2) 0.0118(7) Uani 1 1 d . . . . .
O22 O 0.52231(14) 0.7856(2) 0.9504(2) 0.0128(6) Uani 1 1 d . . . . .
O23 O 0.57437(15) 0.9509(2) 1.0386(2) 0.0156(6) Uani 1 1 d . . . . .
N31 N 0.41986(16) 0.2375(4) 0.7177(2) 0.0164(7) Uani 1 1 d . . . . .
N32 N 0.42921(16) 0.2422(4) 0.6195(2) 0.0143(6) Uani 1 1 d . . . . .
H32 H 0.469392 0.278511 0.617045 0.017 Uiso 1 1 calc R U . . .
C31 C 0.3600(2) 0.1831(4) 0.7186(3) 0.0165(9) Uani 1 1 d . . . . .
H31 H 0.351522 0.178342 0.785623 0.020 Uiso 1 1 calc R U . . .
C32 C 0.3065(2) 0.1301(3) 0.6267(3) 0.0114(9) Uani 1 1 d . . . . .
C33 C 0.2425(2) 0.0704(4) 0.6302(3) 0.0151(9) Uani 1 1 d . . . . .
H33 H 0.232366 0.065173 0.696069 0.018 Uiso 1 1 calc R U . . .
C34 C 0.1948(2) 0.0196(4) 0.5367(3) 0.0161(9) Uani 1 1 d . . . . .
H34 H 0.151857 -0.021692 0.538630 0.019 Uiso 1 1 calc R U . . .
C35 C 0.2086(2) 0.0281(4) 0.4395(3) 0.0151(9) Uani 1 1 d . . . . .
H35 H 0.174890 -0.007812 0.376241 0.018 Uiso 1 1 calc R U . . .
C36 C 0.2696(2) 0.0868(4) 0.4329(3) 0.0132(9) Uani 1 1 d . . . . .
H36 H 0.278096 0.092873 0.365968 0.016 Uiso 1 1 calc R U . . .
C37 C 0.3194(2) 0.1380(3) 0.5277(3) 0.0114(9) Uani 1 1 d . . . . .
C38 C 0.3845(2) 0.1983(4) 0.5287(3) 0.0117(8) Uani 1 1 d . . . . .
H38 H 0.395596 0.206856 0.463871 0.014 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
O21 Th1 O21 68.49(12) . 2_656 ?
O21 Th1 O1 116.74(9) . . ?
O21 Th1 O1 68.81(9) 2_656 . ?
O21 Th1 O1 68.81(9) . 2_656 ?
O21 Th1 O1 116.74(9) 2_656 2_656 ?
O1 Th1 O1 173.87(14) . 2_656 ?
O21 Th1 O22 50.37(8) . . ?
O21 Th1 O22 112.81(8) 2_656 . ?
O1 Th1 O22 113.59(8) . . ?
O1 Th1 O22 67.42(8) 2_656 . ?
O21 Th1 O22 112.81(8) . 2_656 ?
O21 Th1 O22 50.37(8) 2_656 2_656 ?
O1 Th1 O22 67.42(8) . 2_656 ?
O1 Th1 O22 113.59(8) 2_656 2_656 ?
O22 Th1 O22 162.59(11) . 2_656 ?
O21 Th1 O2 71.88(9) . . ?
O21 Th1 O2 68.82(9) 2_656 . ?
O1 Th1 O2 50.14(8) . . ?
O1 Th1 O2 133.19(8) 2_656 . ?
O22 Th1 O2 68.25(8) . . ?
O22 Th1 O2 104.33(8) 2_656 . ?
O21 Th1 O2 68.82(9) . 2_656 ?
O21 Th1 O2 71.89(9) 2_656 2_656 ?
O1 Th1 O2 133.19(8) . 2_656 ?
O1 Th1 O2 50.14(8) 2_656 2_656 ?
O22 Th1 O2 104.33(8) . 2_656 ?
O22 Th1 O2 68.25(8) 2_656 2_656 ?
O2 Th1 O2 132.02(12) . 2_656 ?
O21 Th1 O11 113.84(7) . 2_656 ?
O21 Th1 O11 177.24(10) 2_656 2_656 ?
O1 Th1 O11 108.54(9) . 2_656 ?
O1 Th1 O11 65.87(9) 2_656 2_656 ?
O22 Th1 O11 68.73(8) . 2_656 ?
O22 Th1 O11 128.28(9) 2_656 2_656 ?
O2 Th1 O11 110.22(9) . 2_656 ?
O2 Th1 O11 110.16(9) 2_656 2_656 ?
O21 Th1 O11 177.24(10) . . ?
O21 Th1 O11 113.84(7) 2_656 . ?
O1 Th1 O11 65.87(9) . . ?
O1 Th1 O11 108.54(9) 2_656 . ?
O22 Th1 O11 128.28(9) . . ?
O22 Th1 O11 68.74(8) 2_656 . ?
O2 Th1 O11 110.16(9) . . ?
O2 Th1 O11 110.22(8) 2_656 . ?
O11 Th1 O11 63.87(12) 2_656 . ?
O21 Th1 O12 113.01(8) . 2_656 ?
O21 Th1 O12 128.74(9) 2_656 2_656 ?
O1 Th1 O12 65.93(8) . 2_656 ?
O1 Th1 O12 110.00(8) 2_656 2_656 ?
O22 Th1 O12 67.13(8) . 2_656 ?
O22 Th1 O12 125.08(8) 2_656 2_656 ?
O2 Th1 O12 64.24(8) . 2_656 ?
O2 Th1 O12 159.17(8) 2_656 2_656 ?
O11 Th1 O12 49.35(8) 2_656 2_656 ?
O11 Th1 O12 66.90(9) . 2_656 ?
O21 Th1 O12 128.74(9) . . ?
O21 Th1 O12 113.01(8) 2_656 . ?
O1 Th1 O12 110.00(8) . . ?
O1 Th1 O12 65.93(8) 2_656 . ?
O22 Th1 O12 125.08(8) . . ?
O22 Th1 O12 67.13(8) 2_656 . ?
O2 Th1 O12 159.17(8) . . ?
O2 Th1 O12 64.24(8) 2_656 . ?
O11 Th1 O12 66.90(9) 2_656 . ?
O11 Th1 O12 49.35(8) . . ?
O12 Th1 O12 104.11(11) 2_656 . ?
O3 N1 O1 122.1(3) . . ?
O3 N1 O2 122.4(3) . . ?
O1 N1 O2 115.5(3) . . ?
O3 N1 Th1 169.4(2) . . ?
O1 N1 Th1 57.63(16) . . ?
O2 N1 Th1 58.92(17) . . ?
N1 O1 Th1 97.24(19) . . ?
N1 O2 Th1 95.8(2) . . ?
O13 N11 O11 122.6(3) . . ?
O13 N11 O12 121.5(3) . . ?
O11 N11 O12 115.9(3) . . ?
O13 N11 Th1 174.3(2) . . ?
O11 N11 Th1 58.01(18) . . ?
O12 N11 Th1 58.16(17) . . ?
N11 O11 Th1 97.4(2) . . ?
N11 O12 Th1 97.0(2) . . ?
O23 N21 O22 122.5(3) . . ?
O23 N21 O21 122.3(3) . . ?
O22 N21 O21 115.2(3) . . ?
O23 N21 Th1 172.7(2) . . ?
O22 N21 Th1 58.15(17) . . ?
O21 N21 Th1 57.60(18) . . ?
N21 O21 Th1 97.1(2) . . ?
N21 O22 Th1 96.6(2) . . ?
C31 N31 N32 115.2(3) . . ?
C38 N32 N31 126.5(3) . . ?
C38 N32 H32 116.8 . . ?
N31 N32 H32 116.8 . . ?
N31 C31 C32 124.9(4) . . ?
N31 C31 H31 117.6 . . ?
C32 C31 H31 117.6 . . ?
C37 C32 C33 119.2(4) . . ?
C37 C32 C31 117.1(4) . . ?
C33 C32 C31 123.6(4) . . ?
C34 C33 C32 119.0(4) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 121.0(4) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 H34 119.5 . . ?
C36 C35 C34 121.5(4) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
C35 C36 C37 118.4(4) . . ?
C35 C36 H36 120.8 . . ?
C37 C36 H36 120.8 . . ?
C32 C37 C36 120.8(4) . . ?
C32 C37 C38 117.0(4) . . ?
C36 C37 C38 122.2(4) . . ?
N32 C38 C37 119.4(4) . . ?
N32 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
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
Th1 O21 2.538(3) . ?
Th1 O21 2.538(3) 2_656 ?
Th1 O1 2.543(2) . ?
Th1 O1 2.543(2) 2_656 ?
Th1 O22 2.550(3) . ?
Th1 O22 2.550(3) 2_656 ?
Th1 O2 2.571(3) . ?
Th1 O2 2.571(3) 2_656 ?
Th1 O11 2.589(3) 2_656 ?
Th1 O11 2.589(3) . ?
Th1 O12 2.591(3) 2_656 ?
Th1 O12 2.591(3) . ?
N1 O3 1.212(4) . ?
N1 O1 1.278(4) . ?
N1 O2 1.284(4) . ?
N11 O13 1.222(4) . ?
N11 O11 1.270(4) . ?
N11 O12 1.281(4) . ?
N21 O23 1.210(4) . ?
N21 O22 1.281(4) . ?
N21 O21 1.284(4) . ?
N31 C31 1.301(5) . ?
N31 N32 1.363(4) . ?
N32 C38 1.306(5) . ?
N32 H32 0.8800 . ?
C31 C32 1.421(5) . ?
C31 H31 0.9500 . ?
C32 C37 1.407(5) . ?
C32 C33 1.409(5) . ?
C33 C34 1.379(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.394(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.365(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.408(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.412(5) . ?
C38 H38 0.9500 . ?
