#------------------------------------------------------------------------------
#$Date: 2024-04-05 02:05:43 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/80/7248080.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_7248080
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         'H4 N5 O17 Th, C4 H12 N2, N O3'
_chemical_formula_sum            'C4 H16 N8 O20 Th'
_chemical_formula_weight         728.29
_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   mixed
_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                 97.576(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8020(5)
_cell_length_b                   21.332(2)
_cell_length_c                   13.2767(12)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.46
_cell_volume                     1909.6(3)
_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 0.998
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58650
_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         27.903
_diffrn_reflns_theta_min         1.818
_exptl_absorpt_coefficient_mu    7.931
_exptl_absorpt_correction_T_max  0.59538
_exptl_absorpt_correction_T_min  0.27178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.365
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0142
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0121P)²+1.8689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4275
_reflns_number_total             4548
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01319g2.cif
_cod_data_source_block           B21057_a
_cod_depositor_comments
'Adding full bibliography for 7248080--7248089.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7248080
_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   0.277
_shelx_estimated_absorpt_t_max   0.559
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.88275(2) 0.24580(2) 0.72581(2) 0.00616(3) Uani 1 1 d . . . . .
N1 N 0.9776(3) 0.35906(8) 0.85778(13) 0.0107(3) Uani 1 1 d . . . . .
O1 O 0.8192(2) 0.32716(7) 0.86152(11) 0.0113(3) Uani 1 1 d . . . . .
O2 O 1.1070(2) 0.33342(7) 0.80976(11) 0.0118(3) Uani 1 1 d . . . . .
O3 O 1.0008(2) 0.41101(7) 0.89568(12) 0.0157(3) Uani 1 1 d . . . . .
N11 N 0.6027(3) 0.35493(8) 0.66700(13) 0.0114(4) Uani 1 1 d . . . . .
O11 O 0.5368(2) 0.30152(7) 0.69382(11) 0.0108(3) Uani 1 1 d . . . . .
O12 O 0.7877(2) 0.35656(7) 0.66006(11) 0.0114(3) Uani 1 1 d . . . . .
O13 O 0.4950(2) 0.39972(7) 0.65010(14) 0.0224(4) Uani 1 1 d . . . . .
N21 N 0.5835(3) 0.21130(8) 0.54420(13) 0.0097(3) Uani 1 1 d . . . . .
O21 O 0.7176(2) 0.25313(6) 0.53706(12) 0.0101(3) Uani 1 1 d . . . . .
O22 O 0.5970(2) 0.18254(7) 0.62900(11) 0.0111(3) Uani 1 1 d . . . . .
O23 O 0.4531(2) 0.20072(7) 0.47474(11) 0.0142(3) Uani 1 1 d . . . . .
N31 N 0.9437(2) 0.11200(8) 0.65914(13) 0.0101(3) Uani 1 1 d . . . . .
O31 O 0.9925(2) 0.15865(7) 0.60800(11) 0.0123(3) Uani 1 1 d . . . . .
O32 O 0.9094(2) 0.12429(7) 0.74951(11) 0.0111(3) Uani 1 1 d . . . . .
O33 O 0.9259(2) 0.05888(7) 0.62370(12) 0.0151(3) Uani 1 1 d . . . . .
N41 N 1.2109(3) 0.19469(8) 0.88327(13) 0.0091(3) Uani 1 1 d . . . . .
O41 O 1.2402(2) 0.20413(7) 0.79172(11) 0.0106(3) Uani 1 1 d . . . . .
O42 O 1.0435(2) 0.21392(7) 0.90620(11) 0.0102(3) Uani 1 1 d . . . . .
O43 O 1.3311(2) 0.16897(7) 0.94563(11) 0.0138(3) Uani 1 1 d . . . . .
N51 N 0.5857(3) 0.52826(8) 0.68454(14) 0.0127(4) Uani 1 1 d . . . . .
N61 N 0.3476(3) 0.50726(8) 0.06597(14) 0.0120(4) Uani 1 1 d . . . . .
H61A H 0.243415 0.521510 0.021885 0.014 Uiso 1 1 calc R U . . .
H61B H 0.307893 0.504365 0.128615 0.014 Uiso 1 1 calc R U . . .
N71 N 0.0795(3) 0.51792(8) 0.60261(13) 0.0123(4) Uani 1 1 d . . . . .
H71A H 0.185109 0.525490 0.650643 0.015 Uiso 1 1 calc R U . . .
H71B H -0.033195 0.524676 0.631114 0.015 Uiso 1 1 calc R U . . .
O51 O 0.7544(2) 0.51710(8) 0.73502(12) 0.0173(3) Uani 1 1 d . . . . .
O52 O 0.4366(2) 0.52965(8) 0.73209(11) 0.0152(3) Uani 1 1 d . . . . .
O53 O 0.5684(3) 0.53714(8) 0.59217(12) 0.0208(4) Uani 1 1 d . . . . .
C61 C 0.5166(3) 0.55261(10) 0.06954(17) 0.0140(4) Uani 1 1 d . . . . .
H61C H 0.625610 0.539057 0.121853 0.017 Uiso 1 1 calc R U . . .
H61D H 0.472156 0.594647 0.088657 0.017 Uiso 1 1 calc R U . . .
C62 C 0.5916(3) 0.55623(10) -0.03276(16) 0.0124(4) Uani 1 1 d . . . . .
H62A H 0.486009 0.573263 -0.083859 0.015 Uiso 1 1 calc R U . . .
H62B H 0.706547 0.585051 -0.028176 0.015 Uiso 1 1 calc R U . . .
C72 C 0.0850(3) 0.45127(10) 0.56796(16) 0.0122(4) Uani 1 1 d . . . . .
H72A H 0.075870 0.422877 0.626149 0.015 Uiso 1 1 calc R U . . .
H72B H 0.212350 0.443006 0.541951 0.015 Uiso 1 1 calc R U . . .
C74 C 0.0853(3) 0.56169(10) 0.51492(16) 0.0123(4) Uani 1 1 d . . . . .
H74A H 0.212672 0.556580 0.487307 0.015 Uiso 1 1 calc R U . . .
H74B H 0.077174 0.605505 0.538602 0.015 Uiso 1 1 calc R U . . .
O81 O 1.1265(2) 0.28461(8) 0.62068(13) 0.0120(3) Uani 1 1 d . . . . .
H1 H 1.108(4) 0.2839(13) 0.561(2) 0.018 Uiso 1 1 d . U . . .
H2 H 1.230(4) 0.2919(13) 0.643(2) 0.018 Uiso 1 1 d . U . . .
O91 O 0.6568(2) 0.20341(7) 0.83595(12) 0.0109(3) Uani 1 1 d . . . . .
H4 H 0.668(4) 0.2171(13) 0.895(2) 0.016 Uiso 1 1 d . U . . .
H3 H 0.549(4) 0.1997(13) 0.815(2) 0.016 Uiso 1 1 d . 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
O91 Th1 O81 176.48(5) . . ?
O91 Th1 O22 66.97(5) . . ?
O81 Th1 O22 114.66(5) . . ?
O91 Th1 O12 113.29(5) . . ?
O81 Th1 O12 69.78(5) . . ?
O22 Th1 O12 99.97(5) . . ?
O91 Th1 O2 113.29(5) . . ?
O81 Th1 O2 66.03(5) . . ?
O22 Th1 O2 164.91(5) . . ?
O12 Th1 O2 65.64(5) . . ?
O91 Th1 O1 69.67(5) . . ?
O81 Th1 O1 111.05(5) . . ?
O22 Th1 O1 121.19(5) . . ?
O12 Th1 O1 63.97(5) . . ?
O2 Th1 O1 49.65(5) . . ?
O91 Th1 O42 64.49(5) . . ?
O81 Th1 O42 112.40(5) . . ?
O22 Th1 O42 121.64(5) . . ?
O12 Th1 O42 127.72(5) . . ?
O2 Th1 O42 68.65(5) . . ?
O1 Th1 O42 67.65(5) . . ?
O91 Th1 O31 110.50(5) . . ?
O81 Th1 O31 68.24(5) . . ?
O22 Th1 O31 65.28(5) . . ?
O12 Th1 O31 122.12(5) . . ?
O2 Th1 O31 125.39(5) . . ?
O1 Th1 O31 171.41(5) . . ?
O42 Th1 O31 104.40(5) . . ?
O91 Th1 O21 111.91(5) . . ?
O81 Th1 O21 70.78(5) . . ?
O22 Th1 O21 49.44(4) . . ?
O12 Th1 O21 64.04(4) . . ?
O2 Th1 O21 121.85(4) . . ?
O1 Th1 O21 122.64(5) . . ?
O42 Th1 O21 168.20(4) . . ?
O31 Th1 O21 65.63(5) . . ?
O91 Th1 O32 66.31(5) . . ?
O81 Th1 O32 111.25(5) . . ?
O22 Th1 O32 64.86(5) . . ?
O12 Th1 O32 164.17(5) . . ?
O2 Th1 O32 129.84(5) . . ?
O1 Th1 O32 126.76(4) . . ?
O42 Th1 O32 67.30(5) . . ?
O31 Th1 O32 48.93(4) . . ?
O21 Th1 O32 100.90(4) . . ?
O91 Th1 O11 68.95(5) . . ?
O81 Th1 O11 114.54(5) . . ?
O22 Th1 O11 63.44(5) . . ?
O12 Th1 O11 49.32(4) . . ?
O2 Th1 O11 102.07(5) . . ?
O1 Th1 O11 65.06(5) . . ?
O42 Th1 O11 121.99(4) . . ?
O31 Th1 O11 123.34(5) . . ?
O21 Th1 O11 63.50(5) . . ?
O32 Th1 O11 121.05(4) . . ?
O91 Th1 O41 107.72(5) . . ?
O81 Th1 O41 68.77(5) . . ?
O22 Th1 O41 126.52(5) . . ?
O12 Th1 O41 127.14(5) . . ?
O2 Th1 O41 68.39(5) . . ?
O1 Th1 O41 103.17(5) . . ?
O42 Th1 O41 48.99(4) . . ?
O31 Th1 O41 68.42(5) . . ?
O21 Th1 O41 126.99(5) . . ?
O32 Th1 O41 65.05(5) . . ?
O11 Th1 O41 168.23(5) . . ?
O3 N1 O2 122.40(18) . . ?
O3 N1 O1 122.07(18) . . ?
O2 N1 O1 115.51(16) . . ?
O3 N1 Th1 168.03(13) . . ?
O2 N1 Th1 58.20(9) . . ?
O1 N1 Th1 58.55(9) . . ?
N1 O1 Th1 96.38(11) . . ?
N1 O2 Th1 96.86(11) . . ?
O13 N11 O12 123.09(18) . . ?
O13 N11 O11 121.69(18) . . ?
O12 N11 O11 115.22(16) . . ?
O13 N11 Th1 175.66(15) . . ?
O12 N11 Th1 56.56(9) . . ?
O11 N11 Th1 58.86(9) . . ?
N11 O11 Th1 96.20(11) . . ?
N11 O12 Th1 99.02(11) . . ?
O23 N21 O22 122.82(17) . . ?
O23 N21 O21 121.77(17) . . ?
O22 N21 O21 115.41(16) . . ?
O23 N21 Th1 174.69(14) . . ?
O22 N21 Th1 56.79(9) . . ?
O21 N21 Th1 58.88(10) . . ?
N21 O21 Th1 96.15(11) . . ?
N21 O22 Th1 98.67(11) . . ?
O33 N31 O31 122.47(17) . . ?
O33 N31 O32 121.87(17) . . ?
O31 N31 O32 115.63(16) . . ?
O33 N31 Th1 166.10(13) . . ?
O31 N31 Th1 58.36(9) . . ?
O32 N31 Th1 58.97(9) . . ?
N31 O31 Th1 97.01(11) . . ?
N31 O32 Th1 96.24(11) . . ?
O43 N41 O41 123.07(17) . . ?
O43 N41 O42 121.38(17) . . ?
O41 N41 O42 115.54(16) . . ?
N41 O41 Th1 96.71(11) . . ?
N41 O42 Th1 98.28(11) . . ?
O53 N51 O52 121.11(18) . . ?
O53 N51 O51 120.94(18) . . ?
O52 N51 O51 117.94(17) . . ?
C61 N61 C62 110.66(16) . 3_665 ?
C61 N61 H61A 109.5 . . ?
C62 N61 H61A 109.5 3_665 . ?
C61 N61 H61B 109.5 . . ?
C62 N61 H61B 109.5 3_665 . ?
H61A N61 H61B 108.1 . . ?
C72 N71 C74 110.45(16) . . ?
C72 N71 H71A 109.6 . . ?
C74 N71 H71A 109.6 . . ?
C72 N71 H71B 109.6 . . ?
C74 N71 H71B 109.6 . . ?
H71A N71 H71B 108.1 . . ?
N61 C61 C62 110.63(17) . . ?
N61 C61 H61C 109.5 . . ?
C62 C61 H61C 109.5 . . ?
N61 C61 H61D 109.5 . . ?
C62 C61 H61D 109.5 . . ?
H61C C61 H61D 108.1 . . ?
N61 C62 C61 110.87(17) 3_665 . ?
N61 C62 H62A 109.5 3_665 . ?
C61 C62 H62A 109.5 . . ?
N61 C62 H62B 109.5 3_665 . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 108.1 . . ?
N71 C72 C74 110.44(17) . 3_566 ?
N71 C72 H72A 109.6 . . ?
C74 C72 H72A 109.6 3_566 . ?
N71 C72 H72B 109.6 . . ?
C74 C72 H72B 109.6 3_566 . ?
H72A C72 H72B 108.1 . . ?
N71 C74 C72 110.79(17) . 3_566 ?
N71 C74 H74A 109.5 . . ?
C72 C74 H74A 109.5 3_566 . ?
N71 C74 H74B 109.5 . . ?
C72 C74 H74B 109.5 3_566 . ?
H74A C74 H74B 108.1 . . ?
Th1 O81 H1 123(2) . . ?
Th1 O81 H2 121(2) . . ?
H1 O81 H2 115(3) . . ?
Th1 O91 H4 117.1(19) . . ?
Th1 O91 H3 118(2) . . ?
H4 O91 H3 111(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 O91 2.4313(15) . ?
Th1 O81 2.4479(16) . ?
Th1 O22 2.5676(15) . ?
Th1 O12 2.5716(15) . ?
Th1 O2 2.5717(15) . ?
Th1 O1 2.5790(15) . ?
Th1 O42 2.5892(14) . ?
Th1 O31 2.6016(15) . ?
Th1 O21 2.6123(16) . ?
Th1 O32 2.6144(15) . ?
Th1 O11 2.6203(15) . ?
Th1 O41 2.6280(15) . ?
N1 O3 1.219(2) . ?
N1 O2 1.276(2) . ?
N1 O1 1.281(2) . ?
N11 O13 1.207(2) . ?
N11 O12 1.274(2) . ?
N11 O11 1.291(2) . ?
N21 O23 1.213(2) . ?
N21 O22 1.275(2) . ?
N21 O21 1.288(2) . ?
N31 O33 1.227(2) . ?
N31 O31 1.273(2) . ?
N31 O32 1.279(2) . ?
N41 O43 1.215(2) . ?
N41 O41 1.273(2) . ?
N41 O42 1.284(2) . ?
N51 O53 1.231(2) . ?
N51 O52 1.264(2) . ?
N51 O51 1.273(2) . ?
N61 C61 1.498(3) . ?
N61 C62 1.499(3) 3_665 ?
N61 H61A 0.9100 . ?
N61 H61B 0.9100 . ?
N71 C72 1.496(3) . ?
N71 C74 1.497(3) . ?
N71 H71A 0.9100 . ?
N71 H71B 0.9100 . ?
C61 C62 1.515(3) . ?
C61 H61C 0.9900 . ?
C61 H61D 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C72 C74 1.514(3) 3_566 ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
O81 H1 0.79(3) . ?
O81 H2 0.74(3) . ?
O91 H4 0.84(3) . ?
O91 H3 0.76(3) . ?
