#------------------------------------------------------------------------------
#$Date: 2024-04-05 02:05:43 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/80/7248085.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_7248085
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(C7 H10 N)'
_chemical_formula_sum            'C14 H20 N8 O18 Th'
_chemical_formula_weight         820.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 101.802(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8462(6)
_cell_length_b                   13.2604(9)
_cell_length_c                   11.0517(7)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.43
_cell_volume                     1269.00(15)
_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 0.997
_diffrn_measurement_device_type  '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  0.0432
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19296
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.374
_diffrn_reflns_theta_min         2.430
_exptl_absorpt_coefficient_mu    5.976
_exptl_absorpt_correction_T_max  0.64724
_exptl_absorpt_correction_T_min  0.38296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0095P)²+1.1509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2426
_reflns_number_total             3170
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01319g2.cif
_cod_data_source_block           B22185_b
_cod_depositor_comments
'Adding full bibliography for 7248080--7248089.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7248085
_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   0.294
_shelx_estimated_absorpt_t_max   0.542
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.500000 0.500000 0.00873(4) Uani 1 2 d S . P . .
O11 O 0.5064(2) 0.67421(14) 0.60523(17) 0.0144(4) Uani 1 1 d . . . . .
O12 O 0.7291(2) 0.60900(13) 0.60401(17) 0.0128(4) Uani 1 1 d . . . . .
O13 O 0.7153(2) 0.75743(15) 0.6858(2) 0.0251(5) Uani 1 1 d . . . . .
O21 O 0.4546(2) 0.35433(14) 0.63655(16) 0.0143(4) Uani 1 1 d . . . . .
O22 O 0.5531(2) 0.48645(13) 0.73762(17) 0.0152(4) Uani 1 1 d . . . . .
O23 O 0.4766(2) 0.35957(15) 0.83635(17) 0.0188(4) Uani 1 1 d . . . . .
O31 O 0.2631(2) 0.53040(14) 0.59384(18) 0.0154(4) Uani 1 1 d . . . . .
O32 O 0.2495(2) 0.59398(14) 0.41149(17) 0.0148(4) Uani 1 1 d . . . . .
O33 O 0.0548(2) 0.60969(16) 0.50322(19) 0.0244(5) Uani 1 1 d . . . . .
N11 N 0.6519(3) 0.68372(17) 0.6341(2) 0.0140(5) Uani 1 1 d . . . . .
N21 N 0.4946(3) 0.39825(17) 0.7409(2) 0.0132(5) Uani 1 1 d . . . . .
N31 N 0.1834(3) 0.57913(17) 0.5035(2) 0.0138(5) Uani 1 1 d . . . . .
N41 N 0.9975(3) 0.5366(2) 0.7766(2) 0.0199(6) Uani 1 1 d . . . . .
H41A H 0.915(4) 0.538(3) 0.733(3) 0.030 Uiso 1 1 d . U . . .
C41 C 1.0339(3) 0.4527(2) 0.8459(3) 0.0187(6) Uani 1 1 d . . . . .
H41 H 0.966003 0.396428 0.835425 0.022 Uiso 1 1 calc R U . . .
C42 C 1.1699(3) 0.4497(2) 0.9314(3) 0.0156(6) Uani 1 1 d . . . . .
C43 C 1.2673(3) 0.5342(2) 0.9390(3) 0.0158(6) Uani 1 1 d . . . . .
H43 H 1.363042 0.533332 0.996629 0.019 Uiso 1 1 calc R U . . .
C44 C 1.2287(3) 0.6188(2) 0.8656(3) 0.0153(6) Uani 1 1 d . . . . .
C45 C 1.0870(3) 0.6183(2) 0.7845(3) 0.0192(6) Uani 1 1 d . . . . .
H45 H 1.053735 0.675758 0.734847 0.023 Uiso 1 1 calc R U . . .
C46 C 1.2155(4) 0.3589(2) 1.0124(3) 0.0220(7) Uani 1 1 d . . . . .
H46A H 1.122476 0.325549 1.027900 0.033 Uiso 1 1 calc R U . . .
H46B H 1.280127 0.380289 1.091080 0.033 Uiso 1 1 calc R U . . .
H46C H 1.273532 0.311861 0.970834 0.033 Uiso 1 1 calc R U . . .
C47 C 1.3363(3) 0.7063(2) 0.8705(3) 0.0202(6) Uani 1 1 d . . . . .
H47A H 1.425514 0.686341 0.836117 0.030 Uiso 1 1 calc R U . . .
H47B H 1.371540 0.727681 0.956584 0.030 Uiso 1 1 calc R U . . .
H47C H 1.282441 0.762328 0.822137 0.030 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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 0.00 0.0650
0.00 1.00 0.00 0.1090
1.00 3.00 -2.00 0.1110
-1.00 3.00 1.00 0.1100
0.00 -2.00 1.00 0.0850
0.00 3.00 -2.00 0.1120
1.00 -3.00 1.00 0.0500
1.00 -3.00 2.00 0.0590
-2.00 3.00 1.00 0.1120
0.00 1.00 -2.00 0.1010
2.00 -2.00 3.00 0.0500
-2.00 2.00 -3.00 0.0730
-1.00 1.00 -3.00 0.0700
-3.00 2.00 -3.00 0.0680
-2.00 1.00 -1.00 0.0670
2.00 0.00 3.00 0.0660
-2.00 0.00 -3.00 0.0430
2.00 0.00 1.00 0.0780
-3.00 1.00 1.00 0.0960
-1.00 -1.00 -3.00 0.0500
-3.00 -1.00 -3.00 0.0330
0.00 1.00 2.00 0.1110
0.00 -2.00 -3.00 0.0590
1.00 1.00 1.00 0.0720
3.00 -3.00 2.00 0.0410
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 180.0 3_666 . ?
O21 Th1 O31 111.41(6) 3_666 . ?
O21 Th1 O31 68.59(6) . . ?
O21 Th1 O31 68.59(6) 3_666 3_666 ?
O21 Th1 O31 111.41(6) . 3_666 ?
O31 Th1 O31 180.0 . 3_666 ?
O21 Th1 O32 111.65(6) 3_666 3_666 ?
O21 Th1 O32 68.35(6) . 3_666 ?
O31 Th1 O32 129.86(6) . 3_666 ?
O31 Th1 O32 50.14(6) 3_666 3_666 ?
O21 Th1 O32 68.35(6) 3_666 . ?
O21 Th1 O32 111.65(6) . . ?
O31 Th1 O32 50.14(6) . . ?
O31 Th1 O32 129.86(6) 3_666 . ?
O32 Th1 O32 180.0 3_666 . ?
O21 Th1 O12 111.73(6) 3_666 3_666 ?
O21 Th1 O12 68.27(6) . 3_666 ?
O31 Th1 O12 68.39(6) . 3_666 ?
O31 Th1 O12 111.61(6) 3_666 3_666 ?
O32 Th1 O12 116.16(6) 3_666 3_666 ?
O32 Th1 O12 63.84(6) . 3_666 ?
O21 Th1 O12 68.27(6) 3_666 . ?
O21 Th1 O12 111.73(6) . . ?
O31 Th1 O12 111.61(6) . . ?
O31 Th1 O12 68.39(6) 3_666 . ?
O32 Th1 O12 63.84(6) 3_666 . ?
O32 Th1 O12 116.16(6) . . ?
O12 Th1 O12 180.0 3_666 . ?
O21 Th1 O22 129.94(6) 3_666 . ?
O21 Th1 O22 50.06(6) . . ?
O31 Th1 O22 65.84(6) . . ?
O31 Th1 O22 114.16(6) 3_666 . ?
O32 Th1 O22 67.25(6) 3_666 . ?
O32 Th1 O22 112.75(6) . . ?
O12 Th1 O22 112.35(6) 3_666 . ?
O12 Th1 O22 67.65(6) . . ?
O21 Th1 O22 50.06(6) 3_666 3_666 ?
O21 Th1 O22 129.94(6) . 3_666 ?
O31 Th1 O22 114.16(6) . 3_666 ?
O31 Th1 O22 65.85(6) 3_666 3_666 ?
O32 Th1 O22 112.76(6) 3_666 3_666 ?
O32 Th1 O22 67.24(6) . 3_666 ?
O12 Th1 O22 67.65(6) 3_666 3_666 ?
O12 Th1 O22 112.35(6) . 3_666 ?
O22 Th1 O22 179.999(15) . 3_666 ?
O21 Th1 O11 113.92(6) 3_666 3_666 ?
O21 Th1 O11 66.08(6) . 3_666 ?
O31 Th1 O11 112.34(6) . 3_666 ?
O31 Th1 O11 67.66(6) 3_666 3_666 ?
O32 Th1 O11 70.94(6) 3_666 3_666 ?
O32 Th1 O11 109.06(6) . 3_666 ?
O12 Th1 O11 49.51(6) 3_666 3_666 ?
O12 Th1 O11 130.49(6) . 3_666 ?
O22 Th1 O11 112.28(6) . 3_666 ?
O22 Th1 O11 67.72(6) 3_666 3_666 ?
O21 Th1 O11 66.08(6) 3_666 . ?
O21 Th1 O11 113.92(6) . . ?
O31 Th1 O11 67.66(6) . . ?
O31 Th1 O11 112.34(6) 3_666 . ?
O32 Th1 O11 109.06(6) 3_666 . ?
O32 Th1 O11 70.94(6) . . ?
O12 Th1 O11 130.49(6) 3_666 . ?
O12 Th1 O11 49.51(6) . . ?
O22 Th1 O11 67.72(6) . . ?
O22 Th1 O11 112.28(6) 3_666 . ?
O11 Th1 O11 180.00(8) 3_666 . ?
N11 O11 Th1 97.46(14) . . ?
N11 O12 Th1 97.91(14) . . ?
N21 O21 Th1 98.16(14) . . ?
N21 O22 Th1 95.84(14) . . ?
N31 O31 Th1 97.47(14) . . ?
N31 O32 Th1 96.95(14) . . ?
O13 N11 O11 123.2(2) . . ?
O13 N11 O12 121.7(2) . . ?
O11 N11 O12 115.1(2) . . ?
O13 N11 Th1 178.33(19) . . ?
O11 N11 Th1 57.95(12) . . ?
O12 N11 Th1 57.16(12) . . ?
O23 N21 O21 122.1(2) . . ?
O23 N21 O22 122.4(2) . . ?
O21 N21 O22 115.5(2) . . ?
O23 N21 Th1 173.33(18) . . ?
O21 N21 Th1 56.90(12) . . ?
O22 N21 Th1 58.94(12) . . ?
O33 N31 O31 122.8(2) . . ?
O33 N31 O32 121.7(2) . . ?
O31 N31 O32 115.4(2) . . ?
O33 N31 Th1 178.76(19) . . ?
O31 N31 Th1 57.61(12) . . ?
O32 N31 Th1 57.82(12) . . ?
C45 N41 C41 124.1(3) . . ?
C45 N41 H41A 119(3) . . ?
C41 N41 H41A 116(3) . . ?
N41 C41 C42 119.2(3) . . ?
N41 C41 H41 120.4 . . ?
C42 C41 H41 120.4 . . ?
C41 C42 C43 117.3(3) . . ?
C41 C42 C46 121.6(3) . . ?
C43 C42 C46 121.1(3) . . ?
C44 C43 C42 122.4(3) . . ?
C44 C43 H43 118.8 . . ?
C42 C43 H43 118.8 . . ?
C45 C44 C43 117.2(3) . . ?
C45 C44 C47 120.9(3) . . ?
C43 C44 C47 121.9(3) . . ?
N41 C45 C44 119.6(3) . . ?
N41 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
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 2.5334(18) 3_666 ?
Th1 O21 2.5335(18) . ?
Th1 O31 2.5535(19) . ?
Th1 O31 2.5535(19) 3_666 ?
Th1 O32 2.5565(19) 3_666 ?
Th1 O32 2.5565(19) . ?
Th1 O12 2.5619(18) 3_666 ?
Th1 O12 2.5620(18) . ?
Th1 O22 2.5778(19) . ?
Th1 O22 2.5778(19) 3_666 ?
Th1 O11 2.5817(19) 3_666 ?
Th1 O11 2.5817(19) . ?
O11 N11 1.268(3) . ?
O12 N11 1.285(3) . ?
O13 N11 1.210(3) . ?
O21 N21 1.276(3) . ?
O22 N21 1.282(3) . ?
O23 N21 1.213(3) . ?
O31 N31 1.274(3) . ?
O32 N31 1.287(3) . ?
O33 N31 1.207(3) . ?
N41 C45 1.335(4) . ?
N41 C41 1.352(4) . ?
N41 H41A 0.79(4) . ?
C41 C42 1.370(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.405(4) . ?
C42 C46 1.505(4) . ?
C43 C44 1.386(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.383(4) . ?
C44 C47 1.495(4) . ?
C45 H45 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N41 H41A O12 0.79(4) 2.16(4) 2.889(3) 153(4) . yes
N41 H41A O32 0.79(4) 2.60(4) 3.199(3) 134(3) 3_666 yes
