Structural chemistry of penta- and hexanitrato thorium(iv) complexes isolated using N–H donors
Shore, Madeline C.; Nicholas, Aaron D.; Vasiliu, Monica; Edwards, Kyle C.; de Melo, Gabriel F.; Bertke, Jeffery A.; Dixon, David A.; Knope, Karah E.; CrystEngComm 26 (2024) 1380–1398; doi:10.1039/D3CE01319G

data_7248082
_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_sum            'C15 H18 N10 O21 Th'
_chemical_formula_weight         906.43
_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
_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                 108.057(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2065(10)
_cell_length_b                   12.3878(10)
_cell_length_c                   19.2532(16)
_cell_measurement_reflns_used    9643
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.23
_cell_volume                     2767.9(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61863
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.425
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    5.500
_exptl_absorpt_correction_T_max  0.19403
_exptl_absorpt_correction_T_min  0.11514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_min          0.336
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2568
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0157
_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/[\s^2^(Fo^2^)+(0.0064P)^2^+8.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0353
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2427
_reflns_number_total             2568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01319g2.cif
_cod_data_source_block           mono111722_a
_cod_depositor_comments
'Adding full bibliography for 7248080--7248089.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7248082
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.217
_shelx_estimated_absorpt_t_max   0.259
_shelx_res_checksum              99779