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_7248084
_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            'C20 H24 N12 O24 Th'
_chemical_formula_weight         1048.55
_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
_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                 95.951(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1866(7)
_cell_length_b                   13.3824(9)
_cell_length_c                   13.0890(9)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.08
_cell_volume                     1774.7(2)
_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-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 APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            57273
_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         25.369
_diffrn_reflns_theta_min         2.521
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.312
_exptl_absorpt_correction_T_max  0.14335
_exptl_absorpt_correction_T_min  0.02160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.704
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+1.0068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2931
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01319g2.cif
_cod_data_source_block           mono_a
_cod_depositor_comments
'Adding full bibliography for 7248080--7248089.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7248084
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.365
_shelx_estimated_absorpt_t_max   0.596
_shelx_res_checksum              23964