Crystal structure of [Th3(Cp*)3(O)(OH)3]2Cl2(N3)6: a discrete molecular capsule built from multinuclear organothorium cluster cations
Kelley, Steven P.; Rungthanaphatsophon, Pokpong; Walensky, Justin R.; Acta Crystallographica Section E Crystallographic Communications 77 (2021) –; doi:10.1107/S2056989021008914

data_2022437
_publ_section_title
;
 Crystal structure of [Th3(Cp*)3(O)(OH)3]2Cl2(N3)6: a discrete molecular
 capsule built from multinuclear organothorium cluster cations
;
_journal_coeditor_code           ZL5025
_journal_issue                   10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989021008914
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Th6 (C10 H15)6 Cl2 (N3)6 (O H)6 O2], 0.56C4 H10 O, 1.44C4 H8 O'
_chemical_formula_moiety
'C60 H96 Cl2 N18 O8 Th6, 0.56(C4 H10 O), 1.44(C4 H8 O)'
_chemical_formula_sum            'C68 H113.12 Cl2 N18 O10 Th6'
_chemical_formula_weight         2804.00
_chemical_name_systematic
;Hexa-\m~2~-azido-di-\m~3~-chlorido-hexa-\m~2~-hydroxido-di-\m~3~-oxido-hexakis(pentamethylcyclopentadienyl)hexathorium--diethyl
ether--tetrahydrofuran (1/0.56/1.44)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 121.867(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6783(14)
_cell_length_b                   17.2647(14)
_cell_length_c                   16.383(2)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.36
_cell_volume                     4246.6(7)
_computing_cell_refinement
;
APEX3 and SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
APEX3 and SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker VENTURE CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64622
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.532
_diffrn_reflns_theta_min         2.359
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_exptl_absorpt_coefficient_mu    10.591
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>AXScale</i>; Bruker, 2017)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2598
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.139
_refine_diff_density_min         -0.905
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5050
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+34.2882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                4393
_reflns_number_total             5050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5025sup1.cif
_cod_data_source_block           I
_cod_database_code               2022437
_shelx_estimated_absorpt_t_min   0.266
_shelx_estimated_absorpt_t_max   0.677
_shelx_hkl_checksum              97664
_shelx_res_checksum              90625
_cod_database_fobs_code 2022437