Mixed-valence compounds based on heterometallic-oxo-clusters containing Sb(III,V): crystal structures and proton conduction.
Wen, Wei-Yang; Ma, Wen; Hu, Bing; Xiao, Hui-Ping; Pan, Tian-Yu; Liu, Jia-Ting; Lin, Hao-Wei; Li, Xin-Xiong; Huang, Xiao-Ying; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1156–1162; doi:10.1039/d3dt03904h

data_7714637
_publ_section_title
;
 Mixed-valence compounds based on heterometallic-oxo-clusters containing
 Sb(III,V): crystal structures and proton conduction.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1156
_journal_page_last               1162
_journal_paper_doi               10.1039/d3dt03904h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C48 H66.28 Co11.4 O111.14 Sb14, 10.86(H2 O), Co H12 O6'
_chemical_formula_sum            'C48 H113.2 Co12.4 O128 Sb14'
_chemical_formula_weight         5173.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-10-13
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.3540(10)
_cell_angle_beta                 71.8830(10)
_cell_angle_gamma                64.478(2)
_cell_formula_units_Z            1
_cell_length_a                   13.7182(2)
_cell_length_b                   14.6187(2)
_cell_length_c                   18.7051(2)
_cell_measurement_reflns_used    51741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2210
_cell_measurement_theta_min      2.0910
_cell_volume                     3194.49(9)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19313
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.146
_diffrn_reflns_theta_min         1.794
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.689
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2474
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.754
_refine_diff_density_min         -3.865
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         19313
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+41.0889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16041
_reflns_number_total             19313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03904h2.cif
_cod_data_source_block           X_TW
_cod_depositor_comments
'Adding full bibliography for 7714637--7714638.cif.'
_cod_original_cell_volume        3194.50(9)
_cod_original_formula_sum        'C48 H113.20 Co12.40 O128 Sb14'
_cod_database_code               7714637
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.339
_shelx_res_checksum              91181
_shelx_shelxl_version_number     2018/3