Synthesis, structure, electrochemistry and magnetism of cobalt-, nickel- and zinc-containing [M<sub>4</sub>(OH)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>(α-SiW<sub>10</sub>O<sub>36.5</sub>)<sub>2</sub>]<sup>13-</sup> (M = Co<sup>2+</sup>, Ni<sup>2+</sup>, and Zn<sup>2+</sup>).
Haider, Ali; Bassil, Bassem S.; Lin, Zhengguo; Ma, Xiang; Haferl, Peter J.; Bindra, Jasleen K.; Kinyon, Jared; Zhang, Guangjin; Keita, Bineta; Dalal, Naresh S.; Kortz, Ulrich; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3923–3930; doi:10.1039/d0dt03392h

data_7706505
_publ_section_title
;
 Synthesis, structure, electrochemistry and magnetism of cobalt-, nickel-
 and zinc-containing
 [M<sub>4</sub>(OH)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>(\a-SiW<sub>10</sub>O<sub>36.5</sub>)<sub>2</sub>]<sup>13-</sup>
 (M = Co<sup>2+</sup>, Ni<sup>2+</sup>, and Zn<sup>2+</sup>).
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3923
_journal_page_last               3930
_journal_paper_doi               10.1039/d0dt03392h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'Co4 Cs10 H28 Na3 O99 Si2 W20'
_chemical_formula_weight         6979.19
_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'
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2021-01-20 deposited with the CCDC.	2021-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.616(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1052(7)
_cell_length_b                   15.7954(8)
_cell_length_c                   23.8328(14)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      3.23
_cell_volume                     4849.0(5)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            100865
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         3.416
_exptl_absorpt_coefficient_mu    28.131
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    4.780
_exptl_crystal_description       block
_exptl_crystal_F_000             6038
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.0962
_exptl_transmission_factor_min   0.0362
_refine_diff_density_max         3.503
_refine_diff_density_min         -3.588
_refine_diff_density_rms         0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         10686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+110.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8491
_reflns_number_total             10686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03392h2.cif
_cod_data_source_block           lzg
_cod_depositor_comments
'Adding full bibliography for 7706505--7706507.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'Co4 H28 Cs10 Na3 O99 Si2 W20'
_cod_database_code               7706505
_shelx_estimated_absorpt_t_min   0.0362
_shelx_estimated_absorpt_t_max   0.0962
_shelxl_version_number           2014/6
_shelx_res_checksum              37241