Synthesis, structure, and properties of the multinuclear cobalt core POM Na14[Co3O(H2O)(A-α-PW9O34)2]·~29.5H2O
Rehan, Kanwar; Asma, Maliha; McMillen, Colin D.; Sokolov, Andrei; Sohail, Manzar; Sher, Muhammad; Shafique, Munib Ahmed; Bukhari, Naheed; Tirmizi, Syed Ahmad; Inorganica Chimica Acta 509 (2020) 119690–; doi:10.1016/j.ica.2020.119690

data_1564466
_publ_section_title
;
 Synthesis, structure, and properties of the multinuclear cobalt core POM
 Na14[Co3O(H2O)(A-\a-PW9O34)2]&#x00B7;~29.5H2O
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119690
_journal_paper_doi               10.1016/j.ica.2020.119690
_journal_volume                  509
_journal_year                    2020
_chemical_formula_sum            'Co3 H61 Na14 O99.5 P2 W18'
_chemical_formula_weight         5523.37
_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   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                78.448(2)
_cell_angle_beta                 80.551(2)
_cell_angle_gamma                78.448(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2204(8)
_cell_length_b                   16.7035(11)
_cell_length_c                   23.3466(16)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.54
_cell_volume                     4536.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            205802
_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         26.499
_diffrn_reflns_theta_min         2.368
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    23.480
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    4.044
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             4908
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.051
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_refine_diff_density_max         4.660
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1308
_refine_ls_number_reflns         18814
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0306P)^2^+76.1375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16520
_reflns_number_total             18814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-509-119690.cif
_cod_data_source_block           d8-2797_a
_cod_original_formula_sum        'Co3 H61 Na14 O99.50 P2 W18'
_cod_database_code               1564466
_shelx_estimated_absorpt_t_min   0.093
_shelx_estimated_absorpt_t_max   0.381