Two supramolecular complexes based on polyoxometalates and Co-EDTA units via covalent connection or non-covalent interaction
Teng, Chunlin; Xiao, Hanxi; Cai, Qing; Tang, Jianting; Cai, Tiejun; Deng, Qian; Journal of Solid State Chemistry 243 (2016) 146–153; doi:10.1016/j.jssc.2016.08.021

data_1561347
_publ_section_title
;
 Two supramolecular complexes based on polyoxometalates and Co-EDTA units
 via covalent connection or non-covalent interaction
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              146
_journal_page_last               153
_journal_paper_doi               10.1016/j.jssc.2016.08.021
_journal_volume                  243
_journal_year                    2016
_chemical_formula_sum            'C40 H106 Co4 N8 O133 Si2 W24'
_chemical_formula_weight         7531.63
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                81.734(3)
_cell_angle_beta                 75.230(4)
_cell_angle_gamma                85.989(3)
_cell_formula_units_Z            1
_cell_length_a                   13.0101(5)
_cell_length_b                   14.5594(6)
_cell_length_c                   19.4444(8)
_cell_measurement_reflns_used    9323
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7543
_cell_measurement_theta_min      2.2313
_cell_volume                     3522.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  bruker-CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23927
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    20.102
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3378
_refine_diff_density_max         2.389
_refine_diff_density_min         -3.247
_refine_diff_density_rms         0.403
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     990
_refine_ls_number_reflns         12469
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+87.6540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1985
_reflns_number_gt                9323
_reflns_number_total             12469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2016-243-146.cif
_cod_data_source_block           p
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1561347