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_1561348
_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            'C80 H198 Co8 N16 Na22 O275 Si4 W48'
_chemical_formula_weight         15698.92
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.1600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   15.4691(6)
_cell_length_b                   29.3237(13)
_cell_length_c                   16.5389(7)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5634
_cell_measurement_theta_min      3.1361
_cell_volume                     7333.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.2458
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            97041
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    19.348
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    3.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7056
_refine_diff_density_max         4.314
_refine_diff_density_min         -2.986
_refine_diff_density_rms         0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         12986
_refine_ls_number_restraints     749
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+48.8922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                9597
_reflns_number_total             12986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2016-243-146.cif
_cod_data_source_block           ww
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1561348