An unprecedented polyoxometalate-based hybrid solid constructed from a neutral metal-organic macrocycle and Dawson polyoxotungstate anions.
Xu, Yanqing; Gao, Yuanzhe; Wei, Wei; Wang, Zhiqin; Li, Shan; Hu, Changwen; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5228–5231; doi:10.1039/c3dt32991g

data_7021223
_publ_section_title
;
 An unprecedented polyoxometalate-based hybrid solid constructed from a
 neutral metal-organic macrocycle and Dawson polyoxotungstate anions.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5228
_journal_page_last               5231
_journal_paper_doi               10.1039/c3dt32991g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C42 H186 Cu6 K11 N6 Na O208 P4 W36'
_chemical_formula_weight         11680.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.7675(10)
_cell_length_b                   20.7675(10)
_cell_length_c                   43.170(4)
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      2.45
_cell_volume                     16124.3(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            28783
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    20.121
_exptl_absorpt_correction_T_max  0.0776
_exptl_absorpt_correction_T_min  0.0649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             15786
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         4.848
_refine_diff_density_min         -4.738
_refine_diff_density_rms         0.471
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0937P)^2^+4662.9878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.2347
_reflns_number_gt                2499
_reflns_number_total             3441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32991g.txt
_cod_data_source_block           d:\collab~1\xuyan-~1\wang-2a\g
_cod_depositor_comments
'Adding full bibliography for 7021223--7021224.cif.'
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7021223