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_7021224
_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            'C84 H102 Cu12 Mo48 N12 O307 P4'
_chemical_formula_weight         11683.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_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                   33.1757(9)
_cell_length_b                   33.1757(9)
_cell_length_c                   24.6314(13)
_cell_measurement_reflns_used    4558
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.40
_cell_volume                     23477.9(15)
_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      296(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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43444
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    2.799
_exptl_absorpt_correction_T_max  0.0778
_exptl_absorpt_correction_T_min  0.0639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             16710
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.362
_refine_diff_density_min         -3.525
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9138
_refine_ls_number_restraints     972
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+1614.9392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2079
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                8145
_reflns_number_total             9138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32991g.txt
_cod_data_source_block           d:\dalton~1\as
_cod_depositor_comments
'Adding full bibliography for 7021223--7021224.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7021224