Hydrothermal syntheses and characterizations of two novel frameworks constructed from polyoxometalates, metals and organic units.
Wang, Yan; Ye, Ling; Wang, Tie-Gang; Cui, Xiao-Bing; Shi, Shu-Yun; Wang, Guo-Wu; Xu, Ji-Qing; Dalton transactions (Cambridge, England : 2003) 39 (2010) 1916–1919; doi:10.1039/b919503c

data_7024626
_publ_section_title
;
 Hydrothermal syntheses and characterizations of two novel frameworks
 constructed from polyoxometalates, metals and organic units.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1916
_journal_page_last               1919
_journal_paper_doi               10.1039/b919503c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C50 H55 B N10 Ni2 O47 W12'
_chemical_formula_weight         3882.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 102.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.292(3)
_cell_length_b                   15.146(3)
_cell_length_c                   19.946(4)
_cell_measurement_reflns_used    27801
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.09
_cell_volume                     3924.4(15)
_computing_molecular_graphics    'diamond 3.1'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  RAXIS-RAPID
_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  0.1175
_diffrn_reflns_av_sigmaI/netI    0.1473
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36380
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    18.076
_exptl_absorpt_correction_T_max  0.0808
_exptl_absorpt_correction_T_min  0.0400
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    3.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3500
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.470
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.366
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         16938
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+24.7551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                11938
_reflns_number_total             16938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b919503c.txt
_cod_data_source_block           k1
_cod_original_cell_volume        3924.4(14)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7024626