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_7024627
_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            'C30 H37 N6 Ni O46 P W12'
_chemical_formula_weight         3513.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 115.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.241(5)
_cell_length_b                   11.250(2)
_cell_length_c                   28.261(6)
_cell_measurement_reflns_used    26766
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.13
_cell_volume                     6982(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33470
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    20.063
_exptl_absorpt_correction_T_max  0.0626
_exptl_absorpt_correction_T_min  0.0372
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6232
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_refine_diff_density_max         3.164
_refine_diff_density_min         -4.297
_refine_diff_density_rms         0.369
_refine_ls_extinction_coef       0.000066(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         8008
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0547P)^2^+498.4503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                6352
_reflns_number_total             8008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b919503c.txt
_cod_data_source_block           k2
_cod_original_cell_volume        6981(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7024627