Two-Dimensional Extended (4,4)-Topological Network Constructed from Tetra-NiII-Substituted Sandwich-Type Keggin Polyoxometalate Building Blocks and NiII-Organic Cation Bridges
Zhao, Jun-Wei; Li, Bing; Zheng, Shou-Tian; Yang, Guo-Yu; Crystal Growth & Design 7 (2007) 2658–; doi:10.1021/cg700783b

data_4504467
_publ_section_title
;
 Two-Dimensional Extended (4,4)-Topological Network Constructed from
 Tetra-NiII-Substituted Sandwich-Type Keggin Polyoxometalate Building
 Blocks and NiII-Organic Cation Bridges
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2658
_journal_paper_doi               10.1021/cg700783b
_journal_volume                  7
_journal_year                    2007
_chemical_formula_sum            'C30 H120 Ge2 N20 Ni8 O76 W18'
_chemical_formula_weight         5901.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.159(6)
_cell_angle_beta                 71.100(8)
_cell_angle_gamma                87.683(9)
_cell_formula_units_Z            1
_cell_length_a                   13.338(3)
_cell_length_b                   13.978(3)
_cell_length_c                   17.049(3)
_cell_measurement_reflns_used    6824
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      2.0814
_cell_volume                     2779.7(10)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Saturn70 (4x4 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21810
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    20.484
_exptl_absorpt_correction_T_max  0.6848
_exptl_absorpt_correction_T_min  0.1760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            olivine
_exptl_crystal_density_diffrn    3.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.747
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         12466
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+21.5352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                10063
_reflns_number_total             12466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg700783b-file002.cif
_cod_data_source_block           q
_cod_original_cell_volume        2779.8(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4504467