Synthesis and Characterization of 2D and 3D Structures from Organic Derivatives of Polyoxometalate Clusters: Role of Organic Moiety, Counterion, and Solvent
Bret J. S. Johnson; Rick C. Schroden; Changcheng Zhu; Andreas Stein; Inorganic Chemistry 40 (2001) 5972–5978; doi:10.1021/ic010045g

data_4320451
_publ_section_title
;
 Synthesis and Characterization of 2D and 3D Structures from Organic
 Derivatives of Polyoxometalate Clusters: Role of Organic Moiety,
 Counterion, and Solvent
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5972
_journal_page_last               5978
_journal_paper_doi               10.1021/ic010045g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C24 H20 As4 Mo12 O50'
_chemical_formula_sum            'C24 H20 As4 Mo12 O50'
_chemical_formula_weight         2559.36
_chemical_name_common            00350a
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.450(3)
_cell_length_b                   28.450(3)
_cell_length_c                   11.645(2)
_cell_measurement_reflns_used    4493
_cell_measurement_temperature    293(2)
_cell_volume                     9425(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, 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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            29058
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    3.005
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.663692
_exptl_absorpt_correction_type   multiscans
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.818
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                2276
_reflns_number_total             2827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010045g_3.cif
_cod_data_source_block           00350a
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               4320451