Novel Acetate Polyoxomolybdate "Host" Accommodating a Zigzag-Chainlike "Guest" of Five Edge-Shared Sodium Cations: Na21{[Na5(H2O)14]@[Mo46O134(OH)10(μ-CH3COO)4]}.CH3COONa.~95H2O
Wenbin Yang; Canzhong Lu; Xiang Lin; Honghui Zhuang; Inorganic Chemistry 41 (2002) 452–454; doi:10.1021/ic010267e

data_4317472
_publ_contact_author_address
;
     Fujian Institute of Research  
        on the Structure of Matter,
        Chinese Academy of Sciences,
        Fuzhou, Fujian 350002, 
    P.R.China
;
_publ_contact_author_email       czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax         0086-0591-3714946
_publ_contact_author_name        'Dr. Canzhong Lu'
_publ_contact_author_phone       0591-3792865
_publ_section_title
;
 Novel Acetate Polyoxomolybdate "Host" Accommodating a Zigzag-Chainlike
 "Guest" of Five Edge-Shared Sodium Cations:
 Na21{[Na5(H2O)14]@[Mo46O134(OH)10(\m-CH3COO)4]}.CH3COONa.~95H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              452
_journal_page_last               454
_journal_paper_doi               10.1021/ic010267e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C10 H243 Mo46 N0 Na27 O263'
_chemical_formula_weight         9607.01
_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                87.57
_cell_angle_beta                 67.9810(10)
_cell_angle_gamma                80.6970(10)
_cell_formula_units_Z            1
_cell_length_a                   16.4065(3)
_cell_length_b                   17.4236(2)
_cell_length_c                   20.8247(3)
_cell_measurement_temperature    293(2)
_cell_volume                     5445.08(15)
_computing_cell_refinement       'Simens CCD SAINT'
_computing_data_collection       'Simens SMART CCD'
_computing_data_reduction        'Simens CCD SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Siemens CCD SMART'
_diffrn_measurement_method       omega-scan
_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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.1324
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28434
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    2.754
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.458575
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'black red'
_exptl_crystal_density_diffrn    2.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4636
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.084
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1287
_refine_ls_number_reflns         19014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2328
_reflns_number_gt                11520
_reflns_number_total             19014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010267e.cif
_cod_data_source_block           IC010267E
_cod_original_cell_volume        5445.08(14)
_cod_database_code               4317472