Isolation of stable lacunary Dawson-type structure in a polyoxomolybdate cluster
Akihiko Hashikawa; Makkiko Fujimoto; Yoshihito Hayashi; Hitoshi Miyasaka; Chem.Commun. 47 (2011) 12361–; doi:10.1039/c1cc15439g

data_7107059
_publ_section_title
;
 Isolation of stable lacunary Dawson-type structure in a polyoxomolybdate
 cluster
;
_publ_section_title_footnote
;
;
_journal_name_full               Chem.Commun.
_journal_page_first              12361
_journal_paper_doi               10.1039/c1cc15439g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C50 H110 N2 Mo14 O52, 0.5(C4 H10 O)'
_chemical_formula_sum            'C52 H115 Mo14 N2 O52.5'
_chemical_formula_weight         2951.62
_chemical_name_common            'Reduced Tetradecamolybdate'
_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                 106.695(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.566(4)
_cell_length_b                   14.6753(19)
_cell_length_c                   25.184(4)
_cell_measurement_reflns_used    17766
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      7.0
_cell_volume                     9758(2)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    Platon
_computing_publication_material  Platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELX97
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9732
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         6.99
_exptl_absorpt_coefficient_mu    1.821
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5796
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9732
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+101.6150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                8579
_reflns_number_total             9732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15439g.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               7107059