The pH Dependent Nuclearity Variation of {Mo154-x}-type Polyoxomolybdates and Tectonic Effect on Their Aggregations
Sayaka Shishido; Tomoji Ozeki; Journal of the American Chemical Society 130 (2008) 10588–10595; doi:10.1021/ja800784a

data_4108160
_publ_contact_author_address
;Department of Chemistry and Materials Science
Tokyo Institute of Technology
2-12-1-H-63 O-okayama, Meguro-ku, Tokyo 152-8551, Japan
;
_publ_contact_author_email       tozeki@cms.titech.ac.jp
_publ_contact_author_fax         81(3)57342442
_publ_contact_author_name        'Tomoji Ozeki'
_publ_contact_author_phone       81(3)57342442
_publ_section_title
;
 The pH Dependent Nuclearity Variation of {Mo154-x}-type Polyoxomolybdates
 and Tectonic Effect on Their Aggregations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10588
_journal_page_last               10595
_journal_paper_doi               10.1021/ja800784a
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'H396 Mo138 N28 O556'
_chemical_formula_weight         22927.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.858(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   27.7619(5)
_cell_length_b                   42.6994(10)
_cell_length_c                   30.2459(7)
_cell_measurement_reflns_used    136738
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      1.70
_cell_volume                     35666.8(13)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection
'Crystal Clear (Molecular Structure Corporation, 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond 3.1d (Brandenburg, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         'KEK PF-AR NW2 beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6890
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_sigmaI/netI    0.1153
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            185876
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9145
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_description       plate
_exptl_crystal_F_000             21672
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.443
_refine_diff_density_min         -3.449
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1534
_refine_ls_number_reflns         44232
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.2081
_reflns_number_gt                22308
_reflns_number_total             44232
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja800784a-file015.cif
_cod_data_source_block           crystal_3
_cod_original_cell_volume        35667(1)
_cod_database_code               4108160