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_4108164
_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            'H545 Mo150 N35 O656'
_chemical_formula_weight         25926.71
_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                 72.8254(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   33.4487(5)
_cell_length_b                   53.5509(10)
_cell_length_c                   26.6741(5)
_cell_measurement_reflns_used    294794
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.32
_cell_volume                     45648.4(14)
_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 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       77
_diffrn_reflns_limit_k_min       -77
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            374815
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  0.7922
_exptl_absorpt_correction_T_min  0.7135
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_description       plate
_exptl_crystal_F_000             24676
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.889
_refine_diff_density_min         -2.480
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1793
_refine_ls_number_reflns         73161
_refine_ls_number_restraints     2120
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1695P)^2^+259.5663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2354
_refine_ls_wR_factor_ref         0.2826
_reflns_number_gt                44476
_reflns_number_total             73161
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja800784a-file019.cif
_cod_data_source_block           crystal_7
_cod_original_cell_volume        45648(1)
_cod_database_code               4108164