A New Class of Functionalized Polyoxometalates: Synthetic, Structural, Spectroscopic, and Electrochemical Studies of Organoimido Derivatives of [Mo6O19]2-
Joseph B. Strong; Glenn P. A. Yap; Robert Ostrander; Louise M. Liable-Sands; Arnold L. Rheingold; René Thouvenot; Pierre Gouzerh; Eric A. Maatta; Journal of the American Chemical Society 122 (2000) 639–649; doi:10.1021/ja9927974

data_4115898
_publ_contact_author
;
     Dr. E. A. Maatta
     Department of Chemistry
     Kansas State University
     Manhattan, KS  66506
     USA
;
_publ_contact_author_email       eam@ksu.edu
_publ_contact_author_fax         '+913 532 6666'
_publ_contact_author_phone       '+913 532 6665'
_publ_section_title
;
 A New Class of Functionalized Polyoxometalates: Synthetic, Structural,
 Spectroscopic, and Electrochemical Studies of Organoimido Derivatives of
 [Mo6O19]2-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              639
_journal_page_last               649
_journal_paper_doi               10.1021/ja9927974
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C96 H165 Cl4 Mo6 N7 O14'
_chemical_formula_weight         2358.79
_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                 112.02(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   59.94(4)
_cell_length_b                   15.486(13)
_cell_length_c                   28.99(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     24946(3)
_computing_cell_refinement       XSCANS
_computing_data_collection       'Siemens P4'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0910
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15742
_diffrn_reflns_theta_full        22.05
_diffrn_reflns_theta_max         22.05
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_type   N/A
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             9776
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.528
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.844
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         15265
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.845
_refine_ls_R_factor_all          0.1818
_refine_ls_R_factor_gt           0.1170
_refine_ls_shift/su_max          1.129
_refine_ls_shift/su_mean         0.069
_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          0.3157
_refine_ls_wR_factor_ref         0.3839
_reflns_number_gt                9201
_reflns_number_total             15291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9927974_3.cif
_cod_data_source_block           maa07
_cod_original_cell_volume        24944(34)
_cod_database_code               4115898