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_4115896
_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            'C74 H135 Cl6 Mo6 N5 O16'
_chemical_formula_weight         2139.21
_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                92.03(3)
_cell_angle_beta                 101.77(3)
_cell_angle_gamma                98.51(2)
_cell_formula_units_Z            4
_cell_length_a                   19.573(4)
_cell_length_b                   21.725(5)
_cell_length_c                   23.668(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     9722(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'Siemens P4'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXTL-PLUS 4.2 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.556
_diffrn_measured_fraction_theta_max 0.556
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omege
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       -1
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14127
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_type   N/A
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.88
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         14119
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.97
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.260
_refine_ls_shift/su_mean         0.011
_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          0.1383
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                8920
_reflns_number_total             14127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9927974_1.cif
_cod_data_source_block           maa08
_cod_database_code               4115896