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_4115897
_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            'C36 H81 Mo6 N3 O18'
_chemical_formula_weight         1419.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.873(3)
_cell_length_b                   20.048(3)
_cell_length_c                   31.706(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                     10725(3)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        XDISK
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       wyckoff
_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  0.2194
_diffrn_reflns_av_sigmaI/netI    0.1220
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            8517
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        <1.0%
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.190
_exptl_absorpt_correction_T_min  0.165
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       block
_exptl_crystal_F_000             5712
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.193
_refine_ls_goodness_of_fit_obs   1.29
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         8394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.399
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_obs          0.0695
_refine_ls_shift/esd_max         0.087
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo)+(0.0010F^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0950
_refine_ls_wR_factor_obs         0.0746
_reflns_number_observed          3729
_reflns_number_total             8406
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9927974_2.cif
_cod_data_source_block           maam
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo)+(0.0010F^2^)]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/[\s^2^(Fo)+(0.0010F^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10725.2(32)
_cod_database_code               4115897