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_4115899
_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            'C44 H89 Mo6 N3 O18'
_chemical_formula_weight         1523.82
_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                   18.432(7)
_cell_length_b                   20.580(9)
_cell_length_c                   31.379(12)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     11903(8)
_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      236(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10467
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        <1.0%
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.291
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       block
_exptl_crystal_F_000             6160
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.483
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.386
_refine_ls_goodness_of_fit_obs   1.70
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.685
_refine_ls_restrained_S_obs      1.70
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_obs          0.0780
_refine_ls_shift/esd_max         0.032
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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_all         0.1280
_refine_ls_wR_factor_obs         0.1056
_reflns_number_observed          5286
_reflns_number_total             10467
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9927974_4.cif
_cod_data_source_block           maaf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115899