An Efficient and Convenient Reaction Protocol to Organoimido Derivatives of Polyoxometalates
Yongge Wei; Bubin Xu; Charles L. Barnes; Zhonghua Peng; Journal of the American Chemical Society 123 (2001) 4083–4084; doi:10.1021/ja004033q

data_4115487
_publ_section_title
;
 An Efficient and Convenient Reaction Protocol to Organoimido Derivatives
 of Polyoxometalates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4083
_journal_page_last               4084
_journal_paper_doi               10.1021/ja004033q
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C40 H81 Mo6 N3 O18'
_chemical_formula_weight         1467.72
_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                107.3230(10)
_cell_angle_beta                 97.3240(10)
_cell_angle_gamma                100.0180(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1352(10)
_cell_length_b                   12.4919(10)
_cell_length_c                   19.6515(16)
_cell_measurement_reflns_used    7390
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.2
_cell_volume                     2749.1(4)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18152
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  0.8182
_exptl_absorpt_correction_T_min  0.6799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       rods
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.323
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.868
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+33.3046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                6737
_reflns_number_total             9295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004033q_3.cif
_cod_data_source_block           Ia
_cod_database_code               4115487