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_4115486
_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            'C41.5 H83 I Mo6 N3 O18.5'
_chemical_formula_weight         1622.64
_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                103.7260(10)
_cell_angle_beta                 92.3190(10)
_cell_angle_gamma                99.7870(10)
_cell_formula_units_Z            4
_cell_length_a                   12.4358(5)
_cell_length_b                   19.0658(8)
_cell_length_c                   25.4922(11)
_cell_measurement_reflns_used    7324
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.4
_cell_volume                     5765.5(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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46185
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    1.868
_exptl_absorpt_correction_T_max  0.5610
_exptl_absorpt_correction_T_min  0.4870
_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    1.867
_exptl_crystal_description       prism
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.442
_refine_diff_density_min         -4.809
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1293
_refine_ls_number_reflns         25005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.285
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+37.7166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                19793
_reflns_number_total             25005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004033q_2.cif
_cod_data_source_block           Id
_cod_original_cell_volume        5765.4(4)
_cod_original_formula_sum        'C41.50 H83 I Mo6 N3 O18.50'
_cod_database_code               4115486