High oxidation state imido metallasiloxanes: synthesis and structural characterisation of novel bis-imido chromium(VI) and molybdenum(VI) compounds †
King, Lawrence; Motevalli, Majid; Sullivan, Alice C.; Journal of the Chemical Society, Dalton Transactions  (2000) 1357–; doi:10.1039/a909712k

data_7009277
_publ_section_title
;
 High oxidation state imido metallasiloxanes: synthesis and structural
 characterisation of novel bis-imido chromium(VI) and molybdenum(VI)
 compounds&#x200A;&#x2020;
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1357
_journal_paper_doi               10.1039/a909712k
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C64 H76 Mo1 N4 O6 Si4'
_chemical_formula_structural     'C64 H76 N4 O6 SI4 MO'
_chemical_formula_sum            'C64 H76 Mo2 N4 O6 Si4'
_chemical_formula_weight         1301.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1999-08-27T15:56:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.07(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.395(2)
_cell_length_b                   15.831(3)
_cell_length_c                   17.246(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     3332.0(11)
_computing_cell_refinement       'CAD4/PC (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4/PC (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97(Sheldrick,1997)
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.1991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5846
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.9981
_exptl_absorpt_correction_T_min  0.2933
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.951
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0018(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5846
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.2106
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2059
_refine_ls_wR_factor_ref         0.2454
_reflns_number_gt                2470
_reflns_number_total             5846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909712k.txt
_cod_data_source_block           lkmo2
_cod_original_cell_volume        3332.0(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7009277
_exptl_absorpt_factor_mur        0
_exptl_absorpt_correction_t_ave  0.5609
_diffrn_standards_decay_corr_max 1.03
_diffrn_standards_decay_corr_min 0.973