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_7009276
_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         'C92 H120 N4 O6 SI4 MO2'
_chemical_formula_structural     'C92 H120 N4 O6 SI4 MO2'
_chemical_formula_sum            'C102 H114 Mo2 N4 O6 Si4'
_chemical_formula_weight         1796.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             1999-07-30T14:04:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                116.83(5)
_cell_angle_beta                 112.58(3)
_cell_angle_gamma                90.83(5)
_cell_formula_units_Z            1
_cell_length_a                   17.106(6)
_cell_length_b                   13.531(8)
_cell_length_c                   13.128(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     2438(3)
_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, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.1035
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8869
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.8849
_exptl_absorpt_correction_T_min  0.7802
_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            'tranaparent orange'
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'diamond plate'
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8552
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.176
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.134
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                5614
_reflns_number_total             8552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909712k.txt
_cod_data_source_block           lkmo2n
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2438(2)
_cod_database_code               7009276
_exptl_absorpt_factor_mur        0.12
_exptl_absorpt_correction_t_ave  0.833
_diffrn_standards_decay_corr_max 1.477
_diffrn_standards_decay_corr_min 0.996