Migrations of Alkyl and Aryl Groups from Silicon to Nitrogen in Silylated Aryloxyiminoquinones
Shekar, Sukesh; Brown, Seth N.; Organometallics 32 (2013) 556–; doi:10.1021/om301028c

data_4079899
_publ_section_title
;
 Migrations of Alkyl and Aryl Groups from Silicon to Nitrogen in Silylated
 Aryloxyiminoquinones
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              556
_journal_paper_doi               10.1021/om301028c
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C60 H92 N2 O5 Si2, 2(C6 H6)'
_chemical_formula_sum            'C72 H104 N2 O5 Si2'
_chemical_formula_weight         1133.75
_chemical_name_common
'(ON[Me]O)Si(Me)(\m-O)Si(Me)(ON[Me]O) . 2 C6H6'
_chemical_name_systematic
; 
 Oxidobis(6,6'-2,4,8,10-Tetra-tert-butyl-6,12-dimethyl-12H-
dibenzo[d,g][1,3,6,2]dioxazasilocine) dibenzene solvate
;
_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                72.58(3)
_cell_angle_beta                 84.92(3)
_cell_angle_gamma                89.92(3)
_cell_formula_units_Z            2
_cell_length_a                   13.041(3)
_cell_length_b                   15.124(3)
_cell_length_c                   18.205(4)
_cell_measurement_reflns_used    7442
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.802
_cell_measurement_theta_min      2.257
_cell_volume                     3411.3(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28757
_diffrn_reflns_theta_full        23.13
_diffrn_reflns_theta_max         23.13
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9940
_exptl_absorpt_correction_T_min  0.9628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. 
Madison, WI USA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         9590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+3.4248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                7469
_reflns_number_total             9590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301028c_si_002.cif
_cod_data_source_block           ss111
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3411.4(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079899