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_4079892
_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         'C30 H46 Cl N O2 Si, 2 (C6 H6)'
_chemical_formula_sum            'C42 H58 Cl N O2 Si'
_chemical_formula_weight         672.43
_chemical_name_common            'ClMeSi(ON[Me]O).2 C6H6'
_chemical_name_systematic
; 
2,4,8,10-Tetra-tert-butyl-6-chloro-6,12-dimethyl-12H-
dibenzo[d,g][1,3,6,2]dioxazasilocine bisbenzene solvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7339(6)
_cell_length_b                   17.7599(11)
_cell_length_c                   23.0354(14)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    121(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.27
_cell_volume                     3982.2(4)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      121(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51138
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.9873
_exptl_absorpt_correction_T_min  0.9566
_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            'pale pink'
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1456
_exptl_crystal_recrystallization_method
;
 Crystals were grown from benzene. 
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.765
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         9109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1635
_reflns_number_gt                6873
_reflns_number_total             9109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301028c_si_002.cif
_cod_data_source_block           ss130_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4079892