Formation of a Unsymmetrical Ring System via C‒H Bond Activation of Diazobenzene by Stable N-Heterocyclic Chlorosilylene (PhC(NtBu)2SiCl)
Khan, Shabana; Sen, Sakya S.; Michel, Reent; Kratzert, Daniel; Roesky, Herbert W.; Stalke, Dietmar; Organometallics 30 (2011) 2643–; doi:10.1021/om200207v

data_4064597
_publ_section_title
;
 Formation of a Unsymmetrical Ring System via C--H Bond Activation of
 Diazobenzene by Stable N-Heterocyclic Chlorosilylene (PhC(NtBu)2SiCl)
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2643
_journal_paper_doi               10.1021/om200207v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C42 H55 Cl N6 Si2, C7 H8'
_chemical_formula_sum            'C49 H63 Cl N6 Si2'
_chemical_formula_weight         827.68
_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                94.310(2)
_cell_angle_beta                 97.304(2)
_cell_angle_gamma                108.196(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3427(11)
_cell_length_b                   10.7563(13)
_cell_length_c                   12.2182(15)
_cell_measurement_reflns_used    9210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.392
_cell_measurement_theta_min      2.324
_cell_volume                     1148.4(2)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2010.7-0'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XP in SHELXTL Version 2008/3'
_computing_publication_material  'XP in SHELXTL Version 2008/3'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Quazar mirror optics'
_diffrn_radiation_source         'INCOATEC Mo Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27534
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.98392
_exptl_absorpt_correction_T_min  0.89511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0150P)^2^+2.3944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                4419
_reflns_number_total             4737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200207v_si_001.cif
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064597