A Remarkable End-On Activation of Diazoalkane and Cleavage of Both C–Cl Bonds of Dichloromethane with a Silylene to a Single Product with Five-Coordinate Silicon Atoms
Sen, Sakya S.; Hey, Jakob; Kratzert, Daniel; Roesky, Herbert W.; Stalke, Dietmar; Organometallics 31 (2012) 435–; doi:10.1021/om201031n

data_4068053
_publ_section_title
;
 A Remarkable End-On Activation of Diazoalkane and Cleavage of Both C--Cl
 Bonds of Dichloromethane with a Silylene to a Single Product with
 Five-Coordinate Silicon Atoms
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              435
_journal_paper_doi               10.1021/om201031n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C31 H48 Cl4 N4 Si2'
_chemical_formula_sum            'C31 H48 Cl4 N4 Si2'
_chemical_formula_weight         674.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.029(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8427(7)
_cell_length_b                   13.6256(7)
_cell_length_c                   17.5591(8)
_cell_measurement_reflns_used    9604
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      2.23
_cell_volume                     3496.9(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2008.11'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            98691
_diffrn_reflns_theta_full        29.82
_diffrn_reflns_theta_max         29.82
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9145
_exptl_absorpt_correction_T_min  0.8714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         10034
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0322P)^2^+1.4476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                9075
_reflns_number_total             10034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201031n_si_002.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068053