Reactions of a stable silylene with halocarbons.
Delawar, Mahmood; Gehrhus, Barbara; Hitchcock, Peter B.; Dalton transactions (Cambridge, England : 2003)  (2005) 2945–2953; doi:10.1039/b507462b

data_7008773
_publ_section_title
;
 Reactions of a stable silylene with halocarbons.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2945
_journal_page_last               2953
_journal_paper_doi               10.1039/b507462b
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C65 H106 Br2 N8 Si4, 1.5(C6 H6)'
_chemical_formula_sum            'C74 H115 Br2 N8 Si4'
_chemical_formula_weight         1388.92
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-09-10T16:39:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.796(1)
_cell_angle_beta                 67.561(1)
_cell_angle_gamma                76.029(1)
_cell_formula_units_Z            2
_cell_length_a                   14.8293(3)
_cell_length_b                   15.1696(3)
_cell_length_c                   19.1719(3)
_cell_measurement_reflns_used    34268
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     3861.41(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.736879E-1
_diffrn_orient_matrix_UB_12      -0.23609E-1
_diffrn_orient_matrix_UB_13      -0.121091E-1
_diffrn_orient_matrix_UB_21      -0.152519E-1
_diffrn_orient_matrix_UB_22      -0.36216E-1
_diffrn_orient_matrix_UB_23      0.459599E-1
_diffrn_orient_matrix_UB_31      0.13337E-2
_diffrn_orient_matrix_UB_32      -0.525568E-1
_diffrn_orient_matrix_UB_33      -0.306128E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52154
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_correction_T_min  0.7024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1482
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         13561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+3.5470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                10267
_reflns_number_total             13561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b507462b.txt
_cod_data_source_block           (11d)-sep1504
_cod_original_cell_volume        3861.41(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008773