Insights into the making of a stable silylene.
Gehrhus, Barbara; Hitchcock, Peter B.; Pongtavornpinyo, Ruti; Zhang, Lihong; Dalton transactions (Cambridge, England : 2003)  (2006) 1847–1857; doi:10.1039/b514666f

data_7006843
_publ_section_title
;
 Insights into the making of a stable silylene.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1847
_journal_page_last               1857
_journal_paper_doi               10.1039/b514666f
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
;
C64 H104 N8 Si4, C24 H48 Na O6, C20 H40 Na O5, 2(C4 H8 O)
;
_chemical_formula_sum            'C116 H208 N8 Na2 O13 Si4'
_chemical_formula_weight         2081.24
_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             2004-04-15T11:18:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                85.999(1)
_cell_angle_beta                 79.241(1)
_cell_angle_gamma                89.254(1)
_cell_formula_units_Z            2
_cell_length_a                   14.3212(2)
_cell_length_b                   15.2868(2)
_cell_length_c                   28.9584(4)
_cell_measurement_reflns_used    76591
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     6213.10(15)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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      -0.346375E-1
_diffrn_orient_matrix_UB_12      0.203919E-1
_diffrn_orient_matrix_UB_13      0.306239E-1
_diffrn_orient_matrix_UB_21      0.597654E-1
_diffrn_orient_matrix_UB_22      0.27484E-1
_diffrn_orient_matrix_UB_23      0.52968E-2
_diffrn_orient_matrix_UB_31      -0.167369E-1
_diffrn_orient_matrix_UB_32      0.559372E-1
_diffrn_orient_matrix_UB_33      -0.165977E-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  0.0511
_diffrn_reflns_av_unetI/netI     0.0439
_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       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            82730
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.74
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1056
_refine_ls_number_reflns         21654
_refine_ls_number_restraints     744
_refine_ls_restrained_S_all      4.701
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.1056
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1843P)^2^+18.8612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2858
_refine_ls_wR_factor_ref         0.3128
_reflns_number_gt                16448
_reflns_number_total             21654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514666f.txt
_cod_data_source_block           (13)-apr404
_cod_original_cell_volume        6213.1(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7006843