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_7006844
_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
;
'C136 H228 K4 N16 O2 Si8, C72 H124 K2 N8 O2 Si4, 4(C4 H10 O)'
;
_chemical_formula_sum            'C224 H392 K6 N24 O8 Si12'
_chemical_formula_weight         4121.3
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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             2004-12-10T15:23:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.086(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.8776(7)
_cell_length_b                   15.9344(6)
_cell_length_c                   33.8306(11)
_cell_measurement_reflns_used    154669
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     12102.5(7)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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      -0.3562E-3
_diffrn_orient_matrix_UB_12      -0.62755E-1
_diffrn_orient_matrix_UB_13      -0.1395E-3
_diffrn_orient_matrix_UB_21      -0.346739E-1
_diffrn_orient_matrix_UB_22      0.5149E-3
_diffrn_orient_matrix_UB_23      -0.230611E-1
_diffrn_orient_matrix_UB_31      0.279568E-1
_diffrn_orient_matrix_UB_32      -0.1609E-3
_diffrn_orient_matrix_UB_33      -0.193764E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            32607
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4500
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.77
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         8638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1807
_refine_ls_R_factor_gt           0.1132
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+175.3251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2495
_reflns_number_gt                5263
_reflns_number_total             8638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514666f.txt
_cod_data_source_block           (14)-dec804
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7006844