A Stable Two-Coordinate Acyclic Silylene
Andrey V. Protchenko; Krishna Hassomal Birjkumar; Deepak Dange; Andrew D. Schwarz; Dragoslav Vidovic; Cameron Jones; Nikolas Kaltsoyannis; Philip Mountford; Simon Aldridge; Journal of the American Chemical Society 134 (2012) 6500–6503; doi:10.1021/ja301042u

data_4117832
_publ_contact_author
;
 Prof S. Aldridge
 Chemistry Research Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Simon.Aldridge@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 285201'
_publ_section_title
;
 A Stable Two-Coordinate Acyclic Silylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6500
_journal_page_last               6503
_journal_paper_doi               10.1021/ja301042u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C41 H62 B1 N3 Si1 Sn1'
_chemical_formula_sum            'C41 H62 B N3 Si Sn'
_chemical_formula_weight         754.55
_chemical_name_systematic
;
Sn{B(NDippCH)2}{N(SiMe3)Dipp}
;
_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
_audit_creation_date             10-08-04
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                85.2951(5)
_cell_angle_beta                 83.7451(5)
_cell_angle_gamma                76.5428(5)
_cell_formula_units_Z            4
_cell_length_a                   11.35860(10)
_cell_length_b                   14.4823(2)
_cell_length_c                   28.0668(4)
_cell_measurement_reflns_used    14200
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4455.78(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47603
_diffrn_reflns_theta_full        25.162
_diffrn_reflns_theta_max         27.650
_diffrn_reflns_theta_min         5.140
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.220
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as
contributions to the A and B parts of the calculated structure factors.

PLATON
PLATON, A Multipurpose Crystallographic Tool, A. L. Spek. Utrecht, 
the Netherlands, 1998.; A. Spek, J. Appl. Cryst. (2003), 36, 7-13.

SQUEEZE
A. Spek, J. Appl. Cryst. (2003), 36, 7-13; 
P. van der Sluis & A. L. Spek, Acta Cryst. (1990). A46, 194-201.

MCE
J. Rohlicek & M. Husak, J. Appl. Cryst. (2007), 40, 600-601.

;
_refine_diff_density_max         1.43
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9236
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         13262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.0008955
_refine_ls_shift/su_mean         2.9989126
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 7.45P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1220
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1220
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                9745
_reflns_number_total             19908
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.68
_oxford_diffrn_Wilson_scale      54.90
_oxford_refine_ls_r_factor_ref   0.0696
_oxford_refine_ls_scale          0.13783(4)
_oxford_reflns_number_all        13262
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 065apdv10
_cod_data_source_file            ja301042u_si_002_3.cif
_cod_data_source_block           COMPOUND_3-Sn
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C41 H62 B1 N3 Si1 Sn1'
_cod_database_code               4117832