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_4117837
_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         'C40 H60 Br2 N2 Si4'
_chemical_formula_sum            'C40 H60 Br2 N2 Si4'
_chemical_formula_weight         841.08
_chemical_name_systematic
;
[(Si{N(Dipp)SiMe3}Br)2C10H10]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.04(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.738(2)
_cell_length_b                   27.404(6)
_cell_length_c                   15.095(3)
_cell_measurement_reflns_used    7577
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     4309.2(16)
_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 0.978
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12215
_diffrn_reflns_theta_full        25.225
_diffrn_reflns_theta_max         26.005
_diffrn_reflns_theta_min         5.115
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.021
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       cube
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         4566
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.0011291
_refine_ls_shift/su_mean         0.0000335
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.956 0.584 0.741 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1031
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0597
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4566
_reflns_number_total             8279
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.96
_oxford_diffrn_Wilson_scale      51.96
_oxford_refine_ls_r_factor_ref   0.0603
_oxford_refine_ls_scale          0.0972(2)
_oxford_reflns_number_all        8279
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ja301042u_si_002_8.cif
_cod_data_source_block           COMPOUND_4
_cod_original_cell_volume        4309.3(16)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4117837