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_4117830
_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_absolute_configuration ad
_chemical_formula_moiety         'C41 H62 B1 I2 N3 Si2'
_chemical_formula_sum            'C41 H62 B I2 N3 Si2'
_chemical_formula_weight         917.75
_chemical_name_systematic
;
(I)2Si(B(L))(N(SiMe3)(2,6-C6H3iPr2))
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             11-10-05
_audit_creation_method           CRYSTALS_ver_14.21
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.35230(10)
_cell_length_b                   17.74500(10)
_cell_length_c                   22.19420(10)
_cell_measurement_reflns_used    5644
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4470.95(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10186
_diffrn_reflns_theta_full        27.481
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         5.136
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.49
_refine_ls_abs_structure_details 'Flack (1983), 4568 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.040(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9002
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.0014401
_refine_ls_shift/su_mean         0.0000577
_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: 
 0.691 0.822 0.649 0.343 0.163 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0349
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0281
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                9338
_reflns_number_total             10186
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.59
_oxford_diffrn_Wilson_scale      42.79
_oxford_refine_ls_r_factor_ref   0.0274
_oxford_refine_ls_scale          0.15278(10)
_oxford_reflns_number_all        10186
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'ADS207 At 15: 6 on 5/10'
_cod_data_source_file            ja301042u_si_002_1.cif
_cod_data_source_block           COMPOUND_diiodide
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C41 H62 B1 I2 N3 Si2'
_cod_database_code               4117830