1,1-Bis(N-methylimidazole)-2-(trimethylsilyl)-1-boracyclohexa-1,4-diene Chloride: A Stable Intermediate or Tangent en Route to 1-(N-Methylimidazole)borabenzene?
Cade, Ian A.; Hill, Anthony F.; Organometallics 31 (2012) 2112–; doi:10.1021/om300002y

data_4076529
_publ_section_title
;
 1,1-Bis(N-methylimidazole)-2-(trimethylsilyl)-1-boracyclohexa-1,4-diene
 Chloride: A Stable Intermediate or Tangent en Route to
 1-(N-Methylimidazole)borabenzene?
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              2112
_journal_paper_doi               10.1021/om300002y
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C16 H26 B N4 Si, 0.5(C6 H6), Cl'
_chemical_formula_sum            'C19 H29 B Cl N4 Si'
_chemical_formula_weight         387.82
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 112.1070(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.9186(10)
_cell_length_b                   9.7530(3)
_cell_length_c                   13.6534(3)
_cell_measurement_reflns_used    15032
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.55
_cell_volume                     4431.3(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_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      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23296
_diffrn_reflns_theta_full        25.031
_diffrn_reflns_theta_max         25.031
_diffrn_reflns_theta_min         2.566
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.52
_refine_ls_extinction_coef       230(40)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8612
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3906
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.007324
_refine_ls_structure_factor_coef Fsqd
_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: 
 78.4 123. 61.5 15.1 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1958
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1958
_reflns_limit_h_max              39
_reflns_limit_h_min              -42
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2845
_reflns_number_total             3906
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.22
_oxford_diffrn_Wilson_scale      13.11
_oxford_refine_ls_r_factor_ref   0.0616
_oxford_refine_ls_scale          0.2860(7)
_oxford_reflns_number_all        3906
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om300002y_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C19 H29 B1 Cl1 N4 Si1'
_cod_database_code               4076529