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_4076530
_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), H2 O, Cl'
_chemical_formula_sum            'C19 H31 B Cl N4 O Si'
_chemical_formula_weight         405.83
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 108.3260(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7787(2)
_cell_length_b                   10.0476(2)
_cell_length_c                   18.6854(3)
_cell_measurement_reflns_used    24986
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     2277.44(7)
_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    '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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.064
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52170
_diffrn_reflns_theta_full        27.474
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.632
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.41
_refine_ls_extinction_coef       82(12)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9786
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5193
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.0002357
_refine_ls_shift/su_mean         0.0000409
_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: 
 13.7 20.6 10.3 2.90 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1082
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.1082
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3034
_reflns_number_total             5211
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      4.98
_oxford_refine_ls_r_factor_ref   0.0641
_oxford_refine_ls_scale          0.3646(4)
_oxford_reflns_number_all        5193
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om300002y_si_003.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.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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      'P 1 2/a 1 '
_cod_original_formula_sum        'C19 H31 B1 Cl1 N4 O1 Si1'
_cod_database_code               4076530
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE O   (  1,X'S) H   ( 1,X'S) H   ( 2,X'S) 
RIDE C   (  11,X'S) H   ( 113,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 123,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 163,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 203,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  32,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
REM DIST 1.0, 0.05 = O(1) TO H(1001), O(1) TO H(1002) 
REM REM CONT O(5) TO H(503), O(5) TO H(504) 
REM ANGLE 109.5, 0.03 = H(1001) TO O(1) TO H(1002) 
REM ANGLE 109.5, 0.03 = H(501) TO O(5) TO H(503) 
REM ANGLE 109.5, 0.03 = H(501) TO N(5) TO H(504) 
REM ANGLE 109.5, 0.03 = H(502) TO N(5) TO H(503) 
REM ANGLE 109.5, 0.03 = H(502) TO N(5) TO H(504) 
REM ANGLE 109.5, 0.03 = H(503) TO N(5) TO H(504) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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