#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/34/2213405.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2213405
loop_
_publ_author_name
'Jaganyi, Deogratius'
'Chathuri, Udhir'
'Munro, Orde Q.'
_publ_section_title
;
 N-Boranyl-N-(trimethylsilyl)pyrrolidine
;
_journal_coeditor_code           HK2228
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2689
_journal_page_last               o2689
_journal_paper_doi               10.1107/S1600536807019344
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C7 H20 B N Si'
_chemical_formula_moiety         'C7 H20 B N Si'
_chemical_formula_sum            'C7 H20 B N Si'
_chemical_formula_weight         157.14
_chemical_name_systematic
;
N-Boranyl-N-(trimethylsilyl)pyrrolidine
;
_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'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.080(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.613(5)
_cell_length_b                   10.321(5)
_cell_length_c                   11.753(5)
_cell_measurement_reflns_used    4177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.8768
_cell_measurement_theta_min      3.7566
_cell_volume                     1003.9(9)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis  RED'
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 8.4190
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.598
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2 CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6834
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         33.89
_diffrn_reflns_theta_min         3.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 33
_diffrn_standards_interval_time  0
_diffrn_standards_number         16
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9709
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.04
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0589P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                1970
_reflns_number_total             2436
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hk2228.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2213405
_cod_database_fobs_code          2213405
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C1 0.85439(13) 0.12797(11) 0.34325(10) 0.0169(2) Uani d 1
C C2 0.68293(13) 0.15220(11) 0.35366(10) 0.0194(3) Uani d 1
C C3 0.66737(13) 0.30030(12) 0.36165(10) 0.0194(3) Uani d 1
C C4 0.82484(12) 0.35392(11) 0.34436(10) 0.0153(2) Uani d 1
C C5 1.24120(13) 0.41217(11) 0.40765(11) 0.0198(3) Uani d 1
C C6 1.06149(15) 0.29146(14) 0.17331(11) 0.0239(3) Uani d 1
C C7 1.24759(15) 0.11565(12) 0.36983(13) 0.0257(3) Uani d 1
B B 1.00502(16) 0.24707(13) 0.53477(12) 0.0185(3) Uani d 1
N N 0.94841(11) 0.24928(8) 0.38998(8) 0.0124(2) Uani d 1
Si Si 1.12767(3) 0.26715(3) 0.33653(3) 0.01435(12) Uani d 1
H H1A 0.9113(13) 0.0563(12) 0.3895(10) 0.021(3) Uiso d 1
H H1B 0.8533(14) 0.1164(13) 0.2613(11) 0.023(3) Uiso d 1
H H2A 0.6659(14) 0.1066(13) 0.4225(10) 0.024(3) Uiso d 1
H H2B 0.6058(14) 0.1173(12) 0.2842(10) 0.021(3) Uiso d 1
H H3A 0.5724(14) 0.3351(12) 0.2980(11) 0.022(3) Uiso d 1
H H3B 0.6545(15) 0.3236(13) 0.4371(12) 0.028(3) Uiso d 1
H H4A 0.8639(13) 0.4323(12) 0.3881(10) 0.017(3) Uiso d 1
H H4B 0.8130(13) 0.3645(11) 0.2611(10) 0.013(3) Uiso d 1
H H5A 1.1743(16) 0.4884(14) 0.3951(12) 0.037(4) Uiso d 1
H H5B 1.2849(14) 0.3980(12) 0.4911(11) 0.023(3) Uiso d 1
H H5C 1.3241(16) 0.4273(13) 0.3727(11) 0.033(4) Uiso d 1
H H6A 0.9977(19) 0.2279(14) 0.1352(13) 0.042(5) Uiso d 1
H H6B 1.1574(19) 0.2906(14) 0.1439(14) 0.041(4) Uiso d 1
H H6C 1.0107(16) 0.3754(17) 0.1528(11) 0.046(4) Uiso d 1
H H7A 1.3255(19) 0.1171(15) 0.3272(12) 0.051(4) Uiso d 1
H H7B 1.2976(18) 0.1068(15) 0.4542(14) 0.051(5) Uiso d 1
H H7C 1.1859(17) 0.0430(16) 0.3421(12) 0.047(4) Uiso d 1
H H8A 0.9040(16) 0.2120(13) 0.5674(12) 0.033(4) Uiso d 1
H H8B 1.0372(15) 0.3472(13) 0.5678(10) 0.030(4) Uiso d 1
H H8C 1.1110(16) 0.1800(14) 0.5637(11) 0.040(4) Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N C1 C2 105.47(9) ?
N C1 H1A 107.0(7) ?
C2 C1 H1A 115.4(7) ?
N C1 H1B 108.7(8) ?
C2 C1 H1B 110.8(7) ?
H1A C1 H1B 109.2(10) ?
C1 C2 C3 105.57(8) ?
C1 C2 H2A 110.7(7) ?
C3 C2 H2A 113.0(7) ?
C1 C2 H2B 108.8(7) ?
C3 C2 H2B 111.7(8) ?
H2A C2 H2B 107.0(10) ?
C4 C3 C2 104.82(9) ?
C4 C3 H3A 109.8(7) ?
C2 C3 H3A 112.0(7) ?
C4 C3 H3B 111.6(8) ?
C2 C3 H3B 110.0(8) ?
H3A C3 H3B 108.7(10) ?
N C4 C3 104.97(9) ?
N C4 H4A 107.6(7) ?
C3 C4 H4A 115.0(7) ?
N C4 H4B 108.0(7) ?
C3 C4 H4B 109.2(7) ?
H4A C4 H4B 111.7(9) ?
Si C5 H5A 111.9(8) ?
Si C5 H5B 110.3(8) ?
H5A C5 H5B 109.2(11) ?
Si C5 H5C 108.0(8) ?
H5A C5 H5C 107.2(11) ?
H5B C5 H5C 110.2(11) ?
Si C6 H6A 112.9(10) ?
Si C6 H6B 108.4(9) ?
H6A C6 H6B 106.2(12) ?
Si C6 H6C 111.4(8) ?
H6A C6 H6C 111.1(12) ?
H6B C6 H6C 106.7(11) ?
Si C7 H7A 108.1(10) ?
Si C7 H7B 111.0(9) ?
H7A C7 H7B 111.4(13) ?
Si C7 H7C 112.2(9) ?
H7A C7 H7C 104.5(12) ?
H7B C7 H7C 109.5(12) ?
N B H8A 109.2(7) yes
N B H8B 108.9(6) yes
H8A B H8B 109.1(9) yes
N B H8C 107.9(7) yes
H8A B H8C 110.3(10) yes
H8B B H8C 111.4(9) yes
C4 N C1 102.14(9) yes
C4 N B 110.97(8) yes
C1 N B 110.02(8) yes
C4 N Si 112.67(7) yes
C1 N Si 112.16(7) yes
B N Si 108.77(7) yes
N Si C7 108.42(6) yes
N Si C5 108.43(5) yes
C7 Si C5 113.07(7) yes
N Si C6 108.71(6) yes
C7 Si C6 108.96(6) yes
C5 Si C6 109.17(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N 1.5095(14) yes
C1 C2 1.5357(17) ?
C1 H1A 0.967(12) ?
C1 H1B 0.968(12) ?
C2 C3 1.5395(18) ?
C2 H2A 0.982(12) ?
C2 H2B 0.968(12) ?
C3 C4 1.5296(16) ?
C3 H3A 1.010(12) ?
C3 H3B 0.955(13) ?
C4 N 1.5068(14) yes
C4 H4A 0.967(12) ?
C4 H4B 0.961(11) ?
C5 Si 1.8553(13) yes
C5 H5A 0.962(14) ?
C5 H5B 0.959(12) ?
C5 H5C 0.931(14) ?
C6 Si 1.8606(15) yes
C6 H6A 0.893(15) ?
C6 H6B 0.980(16) ?
C6 H6C 0.971(17) ?
C7 Si 1.8551(14) yes
C7 H7A 0.943(16) ?
C7 H7B 0.969(15) ?
C7 H7C 0.925(16) ?
B N 1.6354(17) yes
B H8A 1.104(14) yes
B H8B 1.112(13) yes
B H8C 1.121(13) yes
N Si 1.8303(13) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
N C1 C2 C3 20.37(11) yes
C1 C2 C3 C4 4.88(11) yes
C2 C3 C4 N -28.50(11) yes
C3 C4 N C1 41.07(11) yes
C3 C4 N B -76.15(10) ?
C3 C4 N Si 161.60(7) ?
C2 C1 N C4 -37.80(11) yes
C2 C1 N B 80.10(10) ?
C2 C1 N Si -158.69(7) ?
C4 N Si C7 -167.46(7) ?
C1 N Si C7 -52.87(9) ?
B N Si C7 69.06(8) ?
C4 N Si C5 69.43(9) ?
C1 N Si C5 -175.98(7) ?
B N Si C5 -54.05(8) ?
C4 N Si C6 -49.15(9) ?
C1 N Si C6 65.44(8) ?
B N Si C6 -172.63(7) ?
