#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/81/7108191.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7108191
loop_
_publ_author_name
'Yuichiro Tokoro'
'Hyeonuk Yeo'
'Kazuo Tanaka'
'Yoshiki Chujo'
_publ_section_title
;
 Synthesis of benzo[h]quinoline-based neutral pentacoordinate
 organosilicon complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8541
_journal_paper_doi               10.1039/c2cc34440h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C16 H17 N Si'
_chemical_formula_weight         251.40
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.586(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2798(6)
_cell_length_b                   6.9773(5)
_cell_length_c                   10.5690(8)
_cell_measurement_temperature    93(2)
_cell_volume                     682.13(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'Yadokari-XG (Wakita, 2000)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, 2000)'
_computing_publication_material  'Yadokari-XG (Wakita, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5341
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.9553
_exptl_absorpt_correction_T_min  0.9553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0812P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                1105
_reflns_number_total             1302
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2cc34440h.txt
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     -p_2yb
_cod_original_sg_symbol_H-M      p_21/m
_cod_database_code               7108191
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.60491(19) 0.0233(3) 0.7595(2) 0.0305(4) Uani 1 1 d .
H1 H 0.548(3) 0.044(4) 0.688(3) 0.086(9) Uiso 1 1 d .
H2 H 0.547(3) -0.021(4) 0.820(3) 0.088(9) Uiso 1 1 d .
H3 H 0.667(3) -0.071(4) 0.745(3) 0.080(8) Uiso 1 1 d .
C2 C 0.6628(3) 0.2500 0.9927(3) 0.0356(6) Uani 1 2 d S
H4 H 0.563(3) 0.2500 1.004(3) 0.041(7) Uiso 1 2 d S
H5 H 0.7022(19) 0.141(3) 1.0395(19) 0.041(5) Uiso 1 1 d .
C3 C 0.9000(2) 0.2500 0.8141(2) 0.0242(5) Uani 1 2 d S
C4 C 0.9746(2) 0.2500 0.6999(2) 0.0231(5) Uani 1 2 d S
C5 C 0.8976(2) 0.2500 0.5765(2) 0.0225(5) Uani 1 2 d S
C6 C 0.6768(3) 0.2500 0.4608(2) 0.0281(6) Uani 1 2 d S
H6 H 0.575(3) 0.2500 0.459(3) 0.040(7) Uiso 1 2 d S
C7 C 0.7396(3) 0.2500 0.3447(2) 0.0346(6) Uani 1 2 d S
H7 H 0.681(3) 0.2500 0.270(3) 0.039(7) Uiso 1 2 d S
C8 C 0.8880(3) 0.2500 0.3480(3) 0.0355(6) Uani 1 2 d S
H8 H 0.934(3) 0.2500 0.280(3) 0.061(10) Uiso 1 2 d S
C9 C 0.9717(2) 0.2500 0.4638(2) 0.0288(6) Uani 1 2 d S
C10 C 1.1266(3) 0.2500 0.4759(3) 0.0380(7) Uani 1 2 d S
H9 H 1.174(3) 0.2500 0.395(3) 0.066(10) Uiso 1 2 d S
C11 C 1.1996(3) 0.2500 0.5898(3) 0.0361(7) Uani 1 2 d S
H10 H 1.301(3) 0.2500 0.598(3) 0.043(8) Uiso 1 2 d S
C12 C 1.1285(2) 0.2500 0.7065(3) 0.0304(6) Uani 1 2 d S
C13 C 1.2069(2) 0.2500 0.8252(3) 0.0379(7) Uani 1 2 d S
H11 H 1.312(3) 0.2500 0.828(2) 0.038(7) Uiso 1 2 d S
C14 C 1.1372(3) 0.2500 0.9342(3) 0.0429(7) Uani 1 2 d S
H12 H 1.190(3) 0.2500 1.016(3) 0.049(8) Uiso 1 2 d S
C15 C 0.9855(3) 0.2500 0.9274(3) 0.0349(6) Uani 1 2 d S
H13 H 0.942(3) 0.2500 1.008(3) 0.056(9) Uiso 1 2 d S
Si1 Si 0.69532(6) 0.2500 0.81908(6) 0.0232(3) Uani 1 2 d S
N1 N 0.75089(19) 0.2500 0.57206(18) 0.0238(5) Uani 1 2 d S
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 0.0000 0.0000 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
C15 C3 C4 116.4(2) .
C15 C3 Si1 118.76(18) .
C4 C3 Si1 124.83(17) .
C12 C4 C5 117.9(2) .
C12 C4 C3 120.5(2) .
C5 C4 C3 121.59(19) .
N1 C5 C9 121.4(2) .
N1 C5 C4 117.14(19) .
C9 C5 C4 121.45(19) .
N1 C6 C7 124.0(2) .
C8 C7 C6 117.7(2) .
C7 C8 C9 120.5(2) .
C8 C9 C5 117.5(2) .
C8 C9 C10 124.2(2) .
C5 C9 C10 118.3(2) .
C11 C10 C9 120.9(2) .
C10 C11 C12 122.5(2) .
C13 C12 C4 119.4(2) .
C13 C12 C11 121.7(2) .
C4 C12 C11 118.9(2) .
C14 C13 C12 120.6(2) .
C13 C14 C15 119.8(3) .
C3 C15 C14 123.3(3) .
C1 Si1 C1 115.00(13) 4_565
C1 Si1 C2 102.98(8) 4_565
C1 Si1 C2 102.98(8) .
C1 Si1 C3 114.28(6) 4_565
C1 Si1 C3 114.28(6) .
C2 Si1 C3 105.35(12) .
C6 N1 C5 118.85(19) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 Si1 1.8755(17) .
C2 Si1 1.884(3) .
C3 C15 1.382(3) .
C3 C4 1.439(3) .
C3 Si1 1.904(2) .
C4 C12 1.424(3) .
C4 C5 1.436(3) .
C5 N1 1.359(3) .
C5 C9 1.422(3) .
C6 N1 1.314(3) .
C6 C7 1.400(4) .
C7 C8 1.375(4) .
C8 C9 1.397(4) .
C9 C10 1.433(3) .
C10 C11 1.333(4) .
C11 C12 1.445(4) .
C12 C13 1.399(4) .
C13 C14 1.365(4) .
C14 C15 1.404(4) .
Si1 C1 1.8755(17) 4_565
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_site_symmetry_4
C15 C3 C4 C12 0.0 .
Si1 C3 C4 C12 180.0 .
C15 C3 C4 C5 180.0 .
Si1 C3 C4 C5 0.0 .
C12 C4 C5 N1 180.0 .
C3 C4 C5 N1 0.0 .
C12 C4 C5 C9 0.0 .
C3 C4 C5 C9 180.0 .
N1 C6 C7 C8 0.0 .
C6 C7 C8 C9 0.0 .
C7 C8 C9 C5 0.0 .
C7 C8 C9 C10 180.0 .
N1 C5 C9 C8 0.0 .
C4 C5 C9 C8 180.0 .
N1 C5 C9 C10 180.0 .
C4 C5 C9 C10 0.0 .
C8 C9 C10 C11 180.0 .
C5 C9 C10 C11 0.0 .
C9 C10 C11 C12 0.0 .
C5 C4 C12 C13 180.0 .
C3 C4 C12 C13 0.0 .
C5 C4 C12 C11 0.0 .
C3 C4 C12 C11 180.0 .
C10 C11 C12 C13 180.0 .
C10 C11 C12 C4 0.0 .
C4 C12 C13 C14 0.0 .
C11 C12 C13 C14 180.0 .
C12 C13 C14 C15 0.000(1) .
C4 C3 C15 C14 0.000(1) .
Si1 C3 C15 C14 180.0 .
C13 C14 C15 C3 0.000(1) .
C15 C3 Si1 C1 112.30(8) 4_565
C4 C3 Si1 C1 -67.70(8) 4_565
C15 C3 Si1 C1 -112.30(8) .
C4 C3 Si1 C1 67.70(8) .
C15 C3 Si1 C2 0.0 .
C4 C3 Si1 C2 180.0 .
C7 C6 N1 C5 0.0 .
C9 C5 N1 C6 0.0 .
C4 C5 N1 C6 180.0 .
