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#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/51/4315124.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_4315124
loop_
_publ_author_name
'Gerrit W. Fester'
'Jana Eckstein'
'Daniela Gerlach'
'Jörg Wagler'
'Erica Brendler'
'Edwin Kroke'
_publ_contact_author
;Wagler, Jörg 
 Institut für Anorganische Chemie  
 Technische Universität Bergakademie Freiberg
 Leipziger Str. 29 
 09596 Freiberg 
 Bundesrepublik Deutschland
;
_publ_contact_author_fax         '03731 39-4058 '
_publ_contact_author_phone       '03731 39-3556 '
_publ_section_title
;
 Reactions of Hydridochlorosilanes with 2,2'-Bipyridine and
 1,10-Phenanthroline: Complexation versus Dismutation and
 Metal-Catalyst-Free 1,4-Hydrosilylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2667
_journal_page_last               2673
_journal_paper_doi               10.1021/ic901620e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C10 H9 Cl3 N2 Si'
_chemical_formula_sum            'C10 H9 Cl3 N2 Si'
_chemical_formula_weight         291.63
_chemical_name_systematic
;
 trichlorosilane 2,2'-bipyridine complex
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.940(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4724(6)
_cell_length_b                   7.6648(3)
_cell_length_c                   12.9933(6)
_cell_measurement_reflns_used    3504
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      2.39
_cell_volume                     1235.47(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 (Farugia)'
_computing_publication_material  'Shelx-97/ciftab(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15199
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.8678
_exptl_absorpt_correction_T_min  0.7897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         4277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0451
_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)+(0.0420P)²+1.8867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                3433
_reflns_number_total             4277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901620e_si_002_2.cif
_cod_data_source_block           compound_2b
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4315124
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.24646(4) 0.36411(7) 0.11154(4) 0.01532(11) Uani 1 1 d . . .
Cl2 Cl 0.19732(4) -0.19754(7) 0.03864(4) 0.01930(12) Uani 1 1 d . . .
Cl3 Cl 0.33393(4) 0.10591(8) -0.04988(4) 0.02015(13) Uani 1 1 d . . .
Si1 Si 0.21891(5) 0.08727(8) 0.06430(5) 0.01287(12) Uani 1 1 d . . .
H1A H 0.122(2) 0.140(4) -0.033(2) 0.015 Uiso 1 1 d . . .
N1 N 0.12568(14) 0.0702(2) 0.17414(14) 0.0131(3) Uani 1 1 d . . .
N2 N 0.32722(14) 0.0244(2) 0.17926(14) 0.0130(3) Uani 1 1 d . . .
C1 C 0.01908(17) 0.0945(3) 0.15774(19) 0.0174(4) Uani 1 1 d . . .
H1 H -0.0132 0.1165 0.0895 0.021 Uiso 1 1 calc R . .
C2 C -0.04492(18) 0.0880(3) 0.2382(2) 0.0210(5) Uani 1 1 d . . .
H2 H -0.1209 0.1011 0.2253 0.025 Uiso 1 1 calc R . .
C3 C 0.00307(19) 0.0621(3) 0.3381(2) 0.0220(5) Uani 1 1 d . . .
H3 H -0.0395 0.0616 0.3946 0.026 Uiso 1 1 calc R . .
C4 C 0.11430(18) 0.0369(3) 0.35514(18) 0.0183(4) Uani 1 1 d . . .
H4 H 0.1488 0.0188 0.4230 0.022 Uiso 1 1 calc R . .
C5 C 0.17286(17) 0.0391(3) 0.27054(17) 0.0136(4) Uani 1 1 d . . .
C6 C 0.28901(16) 0.0070(3) 0.27292(16) 0.0143(4) Uani 1 1 d . . .
C7 C 0.35545(18) -0.0406(3) 0.36060(18) 0.0186(4) Uani 1 1 d . . .
H7 H 0.3273 -0.0517 0.4255 0.022 Uiso 1 1 calc R . .
C8 C 0.46336(19) -0.0718(3) 0.35205(18) 0.0214(5) Uani 1 1 d . . .
H8 H 0.5104 -0.1055 0.4109 0.026 Uiso 1 1 calc R . .
C9 C 0.50220(19) -0.0529(4) 0.25599(19) 0.0218(5) Uani 1 1 d . . .
H9 H 0.5763 -0.0723 0.2488 0.026 Uiso 1 1 calc R . .
C10 C 0.43194(17) -0.0057(3) 0.17114(17) 0.0172(4) Uani 1 1 d . . .
H10 H 0.4585 0.0056 0.1055 0.021 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Si1 N2 80.87(8) . . ?
N1 Si1 Cl3 175.62(6) . . ?
N2 Si1 Cl3 94.85(6) . . ?
N1 Si1 Cl2 88.36(6) . . ?
N2 Si1 Cl2 86.34(6) . . ?
Cl3 Si1 Cl2 92.32(3) . . ?
N1 Si1 Cl1 87.05(6) . . ?
N2 Si1 Cl1 87.14(6) . . ?
Cl3 Si1 Cl1 91.81(3) . . ?
Cl2 Si1 Cl1 172.55(4) . . ?
N1 Si1 H1A 97.5(9) . . ?
N2 Si1 H1A 178.3(9) . . ?
Cl3 Si1 H1A 86.8(9) . . ?
Cl2 Si1 H1A 93.3(9) . . ?
Cl1 Si1 H1A 93.1(9) . . ?
C1 N1 C5 120.22(19) . . ?
C1 N1 Si1 122.42(15) . . ?
C5 N1 Si1 117.31(14) . . ?
C10 N2 C6 119.23(18) . . ?
C10 N2 Si1 125.46(15) . . ?
C6 N2 Si1 115.29(14) . . ?
N1 C1 C2 121.2(2) . . ?
N1 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C1 C2 C3 119.1(2) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 119.6(2) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 118.1(2) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
N1 C5 C4 121.7(2) . . ?
N1 C5 C6 112.60(19) . . ?
C4 C5 C6 125.7(2) . . ?
N2 C6 C7 121.78(19) . . ?
N2 C6 C5 113.69(18) . . ?
C7 C6 C5 124.5(2) . . ?
C8 C7 C6 118.9(2) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C7 C8 C9 119.1(2) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 119.4(2) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
N2 C10 C9 121.6(2) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Si1 2.2256(8) . ?
Cl2 Si1 2.2206(8) . ?
Cl3 Si1 2.1724(8) . ?
Si1 N1 1.9364(19) . ?
Si1 N2 1.9674(18) . ?
Si1 H1A 1.70(3) . ?
N1 C1 1.338(3) . ?
N1 C5 1.349(3) . ?
N2 C10 1.341(3) . ?
N2 C6 1.359(3) . ?
C1 C2 1.381(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.386(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.467(3) . ?
C6 C7 1.386(3) . ?
C7 C8 1.383(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Si1 N1 C1 -178.26(19) . . . . ?
Cl2 Si1 N1 C1 -91.70(18) . . . . ?
Cl1 Si1 N1 C1 94.17(18) . . . . ?
N2 Si1 N1 C5 4.32(16) . . . . ?
Cl2 Si1 N1 C5 90.87(16) . . . . ?
Cl1 Si1 N1 C5 -83.25(16) . . . . ?
N1 Si1 N2 C10 176.1(2) . . . . ?
Cl3 Si1 N2 C10 -4.8(2) . . . . ?
Cl2 Si1 N2 C10 87.19(19) . . . . ?
Cl1 Si1 N2 C10 -96.41(19) . . . . ?
N1 Si1 N2 C6 -2.16(16) . . . . ?
Cl3 Si1 N2 C6 176.89(15) . . . . ?
Cl2 Si1 N2 C6 -91.09(16) . . . . ?
Cl1 Si1 N2 C6 85.31(16) . . . . ?
C5 N1 C1 C2 -0.2(3) . . . . ?
Si1 N1 C1 C2 -177.51(18) . . . . ?
N1 C1 C2 C3 2.3(4) . . . . ?
C1 C2 C3 C4 -2.3(4) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
C1 N1 C5 C4 -2.1(3) . . . . ?
Si1 N1 C5 C4 175.35(18) . . . . ?
C1 N1 C5 C6 177.1(2) . . . . ?
Si1 N1 C5 C6 -5.5(2) . . . . ?
C3 C4 C5 N1 2.1(3) . . . . ?
C3 C4 C5 C6 -177.0(2) . . . . ?
C10 N2 C6 C7 0.2(3) . . . . ?
Si1 N2 C6 C7 178.56(18) . . . . ?
C10 N2 C6 C5 -178.5(2) . . . . ?
Si1 N2 C6 C5 -0.1(2) . . . . ?
N1 C5 C6 N2 3.5(3) . . . . ?
C4 C5 C6 N2 -177.3(2) . . . . ?
N1 C5 C6 C7 -175.1(2) . . . . ?
C4 C5 C6 C7 4.0(4) . . . . ?
N2 C6 C7 C8 -0.2(4) . . . . ?
C5 C6 C7 C8 178.3(2) . . . . ?
C6 C7 C8 C9 0.5(4) . . . . ?
C7 C8 C9 C10 -0.8(4) . . . . ?
C6 N2 C10 C9 -0.4(4) . . . . ?
Si1 N2 C10 C9 -178.65(19) . . . . ?
C8 C9 C10 N2 0.8(4) . . . . ?
