#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/51/4315128.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_4315128
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         'C18 H13 Cl3 N2 Si'
_chemical_formula_sum            'C18 H13 Cl3 N2 Si'
_chemical_formula_weight         391.74
_chemical_name_systematic
; 
 phenyltrichlorosilane 1,10-phenanthroline complex 
;
_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'
_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                 104.071(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8765(4)
_cell_length_b                   13.2802(5)
_cell_length_c                   14.3927(6)
_cell_measurement_reflns_used    5086
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.46
_cell_volume                     1645.73(12)
_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 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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17380
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.8109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0315
_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)+(0.0431P)²+0.7283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                2891
_reflns_number_total             3582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901620e_si_002_6.cif
_cod_data_source_block           compound_3g
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4315128
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_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 0.34977(5) 0.15514(4) 0.13465(3) 0.01837(12) Uani 1 1 d . . .
Cl2 Cl 0.58325(5) 0.33747(3) 0.19558(4) 0.01889(12) Uani 1 1 d . . .
Cl3 Cl 0.71757(5) 0.22328(3) 0.39464(3) 0.01696(12) Uani 1 1 d . . .
Si1 Si 0.55422(6) 0.18912(4) 0.25516(4) 0.01388(13) Uani 1 1 d . . .
N1 N 0.50168(17) 0.06329(12) 0.31746(11) 0.0147(3) Uani 1 1 d . . .
N2 N 0.39123(18) 0.24391(12) 0.31849(11) 0.0149(3) Uani 1 1 d . . .
C1 C 0.5703(2) -0.02616(14) 0.32066(14) 0.0171(4) Uani 1 1 d . . .
H1 H 0.6570 -0.0333 0.2933 0.020 Uiso 1 1 calc R . .
C2 C 0.5185(2) -0.11027(15) 0.36324(14) 0.0204(4) Uani 1 1 d . . .
H2 H 0.5699 -0.1732 0.3643 0.025 Uiso 1 1 calc R . .
C3 C 0.3929(2) -0.10172(15) 0.40360(14) 0.0208(4) Uani 1 1 d . . .
H3 H 0.3547 -0.1589 0.4303 0.025 Uiso 1 1 calc R . .
C4 C 0.3219(2) -0.00656(15) 0.40457(14) 0.0181(4) Uani 1 1 d . . .
C5 C 0.1976(2) 0.01530(16) 0.44959(15) 0.0227(5) Uani 1 1 d . . .
H5 H 0.1527 -0.0379 0.4779 0.027 Uiso 1 1 calc R . .
C6 C 0.1433(2) 0.11038(16) 0.45242(15) 0.0226(5) Uani 1 1 d . . .
H6 H 0.0619 0.1225 0.4834 0.027 Uiso 1 1 calc R . .
C7 C 0.2056(2) 0.19286(16) 0.40992(14) 0.0198(4) Uani 1 1 d . . .
C8 C 0.1587(2) 0.29431(16) 0.41180(15) 0.0220(4) Uani 1 1 d . . .
H8 H 0.0801 0.3126 0.4431 0.026 Uiso 1 1 calc R . .
C9 C 0.2284(2) 0.36615(16) 0.36774(15) 0.0221(4) Uani 1 1 d . . .
H9 H 0.1983 0.4347 0.3689 0.027 Uiso 1 1 calc R . .
C10 C 0.3439(2) 0.33890(15) 0.32087(15) 0.0191(4) Uani 1 1 d . . .
H10 H 0.3896 0.3896 0.2900 0.023 Uiso 1 1 calc R . .
C11 C 0.3237(2) 0.17262(14) 0.36264(14) 0.0157(4) Uani 1 1 d . . .
C12 C 0.3822(2) 0.07304(14) 0.36105(13) 0.0147(4) Uani 1 1 d . . .
C13 C 0.7026(2) 0.12490(14) 0.19771(14) 0.0159(4) Uani 1 1 d . . .
C14 C 0.6666(2) 0.04829(15) 0.12896(15) 0.0210(4) Uani 1 1 d . . .
H14 H 0.5633 0.0233 0.1111 0.025 Uiso 1 1 calc R . .
C15 C 0.7772(3) 0.00756(16) 0.08598(15) 0.0252(5) Uani 1 1 d . . .
H15 H 0.7498 -0.0457 0.0409 0.030 Uiso 1 1 calc R . .
C16 C 0.9280(3) 0.04503(17) 0.10922(16) 0.0268(5) Uani 1 1 d . . .
H16 H 1.0032 0.0191 0.0785 0.032 Uiso 1 1 calc R . .
C17 C 0.9680(2) 0.11993(17) 0.17693(16) 0.0252(5) Uani 1 1 d . . .
H17 H 1.0711 0.1454 0.1933 0.030 Uiso 1 1 calc R . .
C18 C 0.8575(2) 0.15832(15) 0.22142(15) 0.0202(4) Uani 1 1 d . . .
H18 H 0.8876 0.2086 0.2693 0.024 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
C13 Si1 N1 94.64(7) . . ?
C13 Si1 N2 174.66(8) . . ?
N1 Si1 N2 80.13(6) . . ?
C13 Si1 Cl2 94.18(6) . . ?
N1 Si1 Cl2 171.15(5) . . ?
N2 Si1 Cl2 91.03(5) . . ?
C13 Si1 Cl3 96.60(6) . . ?
N1 Si1 Cl3 86.42(5) . . ?
N2 Si1 Cl3 84.29(5) . . ?
Cl2 Si1 Cl3 93.28(3) . . ?
C13 Si1 Cl1 95.10(6) . . ?
N1 Si1 Cl1 86.87(5) . . ?
N2 Si1 Cl1 83.53(5) . . ?
Cl2 Si1 Cl1 91.63(3) . . ?
Cl3 Si1 Cl1 166.94(3) . . ?
C1 N1 C12 118.02(16) . . ?
C1 N1 Si1 127.25(13) . . ?
C12 N1 Si1 114.73(12) . . ?
C10 N2 C11 118.05(16) . . ?
C10 N2 Si1 128.04(13) . . ?
C11 N2 Si1 113.92(12) . . ?
N1 C1 C2 121.95(18) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 120.12(18) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 118.99(18) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C12 C4 C3 116.83(18) . . ?
C12 C4 C5 117.88(18) . . ?
C3 C4 C5 125.25(18) . . ?
C6 C5 C4 121.25(18) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 121.53(18) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C11 C7 C8 116.69(18) . . ?
C11 C7 C6 118.15(19) . . ?
C8 C7 C6 125.15(18) . . ?
C9 C8 C7 119.07(18) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 120.40(19) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
N2 C10 C9 121.83(19) . . ?
N2 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
N2 C11 C7 123.95(18) . . ?
N2 C11 C12 115.84(16) . . ?
C7 C11 C12 120.19(17) . . ?
N1 C12 C4 123.98(18) . . ?
N1 C12 C11 115.05(16) . . ?
C4 C12 C11 120.94(17) . . ?
C14 C13 C18 116.25(18) . . ?
C14 C13 Si1 124.42(15) . . ?
C18 C13 Si1 119.26(15) . . ?
C15 C14 C13 122.18(19) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C14 C15 C16 119.7(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 119.71(19) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.1(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C13 122.0(2) . . ?
C17 C18 H18 119.0 . . ?
C13 C18 H18 119.0 . . ?
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 2.2304(7) . ?
Cl2 Si1 2.1887(7) . ?
Cl3 Si1 2.2188(7) . ?
Si1 C13 1.9170(19) . ?
Si1 N1 2.0044(16) . ?
Si1 N2 2.0236(16) . ?
N1 C1 1.331(2) . ?
N1 C12 1.363(2) . ?
N2 C10 1.332(2) . ?
N2 C11 1.358(2) . ?
C1 C2 1.404(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.381(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.413(3) . ?
C3 H3 0.9500 . ?
C4 C12 1.399(3) . ?
C4 C5 1.439(3) . ?
C5 C6 1.356(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.430(3) . ?
C6 H6 0.9500 . ?
C7 C11 1.407(3) . ?
C7 C8 1.412(3) . ?
C8 C9 1.373(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.405(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.423(3) . ?
C13 C14 1.401(3) . ?
C13 C18 1.405(3) . ?
C14 C15 1.390(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(3) . ?
C17 H17 0.9500 . ?
C18 H18 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
C13 Si1 N1 C1 6.63(17) . . . . ?
N2 Si1 N1 C1 -174.52(17) . . . . ?
Cl3 Si1 N1 C1 -89.71(16) . . . . ?
Cl1 Si1 N1 C1 101.50(16) . . . . ?
C13 Si1 N1 C12 -173.62(13) . . . . ?
N2 Si1 N1 C12 5.23(13) . . . . ?
Cl3 Si1 N1 C12 90.05(12) . . . . ?
Cl1 Si1 N1 C12 -78.74(12) . . . . ?
N1 Si1 N2 C10 176.26(18) . . . . ?
Cl2 Si1 N2 C10 -4.28(17) . . . . ?
Cl3 Si1 N2 C10 88.92(16) . . . . ?
Cl1 Si1 N2 C10 -95.80(17) . . . . ?
N1 Si1 N2 C11 -4.25(13) . . . . ?
Cl2 Si1 N2 C11 175.21(13) . . . . ?
Cl3 Si1 N2 C11 -91.60(13) . . . . ?
Cl1 Si1 N2 C11 83.69(13) . . . . ?
C12 N1 C1 C2 3.0(3) . . . . ?
Si1 N1 C1 C2 -177.24(14) . . . . ?
N1 C1 C2 C3 -0.1(3) . . . . ?
C1 C2 C3 C4 -2.5(3) . . . . ?
C2 C3 C4 C12 2.0(3) . . . . ?
C2 C3 C4 C5 -175.58(19) . . . . ?
C12 C4 C5 C6 -1.9(3) . . . . ?
C3 C4 C5 C6 175.6(2) . . . . ?
C4 C5 C6 C7 0.8(3) . . . . ?
C5 C6 C7 C11 1.4(3) . . . . ?
C5 C6 C7 C8 -178.3(2) . . . . ?
C11 C7 C8 C9 0.5(3) . . . . ?
C6 C7 C8 C9 -179.8(2) . . . . ?
C7 C8 C9 C10 0.4(3) . . . . ?
C11 N2 C10 C9 0.3(3) . . . . ?
Si1 N2 C10 C9 179.82(15) . . . . ?
C8 C9 C10 N2 -0.9(3) . . . . ?
C10 N2 C11 C7 0.7(3) . . . . ?
Si1 N2 C11 C7 -178.88(15) . . . . ?
C10 N2 C11 C12 -177.79(17) . . . . ?
Si1 N2 C11 C12 2.7(2) . . . . ?
C8 C7 C11 N2 -1.1(3) . . . . ?
C6 C7 C11 N2 179.22(18) . . . . ?
C8 C7 C11 C12 177.31(18) . . . . ?
C6 C7 C11 C12 -2.4(3) . . . . ?
C1 N1 C12 C4 -3.5(3) . . . . ?
Si1 N1 C12 C4 176.70(15) . . . . ?
C1 N1 C12 C11 174.42(17) . . . . ?
Si1 N1 C12 C11 -5.4(2) . . . . ?
C3 C4 C12 N1 1.0(3) . . . . ?
C5 C4 C12 N1 178.76(17) . . . . ?
C3 C4 C12 C11 -176.82(18) . . . . ?
C5 C4 C12 C11 0.9(3) . . . . ?
N2 C11 C12 N1 1.7(3) . . . . ?
C7 C11 C12 N1 -176.78(17) . . . . ?
N2 C11 C12 C4 179.75(17) . . . . ?
C7 C11 C12 C4 1.2(3) . . . . ?
N1 Si1 C13 C14 63.02(17) . . . . ?
Cl2 Si1 C13 C14 -116.27(16) . . . . ?
Cl3 Si1 C13 C14 149.94(16) . . . . ?
Cl1 Si1 C13 C14 -24.25(17) . . . . ?
N1 Si1 C13 C18 -120.05(16) . . . . ?
Cl2 Si1 C13 C18 60.67(16) . . . . ?
Cl3 Si1 C13 C18 -33.12(16) . . . . ?
Cl1 Si1 C13 C18 152.69(15) . . . . ?
C18 C13 C14 C15 -0.3(3) . . . . ?
Si1 C13 C14 C15 176.75(16) . . . . ?
C13 C14 C15 C16 -1.8(3) . . . . ?
C14 C15 C16 C17 2.1(3) . . . . ?
C15 C16 C17 C18 -0.4(3) . . . . ?
C16 C17 C18 C13 -1.7(3) . . . . ?
C14 C13 C18 C17 2.0(3) . . . . ?
Si1 C13 C18 C17 -175.15(16) . . . . ?
