#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/24/4072490.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_4072490
loop_
_publ_author_name
'Wagler, Jörg'
_publ_contact_author
;Wagler, Jörg 
 Institut für Anorganische Chemie  
 Technische Universität Bergakademie Freiberg
 Leipziger Str. 29 
 09596 Freiberg 
 Bundesrepublik Deutschland
;
_publ_section_title
;
 A Disilane with a Hypercoordinate Silicon Atom:  Coordination of
 an Imine Ligand versus Si−Si Bond Splitting
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              155
_journal_paper_doi               10.1021/om060698a
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C21 H18 Cl N O3 Si, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C23 H22 Cl N O4 Si'
_chemical_formula_weight         439.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                116.999(2)
_cell_angle_beta                 92.598(3)
_cell_angle_gamma                97.476(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1667(12)
_cell_length_b                   10.6090(12)
_cell_length_c                   11.4683(10)
_cell_measurement_reflns_used    5598
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.72
_cell_volume                     1085.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            15067
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9694
_exptl_absorpt_correction_T_min  0.8286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0381
_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)+(0.0543P)²+0.1774P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                3794
_reflns_number_total             4896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060698asi20060802_101330.cif
_cod_data_source_block           compound_8
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072490
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Cl1 Cl 0.30221(5) 0.35222(5) 0.25962(5) 0.06198(16) Uani 1 1 d .
Si1 Si 0.39918(4) 0.18483(4) 0.26668(4) 0.03672(13) Uani 1 1 d .
O1 O 0.47569(10) 0.17053(11) 0.13595(11) 0.0387(3) Uani 1 1 d .
O2 O 0.24953(11) 0.09464(13) 0.26318(13) 0.0492(3) Uani 1 1 d .
O3 O 0.88113(12) 0.31580(14) 0.02504(14) 0.0549(3) Uani 1 1 d .
N1 N 0.46438(12) 0.00089(13) 0.24036(13) 0.0351(3) Uani 1 1 d .
C1 C 0.60587(14) 0.15546(15) 0.12637(14) 0.0336(3) Uani 1 1 d .
C2 C 0.68133(15) 0.23309(16) 0.07607(15) 0.0384(3) Uani 1 1 d .
H2 H 0.6413 0.2901 0.0479 0.046 Uiso 1 1 calc R
C3 C 0.81599(16) 0.22689(17) 0.06706(16) 0.0410(4) Uani 1 1 d .
C4 C 0.87628(16) 0.13653(18) 0.10355(18) 0.0460(4) Uani 1 1 d .
H4 H 0.9664 0.1310 0.0966 0.055 Uiso 1 1 calc R
C5 C 0.79950(16) 0.05627(17) 0.14983(17) 0.0429(4) Uani 1 1 d .
H5 H 0.8389 -0.0056 0.1719 0.052 Uiso 1 1 calc R
C6 C 0.66387(15) 0.06394(15) 0.16523(15) 0.0351(3) Uani 1 1 d .
C7 C 0.58282(15) -0.02589(15) 0.20909(15) 0.0356(3) Uani 1 1 d .
C8 C 0.64073(15) -0.14521(16) 0.21635(16) 0.0375(3) Uani 1 1 d .
C9 C 0.69414(18) -0.12824(19) 0.33695(18) 0.0488(4) Uani 1 1 d .
H9 H 0.6941 -0.0429 0.4132 0.059 Uiso 1 1 calc R
C10 C 0.74782(19) -0.2392(2) 0.3436(2) 0.0554(5) Uani 1 1 d .
H10 H 0.7841 -0.2282 0.4243 0.066 Uiso 1 1 calc R
C11 C 0.74722(19) -0.3655(2) 0.2306(2) 0.0552(5) Uani 1 1 d .
H11 H 0.7822 -0.4399 0.2354 0.066 Uiso 1 1 calc R
C12 C 0.69520(18) -0.38231(18) 0.1106(2) 0.0496(4) Uani 1 1 d .
H12 H 0.6949 -0.4681 0.0348 0.060 Uiso 1 1 calc R
C13 C 0.64303(16) -0.27137(16) 0.10226(17) 0.0416(4) Uani 1 1 d .
H13 H 0.6100 -0.2817 0.0209 0.050 Uiso 1 1 calc R
C14 C 0.36233(16) -0.08395(17) 0.26790(16) 0.0388(3) Uani 1 1 d .
C15 C 0.36072(18) -0.20980(19) 0.27911(19) 0.0499(4) Uani 1 1 d .
H15 H 0.4373 -0.2511 0.2709 0.060 Uiso 1 1 calc R
C16 C 0.2432(2) -0.2725(2) 0.3027(2) 0.0600(5) Uani 1 1 d .
H16 H 0.2415 -0.3565 0.3100 0.072 Uiso 1 1 calc R
C17 C 0.1293(2) -0.2122(2) 0.3155(2) 0.0619(5) Uani 1 1 d .
H17 H 0.0519 -0.2557 0.3320 0.074 Uiso 1 1 calc R
C18 C 0.12842(18) -0.0882(2) 0.3042(2) 0.0559(5) Uani 1 1 d .
H18 H 0.0514 -0.0475 0.3131 0.067 Uiso 1 1 calc R
C19 C 0.24534(16) -0.02548(18) 0.27937(17) 0.0433(4) Uani 1 1 d .
C20 C 1.0227(2) 0.3282(3) 0.0279(3) 0.0783(7) Uani 1 1 d .
H20A H 1.0625 0.3619 0.1167 0.117 Uiso 1 1 d R
H20B H 1.0555 0.3949 -0.0034 0.117 Uiso 1 1 d R
H20C H 1.0454 0.2360 -0.0276 0.117 Uiso 1 1 d R
C21 C 0.5002(2) 0.28993(19) 0.42958(18) 0.0548(5) Uani 1 1 d .
H21A H 0.5436 0.2270 0.4514 0.082 Uiso 1 1 d R
H21B H 0.4431 0.3359 0.4952 0.082 Uiso 1 1 d R
H21C H 0.5664 0.3614 0.4266 0.082 Uiso 1 1 d R
C22 C 0.8766(2) 0.4460(3) 0.4288(2) 0.0690(6) Uani 1 1 d .
H22A H 0.8198 0.3905 0.3457 0.083 Uiso 1 1 calc R
H22B H 0.8197 0.4775 0.4989 0.083 Uiso 1 1 calc R
C23 C 1.0344(3) 0.6462(2) 0.5514(2) 0.0768(7) Uani 1 1 d .
H23A H 0.9787 0.6797 0.6224 0.092 Uiso 1 1 calc R
H23B H 1.0882 0.7294 0.5525 0.092 Uiso 1 1 calc R
O4 O 0.95251(18) 0.56571(18) 0.42850(16) 0.0810(5) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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
O1 Si1 O2 126.41(6) . .
O1 Si1 C21 116.27(8) . .
O2 Si1 C21 116.68(8) . .
O1 Si1 N1 86.96(5) . .
O2 Si1 N1 83.61(5) . .
C21 Si1 N1 91.95(7) . .
O1 Si1 Cl1 89.61(4) . .
O2 Si1 Cl1 89.65(4) . .
C21 Si1 Cl1 99.40(6) . .
N1 Si1 Cl1 168.51(5) . .
C1 O1 Si1 123.00(9) . .
C19 O2 Si1 118.43(10) . .
C3 O3 C20 118.34(15) . .
C7 N1 C14 128.07(13) . .
C7 N1 Si1 123.40(10) . .
C14 N1 Si1 108.46(9) . .
O1 C1 C2 117.28(12) . .
O1 C1 C6 122.27(13) . .
C2 C1 C6 120.46(13) . .
C1 C2 C3 120.69(14) . .
C1 C2 H2 119.7 . .
C3 C2 H2 119.7 . .
O3 C3 C2 115.03(14) . .
O3 C3 C4 124.65(15) . .
C2 C3 C4 120.30(15) . .
C5 C4 C3 118.63(15) . .
C5 C4 H4 120.7 . .
C3 C4 H4 120.7 . .
C4 C5 C6 122.69(14) . .
C4 C5 H5 118.7 . .
C6 C5 H5 118.7 . .
C5 C6 C1 117.16(14) . .
C5 C6 C7 121.97(13) . .
C1 C6 C7 120.70(13) . .
N1 C7 C6 118.92(12) . .
N1 C7 C8 123.24(13) . .
C6 C7 C8 117.83(13) . .
C9 C8 C13 120.16(14) . .
C9 C8 C7 119.82(14) . .
C13 C8 C7 120.01(14) . .
C8 C9 C10 119.77(17) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C11 C10 C9 119.90(17) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C12 C11 C10 120.48(15) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C13 120.20(17) . .
C11 C12 H12 119.9 . .
C13 C12 H12 119.9 . .
C8 C13 C12 119.44(16) . .
C8 C13 H13 120.3 . .
C12 C13 H13 120.3 . .
C19 C14 C15 119.05(15) . .
C19 C14 N1 109.06(13) . .
C15 C14 N1 131.83(15) . .
C16 C15 C14 119.11(17) . .
C16 C15 H15 120.4 . .
C14 C15 H15 120.4 . .
C17 C16 C15 121.03(17) . .
C17 C16 H16 119.5 . .
C15 C16 H16 119.5 . .
C16 C17 C18 120.84(18) . .
C16 C17 H17 119.6 . .
C18 C17 H17 119.6 . .
C17 C18 C19 118.47(18) . .
C17 C18 H18 120.8 . .
C19 C18 H18 120.8 . .
O2 C19 C18 121.17(15) . .
O2 C19 C14 117.35(14) . .
C18 C19 C14 121.48(16) . .
O3 C20 H20A 109.5 . .
O3 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
O3 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
Si1 C21 H21A 109.5 . .
Si1 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
Si1 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
O4 C22 C23 110.61(18) . 2_766
O4 C22 H22A 109.5 . .
C23 C22 H22A 109.5 2_766 .
O4 C22 H22B 109.5 . .
C23 C22 H22B 109.5 2_766 .
H22A C22 H22B 108.1 . .
O4 C23 C22 109.59(19) . 2_766
O4 C23 H23A 109.8 . .
C22 C23 H23A 109.8 2_766 .
O4 C23 H23B 109.8 . .
C22 C23 H23B 109.8 2_766 .
H23A C23 H23B 108.2 . .
C22 O4 C23 108.72(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 Si1 2.1705(6) .
Si1 O1 1.6750(12) .
Si1 O2 1.6771(12) .
Si1 C21 1.8508(18) .
Si1 N1 2.0392(12) .
O1 C1 1.3571(17) .
O2 C19 1.364(2) .
O3 C3 1.356(2) .
O3 C20 1.426(2) .
N1 C7 1.3019(19) .
N1 C14 1.4251(19) .
C1 C2 1.381(2) .
C1 C6 1.4167(19) .
C2 C3 1.385(2) .
C2 H2 0.9300 .
C3 C4 1.401(2) .
C4 C5 1.375(2) .
C4 H4 0.9300 .
C5 C6 1.406(2) .
C5 H5 0.9300 .
C6 C7 1.452(2) .
C7 C8 1.4971(19) .
C8 C9 1.386(2) .
C8 C13 1.387(2) .
C9 C10 1.391(2) .
C9 H9 0.9300 .
C10 C11 1.376(3) .
C10 H10 0.9300 .
C11 C12 1.376(3) .
C11 H11 0.9300 .
C12 C13 1.391(2) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C19 1.396(2) .
C14 C15 1.396(2) .
C15 C16 1.389(3) .
C15 H15 0.9300 .
C16 C17 1.377(3) .
C16 H16 0.9300 .
C17 C18 1.381(3) .
C17 H17 0.9300 .
C18 C19 1.391(2) .
C18 H18 0.9300 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 O4 1.399(3) .
C22 C23 1.497(3) 2_766
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 O4 1.423(3) .
C23 C22 1.497(3) 2_766
C23 H23A 0.9700 .
C23 H23B 0.9700 .
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
O2 Si1 O1 C1 -132.77(11) .
C21 Si1 O1 C1 37.66(13) .
N1 Si1 O1 C1 -53.01(11) .
Cl1 Si1 O1 C1 137.96(11) .
O1 Si1 O2 C19 97.40(13) .
C21 Si1 O2 C19 -73.00(15) .
N1 Si1 O2 C19 15.97(13) .
Cl1 Si1 O2 C19 -173.35(13) .
O1 Si1 N1 C7 40.49(12) .
O2 Si1 N1 C7 167.65(13) .
C21 Si1 N1 C7 -75.72(14) .
Cl1 Si1 N1 C7 113.3(2) .
O1 Si1 N1 C14 -142.17(11) .
O2 Si1 N1 C14 -15.01(10) .
C21 Si1 N1 C14 101.62(12) .
Cl1 Si1 N1 C14 -69.4(3) .
Si1 O1 C1 C2 -138.16(12) .
Si1 O1 C1 C6 42.13(18) .
O1 C1 C2 C3 177.97(13) .
C6 C1 C2 C3 -2.3(2) .
C20 O3 C3 C2 172.74(17) .
C20 O3 C3 C4 -5.4(3) .
C1 C2 C3 O3 -175.42(14) .
C1 C2 C3 C4 2.8(2) .
O3 C3 C4 C5 177.23(16) .
C2 C3 C4 C5 -0.9(3) .
C3 C4 C5 C6 -1.7(3) .
C4 C5 C6 C1 2.2(2) .
C4 C5 C6 C7 177.42(16) .
O1 C1 C6 C5 179.55(14) .
C2 C1 C6 C5 -0.2(2) .
O1 C1 C6 C7 4.2(2) .
C2 C1 C6 C7 -175.46(14) .
C14 N1 C7 C6 170.60(14) .
Si1 N1 C7 C6 -12.6(2) .
C14 N1 C7 C8 -9.6(2) .
Si1 N1 C7 C8 167.20(11) .
C5 C6 C7 N1 169.78(14) .
C1 C6 C7 N1 -15.1(2) .
C5 C6 C7 C8 -10.0(2) .
C1 C6 C7 C8 165.03(14) .
N1 C7 C8 C9 -78.9(2) .
C6 C7 C8 C9 100.92(18) .
N1 C7 C8 C13 102.27(19) .
C6 C7 C8 C13 -77.92(19) .
C13 C8 C9 C10 -1.2(3) .
C7 C8 C9 C10 179.94(16) .
C8 C9 C10 C11 -0.2(3) .
C9 C10 C11 C12 0.7(3) .
C10 C11 C12 C13 0.2(3) .
C9 C8 C13 C12 2.2(2) .
C7 C8 C13 C12 -178.99(15) .
C11 C12 C13 C8 -1.7(3) .
C7 N1 C14 C19 -172.04(15) .
Si1 N1 C14 C19 10.78(16) .
C7 N1 C14 C15 5.3(3) .
Si1 N1 C14 C15 -171.89(17) .
C19 C14 C15 C16 -0.7(3) .
N1 C14 C15 C16 -177.78(17) .
C14 C15 C16 C17 -0.2(3) .
C15 C16 C17 C18 0.5(3) .
C16 C17 C18 C19 0.1(3) .
Si1 O2 C19 C18 166.78(14) .
Si1 O2 C19 C14 -14.2(2) .
C17 C18 C19 O2 177.95(17) .
C17 C18 C19 C14 -1.0(3) .
C15 C14 C19 O2 -177.72(16) .
N1 C14 C19 O2 0.0(2) .
C15 C14 C19 C18 1.3(3) .
N1 C14 C19 C18 179.02(16) .
C23 C22 O4 C23 -59.6(3) 2_766
C22 C23 O4 C22 59.0(3) 2_766
