#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:44:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178579 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/89/4068912.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_4068912
loop_
_publ_author_name
'Xiong, Yun'
'Yao, Shenglai'
'Driess, Matthias'
_publ_section_title
;
 Reactivity of a Zwitterionic Stable Silylene toward Halosilanes and
 Haloalkanes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1927
_journal_paper_doi               10.1021/om801157u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C30 H42 Cl2 N2 Si'
_chemical_formula_weight         529.65
_chemical_name_systematic
; 
 ? 
;
_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
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.04(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.220(4)
_cell_length_b                   11.608(4)
_cell_length_c                   16.663(5)
_cell_measurement_temperature    150(2)
_cell_volume                     2943.4(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0925
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14028
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0669
_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)+(0.0840P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                3449
_reflns_number_total             5114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801157u_si_001.cif
_cod_data_source_block           Compound4
_cod_original_cell_volume        2943.4(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068912
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
Cl1 Cl 0.15397(6) 0.27161(9) 0.22152(6) 0.0320(3) Uani 1 1 d .
Si1 Si 0.21751(6) 0.20434(9) 0.12343(6) 0.0202(3) Uani 1 1 d .
N1 N 0.23753(17) 0.0601(2) 0.13599(17) 0.0189(7) Uani 1 1 d .
C1 C 0.3348(3) -0.0918(4) 0.1866(2) 0.0345(10) Uani 1 1 d .
H1A H 0.2894 -0.1472 0.1795 0.041 Uiso 1 1 calc R
H1B H 0.3907 -0.1147 0.2072 0.041 Uiso 1 1 calc R
Cl2 Cl 0.09179(9) 0.36887(11) 0.03563(8) 0.0619(4) Uani 1 1 d .
N2 N 0.31789(18) 0.2681(3) 0.11385(17) 0.0202(7) Uani 1 1 d .
C2 C 0.3198(2) 0.0210(3) 0.1670(2) 0.0246(9) Uani 1 1 d .
C3 C 0.3887(2) 0.1054(3) 0.1779(2) 0.0246(9) Uani 1 1 d .
H3 H 0.4392 0.0793 0.2069 0.030 Uiso 1 1 calc R
C4 C 0.3920(2) 0.2164(3) 0.1529(2) 0.0224(9) Uani 1 1 d .
C5 C 0.4690(2) 0.2893(4) 0.1678(3) 0.0373(11) Uani 1 1 d .
H5A H 0.5180 0.2418 0.1877 0.056 Uiso 1 1 calc R
H5B H 0.4550 0.3480 0.2080 0.056 Uiso 1 1 calc R
H5C H 0.4857 0.3271 0.1178 0.056 Uiso 1 1 calc R
C6 C 0.1696(2) -0.0269(3) 0.1240(2) 0.0228(9) Uani 1 1 d .
C7 C 0.1568(2) -0.0750(3) 0.0463(2) 0.0294(10) Uani 1 1 d .
C8 C 0.0954(3) -0.1622(4) 0.0372(3) 0.0387(11) Uani 1 1 d .
H8 H 0.0862 -0.1959 -0.0143 0.046 Uiso 1 1 calc R
C9 C 0.0474(3) -0.2011(4) 0.1006(3) 0.0432(12) Uani 1 1 d .
H9 H 0.0051 -0.2603 0.0925 0.052 Uiso 1 1 calc R
C10 C 0.0603(3) -0.1551(4) 0.1753(3) 0.0346(10) Uani 1 1 d .
H10 H 0.0269 -0.1833 0.2187 0.041 Uiso 1 1 calc R
C11 C 0.1217(2) -0.0671(3) 0.1893(2) 0.0257(9) Uani 1 1 d .
C12 C 0.1327(3) -0.0224(4) 0.2745(2) 0.0325(10) Uani 1 1 d .
H12 H 0.1801 0.0372 0.2752 0.039 Uiso 1 1 calc R
C13 C 0.0486(3) 0.0333(4) 0.3034(3) 0.0543(14) Uani 1 1 d .
H13A H 0.0282 0.0905 0.2640 0.081 Uiso 1 1 calc R
H13B H 0.0599 0.0713 0.3551 0.081 Uiso 1 1 calc R
H13C H 0.0033 -0.0259 0.3097 0.081 Uiso 1 1 calc R
C14 C 0.1599(3) -0.1199(4) 0.3328(3) 0.0493(13) Uani 1 1 d .
H14A H 0.1138 -0.1788 0.3333 0.074 Uiso 1 1 calc R
H14B H 0.1682 -0.0883 0.3870 0.074 Uiso 1 1 calc R
H14C H 0.2150 -0.1546 0.3151 0.074 Uiso 1 1 calc R
C15 C 0.2102(3) -0.0375(4) -0.0247(2) 0.0325(10) Uani 1 1 d .
H15 H 0.2374 0.0387 -0.0113 0.039 Uiso 1 1 calc R
C16 C 0.1534(3) -0.0223(4) -0.1014(3) 0.0476(12) Uani 1 1 d .
H16A H 0.1307 -0.0974 -0.1189 0.071 Uiso 1 1 calc R
H16B H 0.1893 0.0108 -0.1439 0.071 Uiso 1 1 calc R
H16C H 0.1042 0.0294 -0.0903 0.071 Uiso 1 1 calc R
C17 C 0.2844(3) -0.1231(4) -0.0395(3) 0.0494(13) Uani 1 1 d .
H17A H 0.3224 -0.1280 0.0085 0.074 Uiso 1 1 calc R
H17B H 0.3190 -0.0971 -0.0851 0.074 Uiso 1 1 calc R
H17C H 0.2594 -0.1992 -0.0514 0.074 Uiso 1 1 calc R
C18 C 0.3333(2) 0.3636(3) 0.0588(2) 0.0239(9) Uani 1 1 d .
C19 C 0.3207(2) 0.4772(3) 0.0843(2) 0.0256(9) Uani 1 1 d .
C20 C 0.3345(3) 0.5651(4) 0.0293(3) 0.0362(11) Uani 1 1 d .
H20 H 0.3262 0.6429 0.0454 0.043 Uiso 1 1 calc R
C21 C 0.3597(3) 0.5418(4) -0.0478(3) 0.0416(12) Uani 1 1 d .
H21 H 0.3683 0.6033 -0.0844 0.050 Uiso 1 1 calc R
C22 C 0.3727(3) 0.4294(4) -0.0724(3) 0.0399(11) Uani 1 1 d .
H22 H 0.3899 0.4142 -0.1259 0.048 Uiso 1 1 calc R
C23 C 0.3606(2) 0.3382(4) -0.0192(2) 0.0289(10) Uani 1 1 d .
C24 C 0.3790(3) 0.2151(4) -0.0466(2) 0.0368(11) Uani 1 1 d .
H24 H 0.3532 0.1612 -0.0065 0.044 Uiso 1 1 calc R
C25 C 0.3363(4) 0.1900(5) -0.1282(3) 0.0585(14) Uani 1 1 d .
H25A H 0.2737 0.2095 -0.1269 0.088 Uiso 1 1 calc R
H25B H 0.3429 0.1080 -0.1409 0.088 Uiso 1 1 calc R
H25C H 0.3649 0.2363 -0.1694 0.088 Uiso 1 1 calc R
C26 C 0.4779(3) 0.1930(5) -0.0490(3) 0.0615(15) Uani 1 1 d .
H26A H 0.5050 0.2479 -0.0857 0.092 Uiso 1 1 calc R
H26B H 0.4885 0.1143 -0.0678 0.092 Uiso 1 1 calc R
H26C H 0.5035 0.2026 0.0050 0.092 Uiso 1 1 calc R
C27 C 0.2962(2) 0.5112(3) 0.1685(2) 0.0317(10) Uani 1 1 d .
H27 H 0.2886 0.4392 0.2005 0.038 Uiso 1 1 calc R
C28 C 0.2102(3) 0.5790(4) 0.1707(3) 0.0408(11) Uani 1 1 d .
H28A H 0.2153 0.6485 0.1377 0.061 Uiso 1 1 calc R
H28B H 0.1980 0.6010 0.2262 0.061 Uiso 1 1 calc R
H28C H 0.1621 0.5310 0.1496 0.061 Uiso 1 1 calc R
C29 C 0.3704(3) 0.5824(4) 0.2083(3) 0.0427(12) Uani 1 1 d .
H29A H 0.4263 0.5414 0.2032 0.064 Uiso 1 1 calc R
H29B H 0.3578 0.5937 0.2652 0.064 Uiso 1 1 calc R
H29C H 0.3743 0.6575 0.1818 0.064 Uiso 1 1 calc R
C30 C 0.1417(2) 0.2323(3) 0.0340(2) 0.0185(8) Uani 1 1 d .
H30A H 0.1758 0.2249 -0.0157 0.022 Uiso 1 1 calc R
H30B H 0.0952 0.1726 0.0326 0.022 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
N2 Si1 N1 106.08(14)
N2 Si1 C30 112.65(15)
N1 Si1 C30 111.61(15)
N2 Si1 Cl1 110.05(11)
N1 Si1 Cl1 110.90(12)
C30 Si1 Cl1 105.63(12)
C2 N1 C6 116.6(3)
C2 N1 Si1 120.7(2)
C6 N1 Si1 122.4(2)
C4 N2 C18 118.2(3)
C4 N2 Si1 118.5(2)
C18 N2 Si1 122.8(2)
C1 C2 N1 122.4(3)
C1 C2 C3 120.1(3)
N1 C2 C3 117.5(3)
C4 C3 C2 129.6(3)
C3 C4 N2 120.5(3)
C3 C4 C5 122.1(3)
N2 C4 C5 117.3(3)
C11 C6 C7 120.8(3)
C11 C6 N1 120.2(3)
C7 C6 N1 118.9(3)
C8 C7 C6 118.0(4)
C8 C7 C15 119.7(4)
C6 C7 C15 122.2(3)
C9 C8 C7 121.5(4)
C10 C9 C8 120.3(4)
C9 C10 C11 121.4(4)
C10 C11 C6 117.9(4)
C10 C11 C12 117.8(3)
C6 C11 C12 124.3(3)
C11 C12 C13 111.3(4)
C11 C12 C14 111.2(3)
C13 C12 C14 109.3(4)
C7 C15 C17 110.4(3)
C7 C15 C16 112.4(3)
C17 C15 C16 110.3(3)
C19 C18 C23 121.5(4)
C19 C18 N2 120.1(3)
C23 C18 N2 118.4(3)
C20 C19 C18 118.0(4)
C20 C19 C27 117.6(4)
C18 C19 C27 124.4(3)
C21 C20 C19 121.3(4)
C20 C21 C22 120.4(4)
C21 C22 C23 120.4(4)
C22 C23 C18 118.3(4)
C22 C23 C24 119.6(4)
C18 C23 C24 122.1(4)
C25 C24 C23 111.5(4)
C25 C24 C26 110.4(4)
C23 C24 C26 110.5(4)
C19 C27 C28 112.5(3)
C19 C27 C29 110.4(3)
C28 C27 C29 109.6(3)
Cl2 C30 Si1 113.59(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl1 Si1 2.0670(15)
Si1 N2 1.707(3)
Si1 N1 1.714(3)
Si1 C30 1.896(3)
N1 C2 1.421(4)
N1 C6 1.456(4)
C1 C2 1.368(5)
Cl2 C30 1.759(3)
N2 C4 1.425(4)
N2 C18 1.461(4)
C2 C3 1.444(5)
C3 C4 1.355(5)
C4 C5 1.464(5)
C6 C11 1.402(5)
C6 C7 1.419(5)
C7 C8 1.383(6)
C7 C15 1.513(5)
C8 C9 1.373(6)
C9 C10 1.365(6)
C10 C11 1.401(5)
C11 C12 1.517(5)
C12 C13 1.520(6)
C12 C14 1.545(6)
C15 C17 1.528(6)
C15 C16 1.540(5)
C18 C19 1.399(5)
C18 C23 1.405(5)
C19 C20 1.391(5)
C19 C27 1.510(6)
C20 C21 1.375(6)
C21 C22 1.383(6)
C22 C23 1.396(6)
C23 C24 1.527(6)
C24 C25 1.525(6)
C24 C26 1.528(6)
C27 C28 1.529(6)
C27 C29 1.539(5)
