#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:44:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178579 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/89/4068913.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_4068913
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 Cl I N2 Si'
_chemical_formula_weight         621.10
_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
;
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                66.973(3)
_cell_angle_beta                 74.202(3)
_cell_angle_gamma                65.382(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8539(4)
_cell_length_b                   12.5672(4)
_cell_length_c                   13.3929(5)
_cell_measurement_reflns_used    7937
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6062
_cell_measurement_theta_min      3.2248
_cell_volume                     1515.36(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12647
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.056
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0614P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                4261
_reflns_number_total             5310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801157u_si_001.cif
_cod_data_source_block           Compound5
_cod_original_cell_volume        1515.36(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068913
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
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.24957(2) 0.147502(18) 0.951804(16) 0.03006(9) Uani 0.9528(8) 1 d P A .
Cl1 Cl -0.06852(8) 0.43571(7) 0.66994(8) 0.0417(2) Uani 1 1 d . . .
Si1 Si 0.19069(8) 0.29863(7) 0.77367(6) 0.02192(19) Uani 1 1 d . . .
N1 N 0.2521(2) 0.4169(2) 0.73555(18) 0.0225(5) Uani 1 1 d . A .
C1 C 0.3358(3) 0.5683(3) 0.5875(3) 0.0362(8) Uani 1 1 d . A .
H1A H 0.3337 0.6059 0.6375 0.043 Uiso 1 1 calc R . .
H1B H 0.3653 0.6006 0.5119 0.043 Uiso 1 1 calc R . .
N2 N 0.2619(2) 0.2278(2) 0.67498(18) 0.0223(5) Uani 1 1 d . A .
C2 C 0.2973(3) 0.4699(3) 0.6236(2) 0.0253(7) Uani 1 1 d . . .
C3 C 0.2992(3) 0.4136(3) 0.5462(2) 0.0256(7) Uani 1 1 d . A .
H3 H 0.3113 0.4601 0.4711 0.031 Uiso 1 1 calc R . .
C4 C 0.2862(3) 0.3048(3) 0.5665(2) 0.0229(6) Uani 1 1 d . . .
C5 C 0.2895(4) 0.2613(3) 0.4764(2) 0.0347(8) Uani 1 1 d . A .
H5A H 0.1991 0.2604 0.4782 0.052 Uiso 1 1 calc R . .
H5B H 0.3572 0.1778 0.4860 0.052 Uiso 1 1 calc R . .
H5C H 0.3144 0.3172 0.4058 0.052 Uiso 1 1 calc R . .
C6 C 0.2469(3) 0.4777(2) 0.8109(2) 0.0237(6) Uani 1 1 d . . .
C7 C 0.3600(3) 0.4354(3) 0.8651(2) 0.0287(7) Uani 1 1 d . A .
C8 C 0.3559(3) 0.4985(3) 0.9320(3) 0.0381(8) Uani 1 1 d . . .
H8 H 0.4316 0.4709 0.9697 0.046 Uiso 1 1 calc R A .
C9 C 0.2439(4) 0.6006(3) 0.9446(3) 0.0409(9) Uani 1 1 d . A .
H9 H 0.2433 0.6429 0.9900 0.049 Uiso 1 1 calc R . .
C10 C 0.1326(4) 0.6408(3) 0.8909(3) 0.0343(8) Uani 1 1 d . . .
H10 H 0.0553 0.7102 0.9008 0.041 Uiso 1 1 calc R A .
C11 C 0.1320(3) 0.5813(3) 0.8223(2) 0.0277(7) Uani 1 1 d . A .
C12 C 0.0097(3) 0.6346(3) 0.7614(3) 0.0311(7) Uani 1 1 d . . .
H12 H 0.0237 0.5799 0.7186 0.037 Uiso 1 1 calc R A .
C13 C -0.1236(3) 0.6396(3) 0.8401(3) 0.0410(9) Uani 1 1 d . A .
H13A H -0.1090 0.5618 0.9007 0.062 Uiso 1 1 calc R . .
H13B H -0.1952 0.6521 0.8008 0.062 Uiso 1 1 calc R . .
H13C H -0.1517 0.7081 0.8689 0.062 Uiso 1 1 calc R . .
C14 C -0.0032(4) 0.7643(3) 0.6806(3) 0.0470(9) Uani 1 1 d . A .
H14A H -0.0175 0.8197 0.7210 0.071 Uiso 1 1 calc R . .
H14B H -0.0811 0.7955 0.6407 0.071 Uiso 1 1 calc R . .
H14C H 0.0807 0.7604 0.6287 0.071 Uiso 1 1 calc R . .
C15 C 0.4908(3) 0.3286(3) 0.8493(3) 0.0342(8) Uani 1 1 d . . .
H15 H 0.4695 0.2812 0.8153 0.041 Uiso 1 1 calc R A .
C16 C 0.6014(4) 0.3788(4) 0.7697(3) 0.0542(10) Uani 1 1 d . A .
H16A H 0.5662 0.4338 0.7002 0.081 Uiso 1 1 calc R . .
H16B H 0.6829 0.3098 0.7568 0.081 Uiso 1 1 calc R . .
H16C H 0.6251 0.4247 0.8017 0.081 Uiso 1 1 calc R . .
C17 C 0.5460(4) 0.2396(3) 0.9567(3) 0.0485(9) Uani 1 1 d . A .
H17A H 0.5696 0.2835 0.9909 0.073 Uiso 1 1 calc R . .
H17B H 0.6278 0.1716 0.9420 0.073 Uiso 1 1 calc R . .
H17C H 0.4761 0.2065 1.0060 0.073 Uiso 1 1 calc R . .
C18 C 0.3168(3) 0.0946(2) 0.6966(2) 0.0247(7) Uani 1 1 d . . .
C19 C 0.2279(3) 0.0308(3) 0.7176(2) 0.0295(7) Uani 1 1 d . A .
C20 C 0.2848(4) -0.0972(3) 0.7397(3) 0.0386(8) Uani 1 1 d . . .
H20 H 0.2265 -0.1425 0.7555 0.046 Uiso 1 1 calc R A .
C21 C 0.4221(4) -0.1583(3) 0.7391(3) 0.0433(9) Uani 1 1 d . A .
H21 H 0.4586 -0.2451 0.7532 0.052 Uiso 1 1 calc R . .
C22 C 0.5085(4) -0.0942(3) 0.7181(3) 0.0370(8) Uani 1 1 d . . .
H22 H 0.6040 -0.1379 0.7183 0.044 Uiso 1 1 calc R A .
C23 C 0.4581(3) 0.0330(3) 0.6967(2) 0.0285(7) Uani 1 1 d . A .
C24 C 0.5574(3) 0.0994(3) 0.6742(3) 0.0335(7) Uani 1 1 d . . .
H24 H 0.5023 0.1875 0.6694 0.040 Uiso 1 1 calc R A .
C25 C 0.6481(4) 0.0982(3) 0.5650(3) 0.0463(9) Uani 1 1 d . A .
H25A H 0.6989 0.0127 0.5658 0.069 Uiso 1 1 calc R . .
H25B H 0.7125 0.1394 0.5535 0.069 Uiso 1 1 calc R . .
H25C H 0.5910 0.1418 0.5057 0.069 Uiso 1 1 calc R . .
C26 C 0.6439(3) 0.0443(3) 0.7673(3) 0.0453(9) Uani 1 1 d . A .
H26A H 0.5837 0.0462 0.8365 0.068 Uiso 1 1 calc R . .
H26B H 0.7016 0.0926 0.7532 0.068 Uiso 1 1 calc R . .
H26C H 0.7017 -0.0413 0.7721 0.068 Uiso 1 1 calc R . .
C27 C 0.0756(3) 0.0937(3) 0.7159(3) 0.0353(8) Uani 1 1 d . . .
H27 H 0.0529 0.1841 0.6996 0.042 Uiso 1 1 calc R A .
C28 C -0.0030(4) 0.0458(3) 0.8271(3) 0.0462(9) Uani 1 1 d . A .
H28A H 0.0059 -0.0391 0.8393 0.069 Uiso 1 1 calc R . .
H28B H -0.0997 0.0984 0.8281 0.069 Uiso 1 1 calc R . .
H28C H 0.0346 0.0475 0.8850 0.069 Uiso 1 1 calc R . .
C29 C 0.0297(4) 0.0754(3) 0.6201(3) 0.0559(11) Uani 1 1 d . A .
H29A H 0.0885 0.0974 0.5513 0.084 Uiso 1 1 calc R . .
H29B H -0.0656 0.1286 0.6111 0.084 Uiso 1 1 calc R . .
H29C H 0.0385 -0.0110 0.6400 0.084 Uiso 1 1 calc R . .
C30 C 0.0020(4) 0.3520(3) 0.8065(3) 0.0427(9) Uiso 1 1 d R A -1
H30A H -0.0295 0.4085 0.8504 0.064 Uiso 1 1 calc R B -1
H30B H -0.0287 0.2809 0.8488 0.064 Uiso 1 1 calc R C -1
I1A I -0.0456(6) 0.3694(5) 0.7717(5) 0.0468(19) Uiso 0.0472(8) 1 d P A -2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
I1A Cl1 C30 13.9(3)
N2 Si1 N1 106.58(11)
N2 Si1 C30 117.34(13)
N1 Si1 C30 111.90(12)
N2 Si1 I1A 104.95(16)
N1 Si1 I1A 112.73(15)
C30 Si1 I1A 13.79(16)
N2 Si1 I1 109.45(8)
N1 Si1 I1 112.88(9)
C30 Si1 I1 98.73(10)
I1A Si1 I1 109.86(14)
C2 N1 C6 116.3(2)
C2 N1 Si1 120.03(19)
C6 N1 Si1 123.34(17)
C4 N2 C18 118.2(2)
C4 N2 Si1 116.40(18)
C18 N2 Si1 124.70(18)
C1 C2 N1 122.9(3)
C1 C2 C3 119.7(3)
N1 C2 C3 117.4(2)
C4 C3 C2 128.9(3)
C3 C4 N2 121.7(3)
C3 C4 C5 121.9(3)
N2 C4 C5 116.3(2)
C7 C6 C11 121.6(3)
C7 C6 N1 119.0(2)
C11 C6 N1 119.3(3)
C8 C7 C6 118.1(3)
C8 C7 C15 118.3(3)
C6 C7 C15 123.5(3)
C9 C8 C7 121.3(3)
C10 C9 C8 119.8(3)
C9 C10 C11 121.1(3)
C10 C11 C6 118.0(3)
C10 C11 C12 118.2(3)
C6 C11 C12 123.7(3)
C11 C12 C13 111.7(3)
C11 C12 C14 111.1(3)
C13 C12 C14 109.6(3)
C7 C15 C17 113.0(3)
C7 C15 C16 110.2(3)
C17 C15 C16 109.9(3)
C23 C18 C19 121.4(3)
C23 C18 N2 118.7(3)
C19 C18 N2 119.8(3)
C20 C19 C18 117.9(3)
C20 C19 C27 118.9(3)
C18 C19 C27 123.2(3)
C21 C20 C19 121.4(3)
C20 C21 C22 120.1(3)
C21 C22 C23 121.3(3)
C22 C23 C18 117.9(3)
C22 C23 C24 119.3(3)
C18 C23 C24 122.8(3)
C25 C24 C23 111.1(3)
C25 C24 C26 110.9(3)
C23 C24 C26 111.4(3)
C19 C27 C28 111.2(3)
C19 C27 C29 110.4(3)
C28 C27 C29 110.7(3)
Si1 C30 Cl1 106.23(17)
Cl1 I1A Si1 107.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
I1 Si1 2.4457(8)
Cl1 I1A 1.318(6)
Cl1 C30 1.904(3)
Si1 N2 1.711(2)
Si1 N1 1.721(2)
Si1 C30 1.853(4)
Si1 I1A 2.343(6)
N1 C2 1.422(3)
N1 C6 1.463(3)
C1 C2 1.339(4)
N2 C4 1.422(4)
N2 C18 1.457(3)
C2 C3 1.458(4)
C3 C4 1.347(4)
C4 C5 1.494(4)
C6 C7 1.398(4)
C6 C11 1.404(4)
C7 C8 1.393(4)
C7 C15 1.527(4)
C8 C9 1.382(5)
C9 C10 1.382(5)
C10 C11 1.396(4)
C11 C12 1.516(4)
C12 C13 1.534(4)
C12 C14 1.536(4)
C15 C17 1.527(5)
C15 C16 1.543(5)
C18 C23 1.402(4)
C18 C19 1.404(4)
C19 C20 1.398(4)
C19 C27 1.509(4)
C20 C21 1.362(5)
C21 C22 1.384(5)
C22 C23 1.391(4)
C23 C24 1.526(4)
C24 C25 1.526(4)
C24 C26 1.528(5)
C27 C28 1.530(4)
C27 C29 1.619(4)
