#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:55:49 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179028 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/26/4122691.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_4122691
loop_
_publ_author_name
'Hansen, Kerstin'
'Szilvási, Tibor'
'Blom, Burgert'
'Driess, Matthias'
_publ_section_title
;
 An Amplified Ylidic "Half-Parent" Iminosilane LSi═NH.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14207
_journal_paper_doi               10.1021/ja507785z
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C32 H50 N6 Si2'
_chemical_formula_weight         574.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.806(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0265(2)
_cell_length_b                   19.8040(4)
_cell_length_c                   10.3399(3)
_cell_measurement_reflns_used    6415
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3200
_cell_measurement_theta_min      4.4320
_cell_volume                     1677.83(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10526
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         4.47
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.915
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0722
_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)+(0.0784P)²+3.5887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.1878
_reflns_number_gt                2918
_reflns_number_total             3120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja507785z_si_006.cif
_cod_data_source_block           p21m
_cod_depositor_comments
'Adding full bibliography for 4122689--4122694.cif.'
_cod_original_cell_volume        1677.83(7)
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               4122691
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Si1 Si 0.25747(13) 0.7500 0.25374(10) 0.0251(3) Uani 1 2 d S . .
Si2 Si -0.09349(16) 0.7500 -0.00200(15) 0.0486(4) Uani 1 2 d S . .
N1 N 0.3338(2) 0.68124(11) 0.3631(2) 0.0209(5) Uani 1 1 d . A .
N2 N 0.0575(5) 0.7500 0.1681(4) 0.0399(9) Uani 1 2 d S . .
H2 H 0.021(7) 0.7500 0.224(6) 0.048 Uiso 1 2 d S . .
N3 N 0.3244(6) 0.7500 0.1194(4) 0.0431(9) Uani 1 2 d S . .
N4 N 0.4612(8) 0.7500 0.1433(6) 0.0626(13) Uani 1 2 d S . .
N5 N 0.6001(8) 0.7500 0.1582(9) 0.097(2) Uani 1 2 d S . .
C1 C 0.5675(4) 0.62634(16) 0.5543(3) 0.0340(7) Uani 0.50 1 d P A 1
H1A H 0.6618 0.6386 0.6422 0.051 Uiso 0.50 1 calc PR A 1
H1B H 0.6045 0.6012 0.4918 0.051 Uiso 0.50 1 calc PR A 1
H1C H 0.4926 0.5982 0.5775 0.051 Uiso 0.50 1 calc PR A 1
C1A C 0.5675(4) 0.62634(16) 0.5543(3) 0.0340(7) Uani 0.50 1 d P A 2
H1D H 0.663(11) 0.633(4) 0.628(9) 0.051 Uiso 0.50 1 d P B 2
H1E H 0.520(10) 0.585(4) 0.525(8) 0.051 Uiso 0.50 1 d P C 2
C2 C 0.4852(3) 0.68607(14) 0.4838(3) 0.0249(6) Uani 1 1 d . . .
C3 C 0.5522(4) 0.7500 0.5318(4) 0.0266(8) Uani 1 2 d S . .
H3 H 0.6583 0.7500 0.6078 0.032 Uiso 1 2 calc SR . .
C4 C 0.2519(3) 0.61671(13) 0.3279(3) 0.0238(6) Uani 1 1 d . . .
C5 C 0.1333(3) 0.60207(14) 0.3782(3) 0.0310(6) Uani 1 1 d . A .
C6 C 0.0508(4) 0.54062(16) 0.3399(4) 0.0414(8) Uani 1 1 d . . .
H6 H -0.0298 0.5299 0.3732 0.050 Uiso 1 1 calc R A .
C7 C 0.0841(4) 0.49529(16) 0.2547(4) 0.0435(8) Uani 1 1 d . A .
H7 H 0.0259 0.4539 0.2289 0.052 Uiso 1 1 calc R . .
C8 C 0.2014(4) 0.50996(15) 0.2071(3) 0.0372(7) Uani 1 1 d . . .
H8 H 0.2234 0.4783 0.1483 0.045 Uiso 1 1 calc R A .
C9 C 0.2888(3) 0.57018(14) 0.2429(3) 0.0279(6) Uani 1 1 d . A .
C10 C 0.4209(4) 0.58212(15) 0.1912(3) 0.0340(7) Uani 1 1 d . . .
H10 H 0.4764 0.6257 0.2327 0.041 Uiso 1 1 calc R A .
C11 C 0.3474(5) 0.58835(19) 0.0277(4) 0.0505(9) Uani 1 1 d . A .
H11A H 0.2973 0.5453 -0.0153 0.076 Uiso 1 1 calc R . .
H11B H 0.4338 0.5998 -0.0024 0.076 Uiso 1 1 calc R . .
H11C H 0.2643 0.6239 -0.0031 0.076 Uiso 1 1 calc R . .
C12 C 0.5502(5) 0.52588(18) 0.2402(5) 0.0498(9) Uani 1 1 d . A .
H12A H 0.4987 0.4827 0.1995 0.075 Uiso 1 1 calc R . .
H12B H 0.5988 0.5230 0.3444 0.075 Uiso 1 1 calc R . .
H12C H 0.6354 0.5361 0.2079 0.075 Uiso 1 1 calc R . .
C13 C 0.0968(4) 0.65044(16) 0.4762(4) 0.0409(8) Uani 1 1 d . . .
H13 H 0.1260 0.6970 0.4575 0.049 Uiso 1 1 calc R A .
C14 C 0.2000(5) 0.6346(2) 0.6326(4) 0.0559(10) Uani 1 1 d . A .
H14A H 0.1750 0.5889 0.6540 0.084 Uiso 1 1 calc R . .
H14B H 0.1756 0.6673 0.6922 0.084 Uiso 1 1 calc R . .
H14C H 0.3159 0.6375 0.6524 0.084 Uiso 1 1 calc R . .
C15 C -0.0840(5) 0.6508(2) 0.4463(5) 0.0644(12) Uani 1 1 d . A .
H15A H -0.1132 0.6074 0.4747 0.097 Uiso 1 1 calc R . .
H15B H -0.1499 0.6581 0.3443 0.097 Uiso 1 1 calc R . .
H15C H -0.1048 0.6872 0.5008 0.097 Uiso 1 1 calc R . .
C16 C -0.0034(8) 0.7500 -0.1392(6) 0.102(3) Uani 1 2 d S . .
H16A H 0.0921 0.7203 -0.1067 0.154 Uiso 0.50 1 calc PR . .
H16B H 0.0293 0.7960 -0.1506 0.154 Uiso 0.50 1 calc PR . .
H16C H -0.0855 0.7337 -0.2308 0.154 Uiso 0.50 1 calc PR . .
C17 C -0.2080(8) 0.6708(3) -0.0240(6) 0.102(2) Uani 1 1 d . . .
H17A H -0.1382 0.6325 -0.0221 0.153 Uiso 1 1 calc R . .
H17B H -0.3044 0.6714 -0.1154 0.153 Uiso 1 1 calc R . .
H17C H -0.2425 0.6661 0.0537 0.153 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
N2 Si1 N1 113.65(11) . 4_575
N2 Si1 N1 113.65(11) . .
N1 Si1 N1 104.79(15) 4_575 .
N2 Si1 N3 104.0(2) . .
N1 Si1 N3 110.44(12) 4_575 .
N1 Si1 N3 110.44(12) . .
N2 Si2 C17 106.9(2) . .
N2 Si2 C17 106.9(2) . 4_575
C17 Si2 C17 117.0(5) . 4_575
N2 Si2 C16 111.1(3) . .
C17 Si2 C16 107.5(2) . .
C17 Si2 C16 107.5(2) 4_575 .
C2 N1 C4 119.0(2) . .
C2 N1 Si1 119.92(17) . .
C4 N1 Si1 120.88(16) . .
Si1 N2 Si2 140.6(3) . .
N4 N3 Si1 122.1(4) . .
N3 N4 N5 175.5(7) . .
C3 C2 N1 119.2(2) . .
C3 C2 C1 120.9(3) . .
N1 C2 C1 119.9(2) . .
C2 C3 C2 129.3(3) . 4_575
C5 C4 C9 120.9(2) . .
C5 C4 N1 118.6(2) . .
C9 C4 N1 120.5(2) . .
C6 C5 C4 118.3(3) . .
C6 C5 C13 119.8(3) . .
C4 C5 C13 121.8(3) . .
C7 C6 C5 121.1(3) . .
C8 C7 C6 120.0(3) . .
C7 C8 C9 121.5(3) . .
C8 C9 C4 118.1(3) . .
C8 C9 C10 118.8(3) . .
C4 C9 C10 123.1(2) . .
C9 C10 C12 111.8(3) . .
C9 C10 C11 111.0(3) . .
C12 C10 C11 109.8(3) . .
C14 C13 C5 111.7(3) . .
C14 C13 C15 110.0(3) . .
C5 C13 C15 112.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 N2 1.644(4) .
Si1 N1 1.719(2) 4_575
Si1 N1 1.719(2) .
Si1 N3 1.732(4) .
Si2 N2 1.714(4) .
Si2 C17 1.840(6) .
Si2 C17 1.840(6) 4_575
Si2 C16 1.908(7) .
N1 C2 1.415(3) .
N1 C4 1.444(3) .
N3 N4 1.153(7) .
N4 N5 1.197(8) .
C1 C2 1.424(4) .
C2 C3 1.401(3) .
C3 C2 1.401(3) 4_575
C4 C5 1.403(4) .
C4 C9 1.407(4) .
C5 C6 1.395(4) .
C5 C13 1.527(4) .
C6 C7 1.376(5) .
C7 C8 1.374(5) .
C8 C9 1.392(4) .
C9 C10 1.516(4) .
C10 C12 1.537(4) .
C10 C11 1.540(5) .
C13 C14 1.522(5) .
C13 C15 1.528(5) .
