#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/07/4060711.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_4060711
loop_
_publ_author_name
'Shutov, Pavel L.'
'Sorokin, Denis A.'
'Karlov, Sergey S.'
'Harms, Klaus'
'Oprunenko, Yuri F.'
'Churakov, Andrei V.'
'Antipin, Mikhail Yu.'
'Zaitseva, Galina S.'
'Lorberth, Jörg'
_publ_section_title
;
 Azametallatranes of Group 14 Elements. Syntheses and X-ray Studies
;
_journal_coden_ASTM              ORGND7
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              516
_journal_page_last               522
_journal_paper_doi               10.1021/om020708h
_journal_volume                  22
_journal_year                    2003
_chemical_formula_sum            'C21 H44 N4 Si4'
_chemical_formula_weight         464.96
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   20.3499(9)
_cell_length_b                   20.3499(9)
_cell_length_c                   34.489(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.0
_cell_volume                     12368.9(12)
_computing_cell_refinement       'Stoe Cell'
_computing_data_collection       'Stoe Expose'
_computing_data_reduction        'Stoe Integrate'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            28420
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.8738
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4572
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5323
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          1.836
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0438P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                4854
_reflns_number_total             5323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020708h.cif
_cod_data_source_block           shut08a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4060711
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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 0.33742(2) 0.00856(2) 0.046112(14) 0.01986(10) Uani 1 1 d . . .
N1 N 0.31231(7) -0.08297(7) 0.03036(3) 0.0229(3) Uani 1 1 d . . .
Si2 Si 0.34141(3) -0.14438(2) 0.048799(18) 0.02900(11) Uani 1 1 d . . .
C2 C 0.26448(9) -0.10895(9) -0.00493(4) 0.0246(3) Uani 1 1 d . . .
H2A H 0.2200 -0.1021 -0.0013 0.030 Uiso 1 1 calc R . .
H2B H 0.2456 -0.1637 -0.0088 0.030 Uiso 1 1 calc R . .
Si3 Si 0.48733(3) 0.16592(3) 0.051250(13) 0.02872(13) Uani 1 1 d . . .
C3 C 0.30817(9) -0.06542(9) -0.04085(4) 0.0273(3) Uani 1 1 d . . .
H3A H 0.3487 -0.0774 -0.0466 0.033 Uiso 1 1 calc R . .
H3B H 0.2734 -0.0812 -0.0634 0.033 Uiso 1 1 calc R . .
Si4 Si 0.17318(3) -0.00979(3) 0.043165(10) 0.02435(12) Uani 1 1 d . . .
N4 N 0.34140(7) 0.01527(7) -0.03476(4) 0.0270(3) Uani 1 1 d . . .
C5 C 0.42245(9) 0.06284(9) -0.03900(4) 0.0276(3) Uani 1 1 d . . .
H5A H 0.4353 0.1159 -0.0437 0.033 Uiso 1 1 calc R . .
H5B H 0.4401 0.0456 -0.0615 0.033 Uiso 1 1 calc R . .
C6 C 0.46195(9) 0.05873(9) -0.00217(4) 0.0253(3) Uani 1 1 d . . .
H6A H 0.4557 0.0074 0.0002 0.030 Uiso 1 1 calc R . .
H6B H 0.5169 0.0958 -0.0039 0.030 Uiso 1 1 calc R . .
N7 N 0.42971(7) 0.07535(7) 0.03264(3) 0.0236(3) Uani 1 1 d . . .
C8 C 0.29404(9) 0.04906(9) -0.03900(4) 0.0270(3) Uani 1 1 d . . .
H8A H 0.2420 0.0095 -0.0463 0.032 Uiso 1 1 calc R . .
H8B H 0.3144 0.0876 -0.0599 0.032 Uiso 1 1 calc R . .
C9 C 0.29156(9) 0.08643(9) -0.00098(4) 0.0256(3) Uani 1 1 d . . .
H9A H 0.3421 0.1310 0.0042 0.031 Uiso 1 1 calc R . .
H9B H 0.2547 0.1044 -0.0034 0.031 Uiso 1 1 calc R . .
N10 N 0.26940(7) 0.03234(7) 0.03188(4) 0.0221(3) Uani 1 1 d . . .
C11 C 0.34072(8) 0.01036(9) 0.10147(5) 0.0260(3) Uani 1 1 d . . .
C12 C 0.28966(10) 0.01951(11) 0.12430(5) 0.0386(4) Uani 1 1 d . . .
H12A H 0.2519 0.0266 0.1119 0.046 Uiso 1 1 calc R . .
C13 C 0.29151(12) 0.01877(13) 0.16451(5) 0.0479(5) Uani 1 1 d . . .
H13A H 0.2555 0.0252 0.1790 0.057 Uiso 1 1 calc R . .
C14 C 0.34527(12) 0.00877(12) 0.18340(6) 0.0445(5) Uani 1 1 d . . .
H14A H 0.3452 0.0055 0.2109 0.053 Uiso 1 1 calc R . .
C15 C 0.39945(12) 0.00360(14) 0.16164(5) 0.0509(5) Uani 1 1 d . . .
H15A H 0.4387 -0.0006 0.1743 0.061 Uiso 1 1 calc R . .
C16 C 0.39694(11) 0.00454(12) 0.12142(5) 0.0412(4) Uani 1 1 d . . .
H16A H 0.4349 0.0011 0.1071 0.049 Uiso 1 1 calc R . .
C21 C 0.29319(11) -0.18753(13) 0.09569(7) 0.0532(6) Uani 1 1 d . . .
H21A H 0.3018 -0.1472 0.1140 0.080 Uiso 1 1 calc R . .
H21B H 0.3138 -0.2181 0.1064 0.080 Uiso 1 1 calc R . .
H21C H 0.2386 -0.2200 0.0912 0.080 Uiso 1 1 calc R . .
C22 C 0.31551(15) -0.22555(12) 0.01472(8) 0.0625(7) Uani 1 1 d . . .
H22A H 0.2602 -0.2574 0.0135 0.094 Uiso 1 1 calc R . .
H22B H 0.3376 -0.2558 0.0240 0.094 Uiso 1 1 calc R . .
H22C H 0.3353 -0.2058 -0.0112 0.094 Uiso 1 1 calc R . .
C23 C 0.44692(10) -0.09858(11) 0.05440(6) 0.0404(4) Uani 1 1 d . . .
H23A H 0.4676 -0.0460 0.0631 0.061 Uiso 1 1 calc R . .
H23B H 0.4696 -0.0991 0.0294 0.061 Uiso 1 1 calc R . .
H23C H 0.4587 -0.1266 0.0736 0.061 Uiso 1 1 calc R . .
C31 C 0.43414(12) 0.19515(11) 0.08437(7) 0.0536(6) Uani 1 1 d . . .
H31A H 0.4268 0.1699 0.1095 0.080 Uiso 1 1 calc R . .
H31B H 0.3846 0.1807 0.0730 0.080 Uiso 1 1 calc R . .
H31C H 0.4630 0.2503 0.0881 0.080 Uiso 1 1 calc R . .
C32 C 0.57025(11) 0.17132(13) 0.07739(6) 0.0525(5) Uani 1 1 d . . .
H32A H 0.5527 0.1406 0.1010 0.079 Uiso 1 1 calc R . .
H32B H 0.6060 0.2242 0.0842 0.079 Uiso 1 1 calc R . .
H32C H 0.5956 0.1520 0.0606 0.079 Uiso 1 1 calc R . .
C33 C 0.52655(12) 0.23826(10) 0.01140(6) 0.0450(5) Uani 1 1 d . . .
H33A H 0.4851 0.2416 -0.0011 0.068 Uiso 1 1 calc R . .
H33B H 0.5520 0.2232 -0.0078 0.068 Uiso 1 1 calc R . .
H33C H 0.5631 0.2878 0.0223 0.068 Uiso 1 1 calc R . .
C41 C 0.15167(11) 0.05782(12) 0.06959(6) 0.0435(5) Uani 1 1 d . . .
H41A H 0.1748 0.0680 0.0954 0.065 Uiso 1 1 calc R . .
H41B H 0.0966 0.0353 0.0721 0.065 Uiso 1 1 calc R . .
H41C H 0.1724 0.1054 0.0550 0.065 Uiso 1 1 calc R . .
C42 C 0.14067(10) -0.09906(10) 0.07158(5) 0.0360(4) Uani 1 1 d . . .
H42A H 0.1697 -0.1234 0.0636 0.054 Uiso 1 1 calc R . .
H42B H 0.0866 -0.1336 0.0667 0.054 Uiso 1 1 calc R . .
H42C H 0.1487 -0.0869 0.0993 0.054 Uiso 1 1 calc R . .
C43 C 0.11180(10) -0.03769(11) -0.00133(5) 0.0383(4) Uani 1 1 d . . .
H43A H 0.1168 -0.0765 -0.0156 0.057 Uiso 1 1 calc R . .
H43B H 0.1278 0.0069 -0.0179 0.057 Uiso 1 1 calc R . .
H43C H 0.0587 -0.0580 0.0063 0.057 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'
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
N7 Si1 N10 113.74(6) . . ?
N7 Si1 N1 111.96(6) . . ?
N10 Si1 N1 110.87(6) . . ?
N7 Si1 C11 103.75(6) . . ?
N10 Si1 C11 107.46(6) . . ?
N1 Si1 C11 108.60(6) . . ?
C2 N1 Si2 116.15(10) . . ?
C2 N1 Si1 115.12(9) . . ?
Si2 N1 Si1 128.58(7) . . ?
N1 Si2 C21 111.41(8) . . ?
N1 Si2 C23 113.28(7) . . ?
C21 Si2 C23 110.26(10) . . ?
N1 Si2 C22 110.80(8) . . ?
C21 Si2 C22 106.16(12) . . ?
C23 Si2 C22 104.49(11) . . ?
N1 C2 C3 111.86(13) . . ?
N7 Si3 C31 111.91(8) . . ?
N7 Si3 C32 110.56(9) . . ?
C31 Si3 C32 109.72(11) . . ?
N7 Si3 C33 111.00(8) . . ?
C31 Si3 C33 106.60(10) . . ?
C32 Si3 C33 106.87(10) . . ?
N4 C3 C2 110.35(12) . . ?
N10 Si4 C42 111.06(7) . . ?
N10 Si4 C41 111.36(8) . . ?
C42 Si4 C41 111.04(9) . . ?
N10 Si4 C43 112.32(7) . . ?
C42 Si4 C43 106.00(8) . . ?
C41 Si4 C43 104.76(9) . . ?
C5 N4 C8 118.77(13) . . ?
C5 N4 C3 118.43(12) . . ?
C8 N4 C3 118.81(12) . . ?
N4 C5 C6 109.58(12) . . ?
N7 C6 C5 110.80(13) . . ?
C6 N7 Si3 113.52(10) . . ?
C6 N7 Si1 117.65(10) . . ?
Si3 N7 Si1 128.38(8) . . ?
N4 C8 C9 110.21(12) . . ?
N10 C9 C8 111.06(12) . . ?
C9 N10 Si4 112.65(9) . . ?
C9 N10 Si1 115.48(9) . . ?
Si4 N10 Si1 130.59(8) . . ?
C12 C11 C16 115.71(17) . . ?
C12 C11 Si1 123.22(12) . . ?
C16 C11 Si1 121.05(12) . . ?
C13 C12 C11 122.61(17) . . ?
C14 C13 C12 120.26(17) . . ?
C13 C14 C15 118.63(19) . . ?
C14 C15 C16 120.37(18) . . ?
C15 C16 C11 122.24(17) . . ?
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
Si1 N7 1.7428(13) . ?
Si1 N10 1.7497(12) . ?
Si1 N1 1.7532(13) . ?
Si1 C11 1.9102(18) . ?
N1 C2 1.4809(19) . ?
N1 Si2 1.7485(13) . ?
Si2 C21 1.868(2) . ?
Si2 C23 1.8748(18) . ?
Si2 C22 1.875(2) . ?
C2 C3 1.524(2) . ?
Si3 N7 1.7387(13) . ?
Si3 C31 1.864(2) . ?
Si3 C32 1.8672(19) . ?
Si3 C33 1.8757(19) . ?
C3 N4 1.445(2) . ?
Si4 N10 1.7439(13) . ?
Si4 C42 1.8698(17) . ?
Si4 C41 1.8753(19) . ?
Si4 C43 1.8783(17) . ?
N4 C5 1.443(2) . ?
N4 C8 1.444(2) . ?
C5 C6 1.528(2) . ?
C6 N7 1.4860(19) . ?
C8 C9 1.529(2) . ?
C9 N10 1.4842(19) . ?
C11 C12 1.388(2) . ?
C11 C16 1.390(2) . ?
C12 C13 1.388(2) . ?
C13 C14 1.373(3) . ?
C14 C15 1.381(3) . ?
C15 C16 1.388(2) . ?
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
N7 Si1 N1 C2 -101.00(11) . . . . ?
N10 Si1 N1 C2 27.20(12) . . . . ?
C11 Si1 N1 C2 145.04(10) . . . . ?
N7 Si1 N1 Si2 74.24(11) . . . . ?
N10 Si1 N1 Si2 -157.56(9) . . . . ?
C11 Si1 N1 Si2 -39.72(11) . . . . ?
C2 N1 Si2 C21 -110.01(13) . . . . ?
Si1 N1 Si2 C21 74.80(12) . . . . ?
C2 N1 Si2 C23 124.99(12) . . . . ?
Si1 N1 Si2 C23 -50.21(12) . . . . ?
C2 N1 Si2 C22 7.94(15) . . . . ?
Si1 N1 Si2 C22 -167.26(12) . . . . ?
Si2 N1 C2 C3 -106.70(13) . . . . ?
Si1 N1 C2 C3 69.16(14) . . . . ?
N1 C2 C3 N4 -54.50(17) . . . . ?
C2 C3 N4 C5 122.73(15) . . . . ?
C2 C3 N4 C8 -79.99(17) . . . . ?
C8 N4 C5 C6 122.50(15) . . . . ?
C3 N4 C5 C6 -80.21(17) . . . . ?
N4 C5 C6 N7 -52.60(17) . . . . ?
C5 C6 N7 Si3 -103.60(13) . . . . ?
C5 C6 N7 Si1 69.37(15) . . . . ?
C31 Si3 N7 C6 162.61(12) . . . . ?
C32 Si3 N7 C6 -74.77(13) . . . . ?
C33 Si3 N7 C6 43.65(13) . . . . ?
C31 Si3 N7 Si1 -9.44(14) . . . . ?
C32 Si3 N7 Si1 113.18(12) . . . . ?
C33 Si3 N7 Si1 -128.40(11) . . . . ?
N10 Si1 N7 C6 -100.65(11) . . . . ?
N1 Si1 N7 C6 26.00(13) . . . . ?
C11 Si1 N7 C6 142.91(11) . . . . ?
N10 Si1 N7 Si3 71.11(11) . . . . ?
N1 Si1 N7 Si3 -162.23(9) . . . . ?
C11 Si1 N7 Si3 -45.32(11) . . . . ?
C5 N4 C8 C9 -82.87(17) . . . . ?
C3 N4 C8 C9 119.93(15) . . . . ?
N4 C8 C9 N10 -52.99(16) . . . . ?
C8 C9 N10 Si4 -97.78(13) . . . . ?
C8 C9 N10 Si1 70.66(14) . . . . ?
C42 Si4 N10 C9 160.33(11) . . . . ?
C41 Si4 N10 C9 -75.34(12) . . . . ?
C43 Si4 N10 C9 41.81(13) . . . . ?
C42 Si4 N10 Si1 -5.89(13) . . . . ?
C41 Si4 N10 Si1 118.44(11) . . . . ?
C43 Si4 N10 Si1 -124.41(11) . . . . ?
N7 Si1 N10 C9 22.31(12) . . . . ?
N1 Si1 N10 C9 -104.91(10) . . . . ?
C11 Si1 N10 C9 136.55(11) . . . . ?
N7 Si1 N10 Si4 -171.78(9) . . . . ?
N1 Si1 N10 Si4 60.99(12) . . . . ?
C11 Si1 N10 Si4 -57.54(11) . . . . ?
N7 Si1 C11 C12 128.26(15) . . . . ?
N10 Si1 C11 C12 7.49(16) . . . . ?
N1 Si1 C11 C12 -112.49(15) . . . . ?
N7 Si1 C11 C16 -49.89(16) . . . . ?
N10 Si1 C11 C16 -170.66(14) . . . . ?
N1 Si1 C11 C16 69.36(16) . . . . ?
C16 C11 C12 C13 -3.4(3) . . . . ?
Si1 C11 C12 C13 178.31(16) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C12 C13 C14 C15 3.4(4) . . . . ?
C13 C14 C15 C16 -3.3(4) . . . . ?
C14 C15 C16 C11 -0.2(3) . . . . ?
C12 C11 C16 C15 3.5(3) . . . . ?
Si1 C11 C16 C15 -178.19(17) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21158586
