#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:28:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178566 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/75/4067530.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_4067530
loop_
_publ_author_name
'Stueger, Harald'
'Fuerpass, Gottfried'
'Mitterfellner, Thomas'
'Baumgartner, Judith'
_publ_section_title
;
 Synthesis and Reactivity of NH2Derivatives of Dodecamethylcyclohexasilane
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              618
_journal_paper_doi               10.1021/om9010017
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C10 H31 N Si6'
_chemical_formula_weight         333.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 106.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.902(4)
_cell_length_b                   7.3368(15)
_cell_length_c                   16.269(3)
_cell_measurement_reflns_used    2456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.029
_cell_measurement_theta_min      4.739
_cell_volume                     2046.2(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       'ω 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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7846
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.9325
_exptl_absorpt_correction_T_min  0.8275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         2089
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0350
_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)+(0.0539P)²+0.5590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                1752
_reflns_number_total             2089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9010017_si_001.cif
_cod_data_source_block           298j
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2046.2(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4067530
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
N1 N 0.5000 0.7090(3) 0.2500 0.0350(5) Uani 1 2 d SD
H7 H 0.5000 0.824(3) 0.2500 0.14(2) Uiso 1 2 d SD
Si1 Si 0.49382(3) 0.57795(6) 0.15787(3) 0.02946(17) Uani 1 1 d .
Si2 Si 0.37670(3) 0.42115(7) 0.14541(3) 0.03154(17) Uani 1 1 d .
Si3 Si 0.39353(3) 0.39373(7) 0.29402(3) 0.02794(17) Uani 1 1 d .
C1 C 0.49261(16) 0.7317(3) 0.06505(13) 0.0514(6) Uani 1 1 d .
H1A H 0.4495 0.8188 0.0564 0.077 Uiso 1 1 calc R
H1B H 0.4856 0.6584 0.0130 0.077 Uiso 1 1 calc R
H1C H 0.5421 0.7982 0.0774 0.077 Uiso 1 1 calc R
C2 C 0.29242(14) 0.5765(4) 0.09370(14) 0.0592(7) Uani 1 1 d .
H2A H 0.2889 0.5924 0.0329 0.089 Uiso 1 1 calc R
H2B H 0.3007 0.6953 0.1225 0.089 Uiso 1 1 calc R
H2C H 0.2439 0.5226 0.0989 0.089 Uiso 1 1 calc R
C3 C 0.36270(12) 0.1965(3) 0.08769(13) 0.0434(5) Uani 1 1 d .
H3A H 0.3127 0.1435 0.0884 0.065 Uiso 1 1 calc R
H3B H 0.4051 0.1136 0.1164 0.065 Uiso 1 1 calc R
H3C H 0.3630 0.2152 0.0282 0.065 Uiso 1 1 calc R
C4 C 0.31074(12) 0.4981(3) 0.32801(13) 0.0468(6) Uani 1 1 d .
H4A H 0.2623 0.4323 0.3006 0.070 Uiso 1 1 calc R
H4B H 0.3048 0.6264 0.3105 0.070 Uiso 1 1 calc R
H4C H 0.3221 0.4898 0.3905 0.070 Uiso 1 1 calc R
C5 C 0.40558(11) 0.1475(3) 0.32768(12) 0.0360(4) Uani 1 1 d .
H5A H 0.4178 0.1394 0.3903 0.054 Uiso 1 1 calc R
H5B H 0.4482 0.0935 0.3093 0.054 Uiso 1 1 calc R
H5C H 0.3571 0.0815 0.3010 0.054 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0730(16) 0.0163(11) 0.0221(11) 0.000 0.0239(11) 0.000
Si1 0.0527(4) 0.0192(3) 0.0214(3) -0.00046(17) 0.0183(2) -0.0001(2)
Si2 0.0315(3) 0.0432(3) 0.0217(3) 0.0025(2) 0.0104(2) 0.0118(2)
Si3 0.0278(3) 0.0355(3) 0.0225(3) 0.0057(2) 0.0104(2) 0.0104(2)
C1 0.113(2) 0.0239(10) 0.0274(11) 0.0003(8) 0.0360(12) 0.0006(11)
C2 0.0589(15) 0.092(2) 0.0265(12) 0.0116(11) 0.0114(10) 0.0424(13)
C3 0.0362(11) 0.0571(13) 0.0407(12) -0.0110(10) 0.0171(9) -0.0092(10)
C4 0.0421(12) 0.0703(15) 0.0346(12) 0.0129(11) 0.0217(10) 0.0242(11)
C5 0.0365(11) 0.0333(10) 0.0333(11) 0.0023(8) 0.0020(8) -0.0019(8)
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_3
Si1 N1 Si1 113.66(12) 2_655
N1 Si1 C1 109.88(9) .
N1 Si1 Si2 100.18(4) .
C1 Si1 Si2 114.92(9) .
N1 Si1 Si3 101.09(5) 2_655
C1 Si1 Si3 114.83(9) 2_655
Si2 Si1 Si3 113.79(3) 2_655
C3 Si2 C2 109.47(11) .
C3 Si2 Si1 117.41(7) .
C2 Si2 Si1 108.80(9) .
C3 Si2 Si3 113.40(7) .
C2 Si2 Si3 111.02(8) .
Si1 Si2 Si3 96.11(4) .
C5 Si3 C4 109.76(10) .
C5 Si3 Si2 110.52(7) .
C4 Si3 Si2 112.77(7) .
C5 Si3 Si1 115.90(7) 2_655
C4 Si3 Si1 109.74(8) 2_655
Si2 Si3 Si1 97.77(4) 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 Si1 1.7571(13) .
N1 Si1 1.7571(13) 2_655
Si1 C1 1.8802(19) .
Si1 Si2 2.3486(8) .
Si1 Si3 2.3657(9) 2_655
Si2 C3 1.878(2) .
Si2 C2 1.885(2) .
Si2 Si3 2.3573(9) .
Si3 C5 1.8817(19) .
Si3 C4 1.8872(19) .
Si3 Si1 2.3657(9) 2_655
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_4
Si1 N1 Si1 C1 -177.16(10) 2_655 .
Si1 N1 Si1 Si2 61.50(3) 2_655 .
Si1 N1 Si1 Si3 -55.43(2) 2_655 2_655
N1 Si1 Si2 C3 -155.02(10) . .
C1 Si1 Si2 C3 87.31(11) . .
Si3 Si1 Si2 C3 -48.00(9) 2_655 .
N1 Si1 Si2 C2 80.01(10) . .
C1 Si1 Si2 C2 -37.66(11) . .
Si3 Si1 Si2 C2 -172.97(8) 2_655 .
N1 Si1 Si2 Si3 -34.66(6) . .
C1 Si1 Si2 Si3 -152.33(7) . .
Si3 Si1 Si2 Si3 72.36(3) 2_655 .
C3 Si2 Si3 C5 9.12(10) . .
C2 Si2 Si3 C5 132.86(12) . .
Si1 Si2 Si3 C5 -114.30(7) . .
C3 Si2 Si3 C4 -114.15(11) . .
C2 Si2 Si3 C4 9.59(13) . .
Si1 Si2 Si3 C4 122.44(9) . .
C3 Si2 Si3 Si1 130.57(7) . 2_655
C2 Si2 Si3 Si1 -105.69(10) . 2_655
Si1 Si2 Si3 Si1 7.16(3) . 2_655
