#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:53:42 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/08/7040895.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_7040895
loop_
_publ_author_name
'Portius, Peter'
'Davis, Martin'
_publ_section_title
;
 Synthesis of six-coordinate mono-, bis-, and tris(tetrazolato) complexes
 via [3 + 2] cycloadditions of nitriles to silicon-bound azido ligands.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17141
_journal_page_last               17152
_journal_paper_doi               10.1039/c6dt02867e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C14 H14 N16 Si'
_chemical_formula_sum            'C14 H14 N16 Si'
_chemical_formula_weight         434.50
_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
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.555(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7941(6)
_cell_length_b                   13.5508(6)
_cell_length_c                   12.6135(6)
_cell_measurement_reflns_used    6410
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.33
_cell_volume                     1951.19(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11099
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9589
_exptl_absorpt_correction_T_min  0.9378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0316
_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)+(0.0429P)²+1.4588P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                1984
_reflns_number_total             2237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02867e2.cif
_cod_data_source_block           ch1ppx105_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7040891--7040897.cif.
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7040895
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
Si1 Si 1.0000 0.46053(3) 0.2500 0.01567(13) Uani 1 2 d S
C1 C 0.70716(11) 0.43659(9) 0.34531(10) 0.0193(2) Uani 1 1 d .
C2 C 0.63687(11) 0.42049(10) 0.42678(11) 0.0253(3) Uani 1 1 d .
H2A H 0.6436 0.3514 0.4504 0.038 Uiso 1 1 calc R
H2B H 0.5545 0.4361 0.3932 0.038 Uiso 1 1 calc R
H2C H 0.6663 0.4634 0.4903 0.038 Uiso 1 1 calc R
C3 C 0.91693(10) 0.36314(10) 0.03761(10) 0.0203(3) Uani 1 1 d .
H3 H 0.9051 0.4275 0.0070 0.024 Uiso 1 1 calc R
C4 C 0.89139(11) 0.28173(10) -0.03067(10) 0.0239(3) Uani 1 1 d .
H4 H 0.8619 0.2903 -0.1074 0.029 Uiso 1 1 calc R
C5 C 0.90914(12) 0.18805(10) 0.01359(11) 0.0273(3) Uani 1 1 d .
H5 H 0.8915 0.1317 -0.0324 0.033 Uiso 1 1 calc R
C6 C 0.95302(12) 0.17703(10) 0.12571(11) 0.0269(3) Uani 1 1 d .
H6 H 0.9666 0.1132 0.1576 0.032 Uiso 1 1 calc R
C7 C 0.97664(10) 0.26063(9) 0.19018(9) 0.0190(3) Uani 1 1 d .
N1 N 0.84734(9) 0.45179(7) 0.27236(8) 0.0176(2) Uani 1 1 d .
N2 N 0.75038(10) 0.45873(9) 0.19229(9) 0.0283(3) Uani 1 1 d .
N3 N 0.66041(10) 0.44974(10) 0.23716(9) 0.0298(3) Uani 1 1 d .
N4 N 0.82324(9) 0.43796(8) 0.36992(8) 0.0208(2) Uani 1 1 d .
N5 N 0.95828(9) 0.54925(8) 0.14047(8) 0.0210(2) Uani 1 1 d .
N6 N 0.89624(10) 0.61915(8) 0.14915(9) 0.0251(3) Uani 1 1 d .
N7 N 0.83881(13) 0.68580(10) 0.15309(12) 0.0440(4) Uani 1 1 d .
N8 N 0.95829(8) 0.35249(7) 0.14663(8) 0.0166(2) Uani 1 1 d .
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
N5 Si1 N5 96.42(7) 2_755 .
N5 Si1 N1 93.97(5) 2_755 2_755
N5 Si1 N1 90.81(5) . 2_755
N5 Si1 N1 90.81(5) 2_755 .
N5 Si1 N1 93.97(5) . .
N1 Si1 N1 172.83(6) 2_755 .
N5 Si1 N8 172.74(5) 2_755 .
N5 Si1 N8 90.80(5) . .
N1 Si1 N8 86.72(4) 2_755 .
N1 Si1 N8 87.87(4) . .
N5 Si1 N8 90.80(5) 2_755 2_755
N5 Si1 N8 172.74(5) . 2_755
N1 Si1 N8 87.87(4) 2_755 2_755
N1 Si1 N8 86.72(4) . 2_755
N8 Si1 N8 82.00(6) . 2_755
N4 C1 N3 111.76(11) . .
N4 C1 C2 124.16(11) . .
N3 C1 C2 124.07(11) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N8 C3 C4 121.06(12) . .
N8 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C5 C4 C3 119.56(11) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.2 . .
C4 C5 C6 119.41(12) . .
C4 C5 H5 120.3 . .
C6 C5 H5 120.3 . .
C7 C6 C5 118.72(12) . .
C7 C6 H6 120.6 . .
C5 C6 H6 120.6 . .
N8 C7 C6 121.76(11) . .
N8 C7 C7 113.34(6) . 2_755
C6 C7 C7 124.90(8) . 2_755
N2 N1 N4 111.54(10) . .
N2 N1 Si1 123.53(8) . .
N4 N1 Si1 124.93(8) . .
N1 N2 N3 107.32(10) . .
N2 N3 C1 106.02(10) . .
C1 N4 N1 103.36(10) . .
N6 N5 Si1 120.24(9) . .
N7 N6 N5 177.11(14) . .
C3 N8 C7 119.49(10) . .
C3 N8 Si1 124.83(9) . .
C7 N8 Si1 115.65(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 N5 1.8040(11) 2_755
Si1 N5 1.8040(11) .
Si1 N1 1.8949(10) 2_755
Si1 N1 1.8949(10) .
Si1 N8 1.9399(10) .
Si1 N8 1.9399(10) 2_755
C1 N4 1.3257(16) .
C1 N3 1.3486(16) .
C1 C2 1.4897(17) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 N8 1.3463(15) .
C3 C4 1.3853(18) .
C3 H3 0.9500 .
C4 C5 1.381(2) .
C4 H4 0.9500 .
C5 C6 1.3864(19) .
C5 H5 0.9500 .
C6 C7 1.3815(17) .
C6 H6 0.9500 .
C7 N8 1.3558(16) .
C7 C7 1.471(2) 2_755
N1 N2 1.3252(14) .
N1 N4 1.3439(14) .
N2 N3 1.3278(15) .
N5 N6 1.2186(15) .
N6 N7 1.1375(17) .
