#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:27:39 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180263 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/49/7114999.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_7114999
loop_
_publ_author_name
'Kingston, Vijeyakumar'
'Gostevskii, Boris'
'Kalikhman, Inna'
'Kost, Daniel'
_publ_section_title
;
 Equilibrium between neutral hexacoordinate silicon complexes and ionic
 pentacoordinate siliconium salts through fast dissociation--recombination
 of the Si--Cl bond
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1272
_journal_paper_doi               10.1039/b102427m
_journal_year                    2001
_chemical_formula_sum            'C15 H23 F3 N4 O5 S Si'
_chemical_formula_weight         456.52
_chemical_melting_point          '182-184 &#x00A1;C'
_chemical_name_common            6a
_chemical_name_systematic
; 
Bis(N,N-dimethylacethydrazido-N,O)phenylsilicon trifluoromethylsulfonate 
;
_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           SHELXL-97
_cell_angle_alpha                89.784(5)
_cell_angle_beta                 84.087(5)
_cell_angle_gamma                75.050(5)
_cell_formula_units_Z            2
_cell_length_a                   8.4678(15)
_cell_length_b                   11.032(2)
_cell_length_c                   11.517(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1033.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_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            12650
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0585P)²+0.0032P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                3913
_reflns_number_total             5128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102427m.txt
_cod_data_source_block           6a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1033.7(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114999
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
Si1 Si 0.27211(5) 0.79031(4) 0.80126(3) 0.01707(10) Uani 1 1 d .
C1 C -0.00793(18) 0.85138(15) 0.72330(13) 0.0223(3) Uani 1 1 d .
C2 C -0.1365(2) 0.94598(16) 0.67011(16) 0.0307(4) Uani 1 1 d .
H2A H -0.2060 0.9036 0.6316 0.046 Uiso 1 1 calc R
H2B H -0.0844 0.9931 0.6125 0.046 Uiso 1 1 calc R
H2C H -0.2040 1.0039 0.7311 0.046 Uiso 1 1 calc R
C3 C 0.0623(2) 0.63231(17) 0.88988(15) 0.0305(4) Uani 1 1 d .
H3A H 0.0041 0.7082 0.9358 0.046 Uiso 1 1 calc R
H3B H 0.1455 0.5799 0.9347 0.046 Uiso 1 1 calc R
H3C H -0.0162 0.5853 0.8721 0.046 Uiso 1 1 calc R
C4 C 0.2355(2) 0.55244(15) 0.70998(15) 0.0307(4) Uani 1 1 d .
H4A H 0.1628 0.4969 0.7046 0.046 Uiso 1 1 calc R
H4B H 0.3309 0.5093 0.7493 0.046 Uiso 1 1 calc R
H4C H 0.2726 0.5748 0.6313 0.046 Uiso 1 1 calc R
C5 C 0.46520(18) 0.74208(14) 0.96194(12) 0.0207(3) Uani 1 1 d .
C6 C 0.5725(2) 0.65070(15) 1.03283(15) 0.0302(4) Uani 1 1 d .
H6A H 0.6462 0.6915 1.0685 0.045 Uiso 1 1 calc R
H6B H 0.6377 0.5801 0.9828 0.045 Uiso 1 1 calc R
H6C H 0.5047 0.6199 1.0943 0.045 Uiso 1 1 calc R
C7 C 0.21118(19) 0.99974(14) 0.96983(13) 0.0235(3) Uani 1 1 d .
H7A H 0.1658 0.9441 1.0223 0.035 Uiso 1 1 calc R
H7B H 0.1232 1.0525 0.9290 0.035 Uiso 1 1 calc R
H7C H 0.2595 1.0532 1.0153 0.035 Uiso 1 1 calc R
C8 C 0.4085(2) 1.00945(15) 0.80507(14) 0.0263(3) Uani 1 1 d .
H8A H 0.4461 1.0677 0.8528 0.040 Uiso 1 1 calc R
H8B H 0.3225 1.0570 0.7595 0.040 Uiso 1 1 calc R
H8C H 0.5011 0.9611 0.7520 0.040 Uiso 1 1 calc R
C9 C 0.41212(18) 0.77051(14) 0.66489(12) 0.0201(3) Uani 1 1 d .
C10 C 0.5704(2) 0.68936(15) 0.65783(14) 0.0271(3) Uani 1 1 d .
H10 H 0.6046 0.6403 0.7231 0.033 Uiso 1 1 calc R
C11 C 0.6776(2) 0.67975(17) 0.55715(15) 0.0335(4) Uani 1 1 d .
H11 H 0.7846 0.6245 0.5540 0.040 Uiso 1 1 calc R
C12 C 0.6298(2) 0.75020(17) 0.46075(15) 0.0326(4) Uani 1 1 d .
H12 H 0.7037 0.7432 0.3917 0.039 Uiso 1 1 calc R
C13 C 0.4736(2) 0.83083(17) 0.46569(15) 0.0335(4) Uani 1 1 d .
H13 H 0.4397 0.8784 0.3995 0.040 Uiso 1 1 calc R
C14 C 0.3668(2) 0.84213(16) 0.56711(14) 0.0267(3) Uani 1 1 d .
H14 H 0.2611 0.8994 0.5704 0.032 Uiso 1 1 calc R
C15 C 0.1113(2) 0.68172(18) 0.35997(15) 0.0347(4) Uani 1 1 d .
F1 F 0.26517(17) 0.65231(16) 0.38534(12) 0.0700(4) Uani 1 1 d .
F2 F 0.04177(14) 0.59595(10) 0.40816(9) 0.0424(3) Uani 1 1 d .
F3 F 0.0332(2) 0.79084(12) 0.41274(11) 0.0652(4) Uani 1 1 d .
N1 N 0.00946(16) 0.73353(13) 0.71140(11) 0.0254(3) Uani 1 1 d .
N2 N 0.14439(16) 0.66852(12) 0.77795(11) 0.0221(3) Uani 1 1 d .
N3 N 0.47308(15) 0.85586(12) 0.95118(11) 0.0229(3) Uani 1 1 d .
N4 N 0.34126(15) 0.92238(11) 0.88229(10) 0.0186(3) Uani 1 1 d .
O1 O 0.09281(12) 0.89724(10) 0.78559(9) 0.0221(2) Uani 1 1 d .
O2 O 0.35615(13) 0.69824(9) 0.90753(9) 0.0209(2) Uani 1 1 d .
O3 O -0.07466(19) 0.71233(16) 0.19345(13) 0.0552(4) Uani 1 1 d .
O4 O 0.1735(2) 0.78558(13) 0.16620(13) 0.0584(5) Uani 1 1 d .
O5 O 0.19316(17) 0.56316(12) 0.16428(11) 0.0401(3) Uani 1 1 d .
S1 S 0.09933(6) 0.68671(4) 0.20260(3) 0.03063(12) 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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
O2 Si1 O1 137.05(6)
O2 Si1 C9 112.09(6)
O1 Si1 C9 110.86(6)
O2 Si1 N2 87.54(5)
O1 Si1 N2 83.70(6)
C9 Si1 N2 102.21(6)
O2 Si1 N4 84.15(5)
O1 Si1 N4 88.03(5)
C9 Si1 N4 100.55(6)
N2 Si1 N4 157.24(6)
N1 C1 O1 121.32(13)
N1 C1 C2 122.63(14)
O1 C1 C2 116.05(13)
N3 C5 O2 121.09(13)
N3 C5 C6 123.06(13)
O2 C5 C6 115.85(13)
C10 C9 C14 117.83(14)
C10 C9 Si1 121.26(11)
C14 C9 Si1 120.81(12)
C11 C10 C9 120.90(15)
C10 C11 C12 120.45(16)
C13 C12 C11 119.62(16)
C12 C13 C14 120.07(15)
C13 C14 C9 121.11(15)
F1 C15 F2 106.93(16)
F1 C15 F3 108.33(16)
F2 C15 F3 106.71(15)
F1 C15 S1 111.80(13)
F2 C15 S1 111.05(12)
F3 C15 S1 111.76(13)
C1 N1 N2 107.92(12)
N1 N2 C4 107.17(11)
N1 N2 C3 105.31(12)
C4 N2 C3 109.02(12)
N1 N2 Si1 105.96(9)
C4 N2 Si1 115.44(10)
C3 N2 Si1 113.22(10)
C5 N3 N4 108.60(11)
N3 N4 C8 107.46(11)
N3 N4 C7 105.11(11)
C8 N4 C7 108.04(12)
N3 N4 Si1 105.77(8)
C8 N4 Si1 115.45(9)
C7 N4 Si1 114.27(9)
C1 O1 Si1 112.81(9)
C5 O2 Si1 114.42(9)
O4 S1 O5 114.80(9)
O4 S1 O3 115.37(10)
O5 S1 O3 115.03(10)
O4 S1 C15 103.62(9)
O5 S1 C15 102.28(8)
O3 S1 C15 103.21(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Si1 O2 1.6833(11)
Si1 O1 1.6911(11)
Si1 C9 1.8453(15)
Si1 N2 1.9645(13)
Si1 N4 1.9747(13)
C1 N1 1.276(2)
C1 O1 1.3600(17)
C1 C2 1.482(2)
C3 N2 1.503(2)
C4 N2 1.490(2)
C5 N3 1.279(2)
C5 O2 1.3532(17)
C5 C6 1.477(2)
C7 N4 1.5003(19)
C8 N4 1.4862(19)
C9 C10 1.401(2)
C9 C14 1.402(2)
C10 C11 1.383(2)
C11 C12 1.387(2)
C12 C13 1.386(3)
C13 C14 1.387(2)
C15 F1 1.322(2)
C15 F2 1.329(2)
C15 F3 1.330(2)
C15 S1 1.8256(18)
N1 N2 1.4699(17)
N3 N4 1.4729(16)
O3 S1 1.4417(16)
O4 S1 1.4337(14)
O5 S1 1.4343(13)
