#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:57:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178926 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/55/4115555.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_4115555
loop_
_publ_author_name
'Inna Kalikhman'
'Olga Girshberg'
'Lutz Lameyer'
'Dietmar Stalke'
'Daniel Kost'
_publ_section_title
;
 Tautomeric Equilibrium between Penta- and Hexacoordinate Silicon
 Chelates. A Chloride Bridge between Two Pentacoordinate Silicons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4709
_journal_page_last               4716
_journal_paper_doi               10.1021/ja004118r
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C6 H11 Cl2 F3 N2 O Si'
_chemical_formula_weight         283.16
_chemical_name_common            9a
_chemical_name_systematic
; 
(1-((1,1-dimethyl-2-trifluoroacetyl)hydrazonim)methyl-C,O)
methyldichlorosilicon(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.68(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.487(2)
_cell_length_b                   7.1123(6)
_cell_length_c                   13.738(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1206.1(4)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        XCAD4b
_computing_molecular_graphics    'Bruker SHELXTL-Plus'
_computing_publication_material  'Bruker SHELXTL-Plus'
_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  CAD4
_diffrn_measurement_method       2theta/omega
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2303
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.7361
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       prisms
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0039(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0663P)²+0.9968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                1844
_reflns_number_total             2125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004118r_1.cif
_cod_data_source_block           9a
_cod_original_cell_volume        1206.1(3)
_cod_database_code               4115555
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
C1 C 0.6448(2) -0.1390(4) 0.2627(2) 0.0392(7) Uani 1 1 d .
F1 F 0.72834(17) -0.0793(3) 0.2237(2) 0.0831(9) Uani 1 1 d .
F2 F 0.6791(2) -0.2136(4) 0.34920(16) 0.0783(8) Uani 1 1 d .
F3 F 0.60293(17) -0.2801(3) 0.20609(16) 0.0587(6) Uani 1 1 d .
C2 C 0.5625(2) 0.0171(4) 0.2647(2) 0.0290(6) Uani 1 1 d .
O1 O 0.52720(14) 0.0908(3) 0.17963(13) 0.0309(4) Uani 1 1 d .
N1 N 0.53959(17) 0.0554(3) 0.35032(16) 0.0299(5) Uani 1 1 d .
N2 N 0.46361(17) 0.2129(3) 0.34930(15) 0.0254(5) Uani 1 1 d .
C3 C 0.4294(2) 0.2129(4) 0.44927(18) 0.0312(6) Uani 1 1 d .
H3A H 0.3935 0.0936 0.4596 0.047 Uiso 1 1 calc R
H3B H 0.3791 0.3171 0.4539 0.047 Uiso 1 1 calc R
H3C H 0.4933 0.2279 0.4997 0.047 Uiso 1 1 calc R
C4 C 0.5229(2) 0.3922(4) 0.3358(2) 0.0361(7) Uani 1 1 d .
H4A H 0.5860 0.4027 0.3874 0.054 Uiso 1 1 calc R
H4B H 0.4745 0.4994 0.3400 0.054 Uiso 1 1 calc R
H4C H 0.5470 0.3915 0.2711 0.054 Uiso 1 1 calc R
C5 C 0.3635(2) 0.1913(4) 0.27270(18) 0.0254(5) Uani 1 1 d .
H5A H 0.3193 0.3066 0.2740 0.030 Uiso 1 1 calc R
H5B H 0.3204 0.0856 0.2932 0.030 Uiso 1 1 calc R
Si1 Si 0.38375(6) 0.14825(10) 0.14080(5) 0.0259(2) Uani 1 1 d .
Cl1 Cl 0.35519(6) -0.12411(11) 0.08907(6) 0.0423(2) Uani 1 1 d .
Cl2 Cl 0.19769(5) 0.21162(10) 0.10663(5) 0.0360(2) Uani 1 1 d .
C6 C 0.4159(3) 0.3315(5) 0.0543(2) 0.0430(8) Uani 1 1 d .
H6A H 0.4149 0.4552 0.0856 0.065 Uiso 1 1 calc R
H6B H 0.3619 0.3284 -0.0053 0.065 Uiso 1 1 calc R
H6C H 0.4880 0.3079 0.0369 0.065 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
C1 0.0323(15) 0.0352(17) 0.0510(18) -0.0005(14) 0.0090(13) 0.0045(13)
F1 0.0436(12) 0.0506(13) 0.168(3) 0.0138(15) 0.0569(14) 0.0100(10)
F2 0.0903(17) 0.0870(18) 0.0535(13) 0.0026(12) -0.0025(12) 0.0603(15)
F3 0.0626(13) 0.0336(11) 0.0785(15) -0.0096(10) 0.0060(11) 0.0103(9)
C2 0.0222(13) 0.0258(14) 0.0393(16) -0.0006(12) 0.0054(11) -0.0025(10)
O1 0.0264(9) 0.0335(11) 0.0342(10) 0.0021(8) 0.0091(8) 0.0013(8)
N1 0.0239(11) 0.0284(12) 0.0363(13) 0.0007(10) 0.0009(9) 0.0044(10)
N2 0.0221(11) 0.0261(11) 0.0275(11) -0.0001(9) 0.0017(9) 0.0020(9)
C3 0.0308(14) 0.0386(16) 0.0227(13) -0.0024(11) -0.0001(10) 0.0053(12)
C4 0.0326(15) 0.0275(15) 0.0474(17) -0.0045(13) 0.0039(13) -0.0070(12)
C5 0.0205(12) 0.0280(13) 0.0269(13) -0.0010(11) 0.0011(10) 0.0005(10)
Si1 0.0275(4) 0.0254(4) 0.0251(4) 0.0012(3) 0.0049(3) -0.0002(3)
Cl1 0.0392(4) 0.0331(4) 0.0553(5) -0.0146(3) 0.0097(3) -0.0022(3)
Cl2 0.0305(4) 0.0383(4) 0.0359(4) -0.0009(3) -0.0054(3) 0.0046(3)
C6 0.0490(18) 0.0461(18) 0.0365(16) 0.0136(14) 0.0146(13) 0.0018(15)
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'
Cl Cl 0.1484 0.1585 '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
F2 C1 F1 109.2(3)
F2 C1 F3 105.7(3)
F1 C1 F3 105.9(3)
F2 C1 C2 114.1(3)
F1 C1 C2 110.7(3)
F3 C1 C2 110.8(2)
N1 C2 O1 130.5(3)
N1 C2 C1 114.7(2)
O1 C2 C1 114.8(2)
C2 O1 Si1 122.40(17)
C2 N1 N2 112.8(2)
N1 N2 C3 105.4(2)
N1 N2 C4 108.63(19)
C3 N2 C4 109.1(2)
N1 N2 C5 113.19(19)
C3 N2 C5 108.5(2)
C4 N2 C5 111.8(2)
N2 C5 Si1 117.77(17)
O1 Si1 C6 92.66(13)
O1 Si1 C5 91.34(12)
C6 Si1 C5 125.11(14)
O1 Si1 Cl1 90.09(8)
C6 Si1 Cl1 118.73(12)
C5 Si1 Cl1 115.98(9)
O1 Si1 Cl2 174.35(7)
C6 Si1 Cl2 92.34(12)
C5 Si1 Cl2 83.63(11)
Cl1 Si1 Cl2 89.83(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 F2 1.313(4)
C1 F1 1.313(4)
C1 F3 1.327(4)
C1 C2 1.516(4)
C2 N1 1.281(3)
C2 O1 1.295(3)
O1 Si1 1.836(2)
N1 N2 1.467(3)
N2 C3 1.499(3)
N2 C4 1.500(3)
N2 C5 1.516(3)
C5 Si1 1.892(3)
Si1 C6 1.848(3)
Si1 Cl1 2.0756(11)
Si1 Cl2 2.3436(12)
