#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:54:14 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179268 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318807.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_4318807
loop_
_publ_author_name
'Alexander A. Kolomeitsev'
'German Bissky'
'Jan Barten'
'Natalya Kalinovich'
'Enno Lork'
'Gerd-Volker Röschenthaler'
_publ_section_title
;
 Hexaalkylguanidinium and 2-(Dialkylamino)-1,3-dimethylimidazolinium
 Trimethyldifluorosiliconates and Perfluoroalkoxides. Accidental Isolation
 and Molecular Structure of [C(NMe2)3]+F-.6CH2Cl2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6118
_journal_page_last               6124
_journal_paper_doi               10.1021/ic020081v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C12 H29 F2 N3 Si'
_chemical_formula_weight         281.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 96.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.135(2)
_cell_length_b                   8.600(2)
_cell_length_c                   10.580(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      1.65
_cell_volume                     825.0(3)
_computing_cell_refinement       'STOE Cell'
_computing_data_collection       'STOE Expose'
_computing_data_reduction        'STOE Integrate'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0829
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11447
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        'random variation +/-2.0'
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9278
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0496
_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)+(0.0804P)²+0.1455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                1195
_reflns_number_total             1621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020081v_1.cif
_cod_data_source_block           ak21i
_cod_database_code               4318807
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.2500 0.25697(11) 0.2500 0.0444(3) Uani 1 2 d S . .
F1 F 0.09519(16) 0.2563(2) 0.33602(14) 0.0583(4) Uani 1 1 d . . .
N1 N 0.1493(2) 0.3658(2) 0.68052(18) 0.0421(5) Uani 1 1 d . . .
N2 N 0.2500 0.1210(3) 0.7500 0.0437(6) Uani 1 2 d S . .
C1 C 0.1407(3) 0.3663(4) 0.1151(3) 0.0603(7) Uani 1 1 d . . .
H1A H 0.0354 0.3440 0.1148 0.084(3) Uiso 1 1 calc R . .
H1B H 0.1722 0.3333 0.0339 0.084(3) Uiso 1 1 calc R . .
H1C H 0.1577 0.4782 0.1266 0.084(3) Uiso 1 1 calc R . .
C2 C 0.2500 0.0386(5) 0.2500 0.0560(8) Uani 1 2 d S . .
H2A H 0.1778 0.0006 0.1808 0.084(3) Uiso 0.50 1 calc PR . .
H2B H 0.2238 0.0006 0.3316 0.084(3) Uiso 0.50 1 calc PR . .
H2C H 0.3484 0.0006 0.2376 0.084(3) Uiso 0.50 1 calc PR . .
C3 C 0.2500 0.2779(3) 0.7500 0.0386(6) Uani 1 2 d S . .
C4 C 0.0011(3) 0.3198(3) 0.6274(3) 0.0513(6) Uani 1 1 d . . .
H4A H -0.0005 0.2983 0.5363 0.084(3) Uiso 1 1 calc R . .
H4B H -0.0681 0.4041 0.6394 0.084(3) Uiso 1 1 calc R . .
H4C H -0.0277 0.2261 0.6709 0.084(3) Uiso 1 1 calc R . .
C5 C 0.1962(3) 0.5296(3) 0.6892(2) 0.0455(5) Uani 1 1 d . . .
H5A H 0.1117 0.5998 0.6963 0.057(4) Uiso 1 1 calc R . .
H5B H 0.2453 0.5606 0.6146 0.057(4) Uiso 1 1 calc R . .
C6 C 0.2021(3) 0.0330(3) 0.6325(2) 0.0459(5) Uani 1 1 d . . .
H6A H 0.1767 0.1065 0.5612 0.057(4) Uiso 1 1 calc R . .
H6B H 0.1125 -0.0276 0.6439 0.057(4) Uiso 1 1 calc R . .
C7 C 0.1781(3) -0.0764(3) 0.9001(2) 0.0568(6) Uani 1 1 d . . .
H7A H 0.2145 -0.1367 0.9761 0.084(3) Uiso 1 1 calc R . .
H7B H 0.1508 -0.1472 0.8286 0.084(3) Uiso 1 1 calc R . .
H7C H 0.0916 -0.0160 0.9168 0.084(3) 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
Si1 0.0424(5) 0.0487(5) 0.0428(5) 0.000 0.0073(3) 0.000
F1 0.0500(8) 0.0722(10) 0.0543(8) 0.0072(7) 0.0133(6) 0.0080(7)
N1 0.0409(9) 0.0396(9) 0.0439(10) 0.0006(8) -0.0021(7) 0.0010(7)
N2 0.0516(15) 0.0382(13) 0.0391(13) 0.000 -0.0031(11) 0.000
C1 0.0610(15) 0.0637(16) 0.0569(15) 0.0124(12) 0.0105(12) -0.0013(12)
C2 0.0544(19) 0.060(2) 0.0527(19) 0.000 0.0021(15) 0.000
C3 0.0393(14) 0.0393(15) 0.0374(14) 0.000 0.0050(11) 0.000
C4 0.0419(12) 0.0554(14) 0.0545(13) -0.0005(11) -0.0029(10) 0.0014(10)
C5 0.0511(12) 0.0395(11) 0.0457(12) 0.0034(9) 0.0052(10) 0.0032(9)
C6 0.0541(12) 0.0420(11) 0.0402(11) -0.0037(9) -0.0001(9) -0.0026(9)
C7 0.0700(16) 0.0512(14) 0.0492(13) 0.0011(11) 0.0078(11) -0.0064(12)
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'
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'
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
F1 Si1 F1 179.62(13) 2 . ?
F1 Si1 C2 89.81(6) 2 . ?
F1 Si1 C2 89.81(6) . . ?
F1 Si1 C1 89.72(10) 2 . ?
F1 Si1 C1 90.47(10) . . ?
C2 Si1 C1 119.83(10) . . ?
F1 Si1 C1 90.47(10) 2 2 ?
F1 Si1 C1 89.72(10) . 2 ?
C2 Si1 C1 119.83(10) . 2 ?
C1 Si1 C1 120.3(2) . 2 ?
C3 N1 C4 127.1(2) . . ?
C3 N1 C5 109.33(18) . . ?
C4 N1 C5 122.27(19) . . ?
C3 N2 C6 120.87(13) . . ?
C3 N2 C6 120.87(13) . 2_556 ?
C6 N2 C6 118.3(3) . 2_556 ?
N1 C3 N1 111.2(3) . 2_556 ?
N1 C3 N2 124.38(13) . . ?
N1 C3 N2 124.38(13) 2_556 . ?
N1 C5 C5 101.87(12) . 2_556 ?
N2 C6 C7 111.22(19) . 2_556 ?
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 F1 1.7725(15) 2 ?
Si1 F1 1.7725(15) . ?
Si1 C2 1.878(4) . ?
Si1 C1 1.890(3) . ?
Si1 C1 1.890(3) 2 ?
N1 C3 1.339(2) . ?
N1 C4 1.456(3) . ?
N1 C5 1.471(3) . ?
N2 C3 1.349(4) . ?
N2 C6 1.476(3) . ?
N2 C6 1.476(3) 2_556 ?
C3 N1 1.339(2) 2_556 ?
C5 C5 1.522(5) 2_556 ?
C6 C7 1.514(4) 2_556 ?
C7 C6 1.514(4) 2_556 ?
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
C4 N1 C3 N1 -158.3(3) . . . 2_556 ?
C5 N1 C3 N1 8.57(11) . . . 2_556 ?
C4 N1 C3 N2 21.7(3) . . . . ?
C5 N1 C3 N2 -171.43(11) . . . . ?
C6 N2 C3 N1 35.62(15) . . . . ?
C6 N2 C3 N1 -144.38(15) 2_556 . . . ?
C6 N2 C3 N1 -144.38(15) . . . 2_556 ?
C6 N2 C3 N1 35.62(15) 2_556 . . 2_556 ?
C3 N1 C5 C5 -21.0(3) . . . 2_556 ?
C4 N1 C5 C5 146.7(2) . . . 2_556 ?
C3 N2 C6 C7 122.96(17) . . . 2_556 ?
C6 N2 C6 C7 -57.04(17) 2_556 . . 2_556 ?
