#------------------------------------------------------------------------------
#$Date: 2016-02-20 17:35:30 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/48/2214802.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214802
loop_
_publ_author_name
'Rutt, Oliver J.'
'Cowley, Andrew R.'
'Clarke, Simon J.'
_publ_section_title
;
 Bis(ethylamino)tetrafluorosilicon
;
_journal_coeditor_code           MG2025
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3406
_journal_page_last               o3406
_journal_paper_doi               10.1107/S1600536807032102
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C4 H14 F4 N2 Si'
_chemical_formula_moiety         'C4 H14 F4 N2 Si'
_chemical_formula_sum            'C4 H14 F4 N2 Si'
_chemical_formula_weight         194.25
_chemical_name_systematic
;
bis(ethylamine)tetrafluorosilicon
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.00
_cell_angle_beta                 99.655(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4788(4)
_cell_length_b                   6.9602(3)
_cell_length_c                   7.2206(4)
_cell_measurement_reflns_used    4140
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     420.08(4)
_computing_cell_refinement       DENZO
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ATOMS (Dowty, 2005)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4140
_diffrn_reflns_theta_full        27.464
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         5.692
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       plate
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0710
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         670
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000471
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)²]²
 Ai are:
 1.21 0.411 0.931
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0517
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0422
_reflns_number_gt                670
_reflns_number_total             946
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            mg2025.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2214802
_cod_database_fobs_code          2214802
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
loop_
_atom_site_type_symbol
_atom_site_label
_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
Si Si1 0.5000 0.5000 0.5000 0.0222 Uani 1.0000
F F1 0.54851(14) 0.26642(17) 0.51774(15) 0.0295 Uani 1.0000
F F2 0.65474(14) 0.55391(18) 0.66675(15) 0.0293 Uani 1.0000
N N1 0.6294(2) 0.5299(3) 0.3080(2) 0.0254 Uani 1.0000
C C1 0.7992(3) 0.4765(6) 0.3436(4) 0.0634 Uani 1.0000
C C2 0.8842(3) 0.5125(4) 0.1797(4) 0.0452 Uani 1.0000
H H1 0.595(4) 0.463(4) 0.219(5) 0.042(8) Uiso 1.0000
H H2 0.622(3) 0.638(5) 0.266(4) 0.038(7) Uiso 1.0000
H H11 0.8538 0.5527 0.4533 0.0774 Uiso 1.0000
H H12 0.8073 0.3365 0.3748 0.0774 Uiso 1.0000
H H21 0.9988 0.4730 0.2139 0.0559 Uiso 1.0000
H H22 0.8783 0.6524 0.1475 0.0559 Uiso 1.0000
H H23 0.8319 0.4361 0.0690 0.0559 Uiso 1.0000
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Si1 0.0300(4) 0.0208(4) 0.0167(3) 0.0004(3) 0.0061(2) -0.0001(3)
F1 0.0445(7) 0.0213(6) 0.0249(5) 0.0039(5) 0.0124(4) 0.0028(4)
F2 0.0316(6) 0.0361(7) 0.0200(6) -0.0021(5) 0.0035(4) -0.0027(5)
N1 0.0337(9) 0.0229(10) 0.0206(8) 0.0002(7) 0.0073(6) 0.0010(7)
C1 0.0404(13) 0.117(3) 0.0363(13) 0.0222(16) 0.0156(10) 0.0181(16)
C2 0.0438(12) 0.0520(15) 0.0439(14) -0.0004(12) 0.0199(10) -0.0006(11)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C   ' 0.0033 0.0016 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 International_Tables_Vol_IV_Table_2.2B
'F   ' 0.0171 0.0103 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0061 0.0033 International_Tables_Vol_IV_Table_2.2B
'Si  ' 0.0817 0.0704 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F1 Si1 F1 . 2_666 180. no
F1 Si1 F2 . . 90.56(6) yes
F1 Si1 F2 2_666 . 89.44(6) yes
F1 Si1 F2 . 2_666 89.44(6) no
F1 Si1 F2 2_666 2_666 90.56(6) no
F2 Si1 F2 . 2_666 180. no
F1 Si1 N1 . . 89.86(6) yes
F1 Si1 N1 2_666 . 90.14(6) no
F2 Si1 N1 . . 91.23(6) yes
F2 Si1 N1 2_666 . 88.77(6) no
F1 Si1 N1 . 2_666 90.14(6) no
F1 Si1 N1 2_666 2_666 89.86(6) no
F2 Si1 N1 . 2_666 88.77(6) no
F2 Si1 N1 2_666 2_666 91.23(6) no
N1 Si1 N1 . 2_666 180. no
Si1 N1 C1 . . 120.61(15) yes
Si1 N1 H1 . . 110(2) no
C1 N1 H1 . . 102(2) no
Si1 N1 H2 . . 111.(2) no
C1 N1 H2 . . 108.(2) no
H1 N1 H2 . . 104(3) no
N1 C1 C2 . . 113.9(2) yes
N1 C1 H11 . . 108.357 no
C2 C1 H11 . . 108.357 no
N1 C1 H12 . . 108.357 no
C2 C1 H12 . . 108.357 no
H11 C1 H12 . . 109.467 no
C1 C2 H21 . . 109.467 no
C1 C2 H22 . . 109.467 no
H21 C2 H22 . . 109.476 no
C1 C2 H23 . . 109.467 no
H21 C2 H23 . . 109.476 no
H22 C2 H23 . . 109.476 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 F1 . 1.6766(12) yes
Si1 F1 2_666 1.6766(12) no
Si1 F2 . 1.6679(11) yes
Si1 F2 2_666 1.6679(11) no
Si1 N1 . 1.9183(17) yes
Si1 N1 2_666 1.9183(17) no
N1 C1 . 1.467(3) yes
N1 H1 . 0.81(3) no
N1 H2 . 0.81(3) no
C1 C2 . 1.506(3) yes
C1 H11 . 1.000 no
C1 H12 . 1.000 no
C2 H21 . 1.000 no
C2 H22 . 1.000 no
C2 H23 . 1.000 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 F1 4_554 0.81(3) 2.15(3) 2.938(2) 165(3) yes
N1 H2 F2 4_564 0.81(3) 2.29(3) 3.091(2) 168(3) yes
