#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:55:14 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229992 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045594.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_7045594
loop_
_publ_author_name
'Durka, Krzysztof'
'Urban, Mateusz'
'Czub, Maja'
'Dąbrowski, Marek'
'Tomaszewski, Patryk'
'Luliński, Sergiusz'
_publ_section_title
;
 An intramolecular ortho-assisted activation of the silicon-hydrogen bond
 in arylsilanes: an experimental and theoretical study.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3705
_journal_page_last               3716
_journal_paper_doi               10.1039/c7dt04858k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C9 H9 F O2 Si'
_chemical_formula_weight         196.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-10-24 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.265(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2067(7)
_cell_length_b                   7.1378(3)
_cell_length_c                   7.5388(3)
_cell_measurement_reflns_used    5712
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.9840
_cell_measurement_theta_min      2.4390
_cell_volume                     911.08(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10042
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.364
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0831P)²+0.3748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1584
_reflns_number_total             1797
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04858k2.cif
_cod_data_source_block           COSi
_cod_depositor_comments
'Adding full bibliography for 7045594--7045595.cif.'
_cod_database_code               7045594
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Si Si 0.10379(2) 0.0000 0.20607(5) 0.01320(13) Uani 1 2 d S T P
O2 O 0.07888(6) 0.0000 -0.02322(14) 0.0165(2) Uani 1 2 d S T P
O1 O 0.12991(7) 0.0000 -0.27675(15) 0.0210(2) Uani 1 2 d S T P
F1 F 0.27849(6) 0.0000 0.49440(12) 0.0258(2) Uani 1 2 d S T P
C4 C 0.35510(9) 0.0000 0.2648(2) 0.0177(3) Uani 1 2 d S T P
H4 H 0.4021 0.0000 0.3528 0.021 Uiso 1 2 calc R U P
C7 C 0.14038(8) 0.0000 -0.11456(19) 0.0149(3) Uani 1 2 d S T P
C8 C 0.06856(6) 0.21344(14) 0.30355(14) 0.0182(2) Uani 1 1 d . . .
H8A H 0.0882 0.3239 0.2482 0.027 Uiso 1 1 calc R U .
H8B H 0.0881 0.2153 0.4339 0.027 Uiso 1 1 calc R U .
H8C H 0.0107 0.2147 0.2805 0.027 Uiso 1 1 calc R U .
C6 C 0.29001(9) 0.0000 -0.0483(2) 0.0163(3) Uani 1 2 d S T P
H6 H 0.2925 0.0000 -0.1732 0.020 Uiso 1 2 calc R U P
C2 C 0.21152(8) 0.0000 0.19340(18) 0.0141(2) Uani 1 2 d S T P
C5 C 0.35850(9) 0.0000 0.0816(2) 0.0175(3) Uani 1 2 d S T P
H5 H 0.4085 0.0000 0.0446 0.021 Uiso 1 2 calc R U P
C3 C 0.28138(9) 0.0000 0.31625(19) 0.0167(3) Uani 1 2 d S T P
C1 C 0.21761(8) 0.0000 0.01058(18) 0.0135(2) Uani 1 2 d S T P
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'
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'
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
O2 Si C8 111.32(4) . .
O2 Si C8 111.32(4) . 6
C8 Si C8 111.75(6) . 6
O2 Si C2 91.17(5) . .
C8 Si C2 114.82(4) . .
C8 Si C2 114.82(4) 6 .
C7 O2 Si 115.80(9) . .
C5 C4 C3 118.55(13) . .
C5 C4 H4 120.7 . .
C3 C4 H4 120.7 . .
O1 C7 O2 121.64(13) . .
O1 C7 C1 126.86(13) . .
O2 C7 C1 111.50(11) . .
Si C8 H8A 109.5 . .
Si C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C5 C6 C1 117.92(13) . .
C5 C6 H6 121.0 . .
C1 C6 H6 121.0 . .
C3 C2 C1 116.82(12) . .
C3 C2 Si 135.81(10) . .
C1 C2 Si 107.36(10) . .
C6 C5 C4 121.19(13) . .
C6 C5 H5 119.4 . .
C4 C5 H5 119.4 . .
F1 C3 C2 118.96(12) . .
F1 C3 C4 118.26(13) . .
C2 C3 C4 122.78(13) . .
C6 C1 C2 122.74(13) . .
C6 C1 C7 123.09(12) . .
C2 C1 C7 114.16(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si O2 1.7051(11) .
Si C8 1.8404(10) .
Si C8 1.8405(10) 6
Si C2 1.8731(14) .
O2 C7 1.3615(16) .
O1 C7 1.2038(17) .
F1 C3 1.3528(16) .
C4 C5 1.393(2) .
C4 C3 1.391(2) .
C4 H4 0.9500 .
C7 C1 1.486(2) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C6 C5 1.392(2) .
C6 C1 1.3951(19) .
C6 H6 0.9500 .
C2 C3 1.381(2) .
C2 C1 1.4007(18) .
C5 H5 0.9500 .
