Synthesis and characterisation of new silicon–perfluoropropenyl compounds
Alluhaibi, Lulu; Brisdon, Alan; Klejna, Sylwia; Muneer, Abeer; RSC Advances 13 (2023) 13547–13555; doi:10.1039/D3RA01353G

data_7246728
_publ_section_title
;
 Synthesis and characterisation of new silicon--perfluoropropenyl
 compounds
;
_journal_issue                   20
_journal_name_full               'RSC Advances'
_journal_page_first              13547
_journal_page_last               13555
_journal_paper_doi               10.1039/D3RA01353G
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C18 H10 F10 Si'
_chemical_formula_sum            'C18 H10 F10 Si'
_chemical_formula_weight         444.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                81.603(8)
_cell_angle_beta                 88.316(7)
_cell_angle_gamma                63.297(9)
_cell_formula_units_Z            2
_cell_length_a                   9.4952(8)
_cell_length_b                   10.2127(10)
_cell_length_c                   10.9000(9)
_cell_measurement_reflns_used    2764
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      26.8660
_cell_measurement_theta_min      3.7650
_cell_volume                     933.35(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -2.00 126.00   1.00   21.95    --   33.26  57.00 -30.00  128
  2  \w     79.00 105.00   1.00   21.95    --   33.26  57.00-180.00   26
  3  \w     -8.00  92.00   1.00    5.49    --    0.47  57.00-150.00  100
  4  \w     13.00  39.00   1.00   21.95    --  -32.32-125.00-150.00   26
  5  \w     -4.00  93.00   1.00   21.95    --   33.26 -99.00  90.00   97
  6  \w    -19.00 128.00   1.00   21.95    --   33.26  77.00  30.00  147
  7  \w    -10.00  16.00   1.00   21.95    --   33.26  57.00-180.00   26
  8  \w    -41.00   0.00   1.00    5.49    --    0.47  57.00-180.00   41
  9  \w   -127.00-101.00   1.00   21.95    --  -32.32 -99.00-120.00   26
 10  \w    -86.00 -61.00   1.00    5.49    --    0.47-178.00 -60.00   25
 11  \w    -60.00  88.00   1.00   21.95    --   33.26 -57.00 120.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0356785000
_diffrn_orient_matrix_UB_12      -0.0378792000
_diffrn_orient_matrix_UB_13      -0.0263807000
_diffrn_orient_matrix_UB_21      -0.0118705000
_diffrn_orient_matrix_UB_22      0.0471886000
_diffrn_orient_matrix_UB_23      -0.0573539000
_diffrn_orient_matrix_UB_31      0.0747666000
_diffrn_orient_matrix_UB_32      -0.0501928000
_diffrn_orient_matrix_UB_33      -0.0186733000
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7301
_diffrn_reflns_theta_full        25.9998
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.23
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5810
_exptl_crystal_description       irregular
_exptl_crystal_F_000             444.5991
_exptl_crystal_preparation
'the complex has be prepared from reaction between Ph2SiCl2 and CF3CF=CFLi'
_exptl_crystal_recrystallization_method
'slow evaporation of achloroform solution'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.5058
_refine_diff_density_min         -0.3793
_refine_diff_density_rms         0.0873
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.2980
_refine_ls_goodness_of_fit_ref   1.0478
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0478
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.6045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2932
_reflns_number_total             3668
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ra01353g2.cif
_cod_data_source_block           argp494
_cod_original_cell_volume        933.36(16)
_cod_database_code               7246728
_chemical_oxdiff_formula         C18H10Si1F10Cl
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C11(H11), C12(H12), C15(H15), C8(H8), C9(H9), C18(H18), C10(H10),
 C17(H17), C14(H14)
;
_olex2_date_sample_data_collection 2015-12-20
_olex2_exptl_crystal_mounting_method 'less than 1 mg'
_olex2_submission_original_sample_id argp494
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.600
_oxdiff_exptl_absorpt_empirical_full_min 0.437