Synthesis, structures and photophysical properties of hexacoordinated organosilicon compounds with 2-(2-pyridyl)phenyl groups.
Furuta, Shohei; Mori, Toshiaki; Yoshigoe, Yusuke; Sekine, Kohei; Kuninobu, Yoichiro; Organic & biomolecular chemistry 18 (2020) 3239–3242; doi:10.1039/d0ob00484g

data_7157436
_publ_section_title
;
 Synthesis, structures and photophysical properties of hexacoordinated
 organosilicon compounds with 2-(2-pyridyl)phenyl groups.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3239
_journal_page_last               3242
_journal_paper_doi               10.1039/d0ob00484g
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C24 H14 F8 N2 Si'
_chemical_formula_sum            'C24 H14 F8 N2 Si'
_chemical_formula_weight         510.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                80.924(2)
_cell_angle_beta                 74.043(2)
_cell_angle_gamma                85.365(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8983(2)
_cell_length_b                   10.1395(3)
_cell_length_c                   14.2203(4)
_cell_measurement_reflns_used    10917
_cell_measurement_temperature    113
_cell_measurement_theta_max      31.0320
_cell_measurement_theta_min      2.3480
_cell_volume                     1080.40(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn70 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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   -110.00  70.00   0.50   16.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   16.00    --  -20.00  45.00 270.00  360
  3  \w   -110.00  70.00   0.50   16.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00 -20.00   0.50   16.00    --  -20.00  45.00  90.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0454821000
_diffrn_orient_matrix_UB_12      0.0617477000
_diffrn_orient_matrix_UB_13      -0.0095425000
_diffrn_orient_matrix_UB_21      0.0511822000
_diffrn_orient_matrix_UB_22      0.0316357000
_diffrn_orient_matrix_UB_23      0.0232196000
_diffrn_orient_matrix_UB_31      0.0636355000
_diffrn_orient_matrix_UB_32      0.0145825000
_diffrn_orient_matrix_UB_33      -0.0460011000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15251
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.036
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       prism
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4932
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.6158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4339
_reflns_number_total             4932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob00484g6.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7157434--7157436.cif.'
_cod_database_code               7157436
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.962
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F3-C23B \\sim F3-C23A
 with sigma of 0.02
 C4-C23B \\sim C4-C23A
 with sigma of 0.02
 F4A-C23B \\sim F4B-C23A
 with sigma of 0.02
 C23B-F5A \\sim C23A-F5B
 with sigma of 0.02
 F3-F4A \\sim F3-F4B
 with sigma of 0.04
 F3-F5A \\sim F3-F5B
 with sigma of 0.04
 C4-F4A \\sim C4-F4B
 with sigma of 0.04
 C4-F5A \\sim C4-F5B
 with sigma of 0.04
 F4A-F5A \\sim F4B-F5B
 with sigma of 0.04
3. Rigid bond restraints
 C23A, C23B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C23A \\sim C23B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Sof(C23A)=Sof(F5B)=Sof(F4B)=1-FVAR(1)
 Sof(F4A)=Sof(C23B)=Sof(F5A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C22(H22), C19(H19), C16(H16), C14(H14), C8(H8), C2(H2),
 C10(H10), C20(H20), C9(H9), C5(H5), C21(H21), C3(H3)
;
_shelx_res_checksum              86857
_shelx_hkl_checksum              77435
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.130
_oxdiff_exptl_absorpt_empirical_full_min 0.721