Dual Chalcogen-Chalcogen Bonding Catalysis.
Wang, Wei; Zhu, Haofu; Feng, Lei; Yu, Qun; Hao, Jing-Cheng; Zhu, Rongxiu; Wang, Yao; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12610

data_4134093
_publ_section_title
;
 Dual Chalcogen-Chalcogen Bonding Catalysis.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12610
_journal_year                    2020
_chemical_formula_moiety         'C24 H20 P S, B F4'
_chemical_formula_sum            'C24 H20 B F4 P S'
_chemical_formula_weight         458.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.9880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0332(2)
_cell_length_b                   11.7530(2)
_cell_length_c                   16.0509(2)
_cell_measurement_reflns_used    7679
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8000
_cell_measurement_theta_min      4.4120
_cell_volume                     2264.52(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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   -112.00 -64.00   1.00    0.10    --  -48.45-137.00-116.00   48
  2  \w    -97.00 -49.00   1.00    0.10    --  -48.45 132.00 129.00   48
  3  \w   -120.00 -66.00   1.00    0.10    --  -48.45-132.00  60.00   54
  4  \w     43.00  68.00   1.00    0.10    --   48.45-132.00  60.00   25
  5  \w   -112.00 -69.00   1.00    1.00    --  -86.25-132.00  60.00   43
  6  \w   -158.00-115.00   1.00    1.00    --  -86.25-132.00  60.00   43
  7  \w   -121.00 -96.00   1.00    1.00    --  -86.25-137.00-116.00   25
  8  \w     36.00 122.00   1.00    1.00    --  106.49-132.00  60.00   86
  9  \w     89.00 124.00   1.00    1.00    --  106.49-137.00-116.00   35
 10  \w   -120.00 -33.00   1.00    0.10    --  -48.45 -57.00  60.00   87
 11  \w     34.00 120.00   1.00    1.00    --  106.49 -57.00  30.00   86
 12  \w     92.00 156.00   1.00    1.00    --  106.49 125.00 -30.00   64
 13  \w     33.00  60.00   1.00    1.00    --  106.49 -19.00-150.00   27
 14  \w     64.00 118.00   1.00    1.00    --  106.49 -19.00-150.00   54
 15  \w     45.00 118.00   1.00    1.00    --  106.49 -38.00-180.00   73
 16  \w     93.00 118.00   1.00    1.00    --  106.49 132.00 129.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0686418000
_diffrn_orient_matrix_UB_12      0.0111541000
_diffrn_orient_matrix_UB_13      -0.0771259000
_diffrn_orient_matrix_UB_21      0.0034098000
_diffrn_orient_matrix_UB_22      -0.1305726000
_diffrn_orient_matrix_UB_23      -0.0079538000
_diffrn_orient_matrix_UB_31      -0.1083493000
_diffrn_orient_matrix_UB_32      0.0029627000
_diffrn_orient_matrix_UB_33      -0.0569950000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12637
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         4.447
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
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    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0818
_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^)+(0.0673P)^2^+5.7598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3476
_reflns_number_total             4000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12610_si_003.cif
_cod_data_source_block           190929a
_cod_database_code               4134093
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     CPS
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.656
_reflns_odcompleteness_completeness 98.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F4A \\sim B1:
within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
3. Others
 Fixed Sof: F1(0.5) F1A(0.5) F2(0.5) F2A(0.5) F3(0.5) F3A(0.5) F4(0.5) F4A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              27368
_shelx_hkl_checksum              98688
_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 1.543
_oxdiff_exptl_absorpt_empirical_full_min 0.738