Involving Single-Atom Silver(0) in Selective Dehalogenation by AgF under Visible-Light Irradiation
Wu, Wenli; Cui, Enxin; Zhang, Yun; Zhang, Chen; Zhu, Feng; Tung, Chen-Ho; Wang, Yifeng; ACS Catalysis 9 (2019) 6335–; doi:10.1021/acscatal.9b01929

data_4514787
_publ_section_title
;
 Involving Single-Atom Silver(0) in Selective Dehalogenation by AgF under
 Visible-Light Irradiation
;
_journal_issue                   7
_journal_name_full               'ACS Catalysis'
_journal_page_first              6335
_journal_paper_doi               10.1021/acscatal.9b01929
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C8 H6 N'
_chemical_formula_sum            'C8 H6 N'
_chemical_formula_weight         116.14
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.593(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8048(3)
_cell_length_b                   5.9454(3)
_cell_length_c                   13.2408(5)
_cell_measurement_reflns_used    1495
_cell_measurement_temperature    172.98(10)
_cell_measurement_theta_max      75.4910
_cell_measurement_theta_min      6.4370
_cell_volume                     613.78(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.943
_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    -62.00 -37.00   1.00    0.10    --  -86.25 142.00-137.00   25
  2  \w    -96.00 -23.00   1.00    0.10    --  -48.45 142.00-137.00   73
  3  \w     37.00 123.00   1.00    0.10    --  107.75 -57.00 -60.00   86
  4  \w    110.00 135.00   1.00    0.10    --  107.75 128.00  51.00   25
  5  \w   -118.00 -26.00   1.00    0.10    --  -48.45 -77.00  90.00   92
  6  \w   -105.00 -70.00   1.00    0.10    --  -86.25-128.00 -23.00   35
  7  \w   -120.00 -72.00   1.00    0.10    --  -48.45-128.00 -23.00   48
  8  \w    -86.00 -61.00   1.00    0.10    --  -48.45-142.00 165.00   25
  9  \w   -158.00 -83.00   1.00    0.10    --  -86.25 -99.00-120.00   75
 10  \w     56.00  81.00   1.00    0.10    --   48.45-142.00 165.00   25
 11  \w     42.00 129.00   1.00    0.10    --  107.75-142.00 165.00   87
 12  \w     58.00 122.00   1.00    0.10    --  107.75-128.00 -23.00   64
 13  \w     96.00 134.00   1.00    0.10    --  107.75  37.00 -30.00   38
 14  \w    153.00 178.00   1.00    0.10    --  107.75  37.00 -30.00   25
 15  \w     86.00 174.00   1.00    0.10    --  107.75  77.00 120.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0362116000
_diffrn_orient_matrix_UB_12      -0.2510083000
_diffrn_orient_matrix_UB_13      -0.0181512000
_diffrn_orient_matrix_UB_21      -0.1650859000
_diffrn_orient_matrix_UB_22      -0.0629898000
_diffrn_orient_matrix_UB_23      0.0530070000
_diffrn_orient_matrix_UB_31      -0.1023929000
_diffrn_orient_matrix_UB_32      0.0124601000
_diffrn_orient_matrix_UB_33      -0.1021084000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3467
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.353
_diffrn_reflns_theta_min         6.458
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
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    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0823P)^2^+0.1821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                987
_reflns_number_total             1219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b01929_si_004.cif
_cod_data_source_block           exp_283
_cod_database_code               4514787
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C N H '
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C2(H2), C6(H6)
;
_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 1.641
_oxdiff_exptl_absorpt_empirical_full_min 0.562