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_4514786
_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         'C16 H12 N2'
_chemical_formula_sum            'C16 H12 N2'
_chemical_formula_weight         232.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-12-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5559(5)
_cell_length_b                   13.9087(12)
_cell_length_c                   11.4271(7)
_cell_measurement_reflns_used    1825
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.2210
_cell_measurement_theta_min      4.9540
_cell_volume                     1200.91(15)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.939
_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    -70.00 -14.00   1.00    0.65    --  -86.25 125.00 -56.00   56
  2  \w     93.00 119.00   1.00    0.10    --   48.45  29.00-115.00   26
  3  \w    104.00 163.00   1.00    0.65    --  107.75  95.00  51.00   59
  4  \w     44.00  88.00   1.00    0.65    --  107.75 -29.00  83.00   44
  5  \w     31.00  90.00   1.00    0.10    --   48.45-125.00 150.00   59
  6  \w    103.00 168.00   1.00    0.65    --  107.75  37.00  30.00   65
  7  \w     54.00 105.00   1.00    0.65    --  107.75 -99.00 -60.00   51
  8  \w   -107.00 -70.00   1.00    0.10    --  -48.45-125.00 -90.00   37
  9  \w   -116.00 -72.00   1.00    0.10    --  -48.45-125.00  30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0178687000
_diffrn_orient_matrix_UB_12      -0.1250877000
_diffrn_orient_matrix_UB_13      -0.0403334000
_diffrn_orient_matrix_UB_21      -0.2024451000
_diffrn_orient_matrix_UB_22      0.0075609000
_diffrn_orient_matrix_UB_23      0.0108357000
_diffrn_orient_matrix_UB_31      -0.0144640000
_diffrn_orient_matrix_UB_32      0.0499023000
_diffrn_orient_matrix_UB_33      -0.1026092000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3443
_diffrn_reflns_point_group_measured_fraction_full 0.770
_diffrn_reflns_point_group_measured_fraction_max 0.716
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.881
_diffrn_reflns_theta_min         5.009
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40257
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Flack x determined using 406 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.791
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1806
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.790
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.1656
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3673
_refine_ls_wR_factor_ref         0.3940
_reflns_Friedel_coverage         0.452
_reflns_Friedel_fraction_full    0.524
_reflns_Friedel_fraction_max     0.470
_reflns_number_gt                1619
_reflns_number_total             1806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b01929_si_002.cif
_cod_data_source_block           20180618-wwl-2
_cod_database_code               4514786
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C N H'
_reflns_odcompleteness_completeness 99.14
_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, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8B,H8A)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C9(H9), C3(H3), C14(H14), C6(H6), C4(H4), C7(H7), C13(H13), C16(H16),
 C15(H15)
;
_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 2.709
_oxdiff_exptl_absorpt_empirical_full_min 0.430