Chalcogen-Chalcogen Bonding Catalysis Enables Assembly of Discrete Molecules.
Wang, Wei; Zhu, Haofu; Liu, Shuya; Zhao, Zhiguo; Zhang, Liang; Hao, Jingcheng; Wang, Yao; Journal of the American Chemical Society 141 (2019) 9175–9179; doi:10.1021/jacs.9b03806

data_4128715
_publ_section_title
;
 Chalcogen-Chalcogen Bonding Catalysis Enables Assembly of Discrete
 Molecules.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9175
_journal_page_last               9179
_journal_paper_doi               10.1021/jacs.9b03806
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C21 H21 N O3'
_chemical_formula_sum            'C21 H21 N O3'
_chemical_formula_weight         335.39
_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     direct
_audit_creation_date             2019-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.236(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5790(4)
_cell_length_b                   17.1831(3)
_cell_length_c                   11.6372(5)
_cell_measurement_reflns_used    5028
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      75.7030
_cell_measurement_theta_min      4.8440
_cell_volume                     1746.62(14)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.908
_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   -118.00 -81.00   1.00    0.50    --  -48.45-164.00-141.00   37
  2  \w    -78.00 -45.00   1.00    0.50    --  -48.45-164.00-141.00   33
  3  \w    -49.00  -3.00   1.00    0.50    --  -48.45 116.00  95.00   46
  4  \w     72.00 120.00   1.00    0.50    --   48.45 164.00-116.00   48
  5  \w     59.00  92.00   1.00    0.50    --   48.45-116.00   7.00   33
  6  \w   -142.00-117.00   1.00    6.00    --  -86.25-116.00   7.00   25
  7  \w    -66.00 -31.00   1.00    6.00    --  -86.25 164.00-116.00   35
  8  \w     35.00 113.00   1.00    6.00    --  106.49-116.00   7.00   78
  9  \w    114.00 139.00   1.00    6.00    --  106.49 116.00  95.00   25
 10  \w     77.00 144.00   1.00    6.00    --  106.49-164.00-141.00   67
 11  \w   -120.00 -70.00   1.00    0.50    --  -48.45-125.00 150.00   50
 12  \w   -119.00 -70.00   1.00    0.50    --  -48.45-125.00  60.00   49
 13  \w   -119.00 -94.00   1.00    6.00    --  -86.25-164.00-141.00   25
 14  \w     32.00  85.00   1.00    6.00    --  106.49 -15.00 -60.00   53
 15  \w     33.00 114.00   1.00    6.00    --  106.49 -30.00   0.00   81
 16  \w     98.00 163.00   1.00    6.00    --  106.49  15.00 120.00   65
 17  \w     89.00 118.00   1.00    6.00    --  106.49 -15.00 -60.00   29
 18  \w     35.00 119.00   1.00    6.00    --  106.49 -45.00 -30.00   84
;
_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      -0.1080720000
_diffrn_orient_matrix_UB_12      -0.0606464000
_diffrn_orient_matrix_UB_13      -0.0906870000
_diffrn_orient_matrix_UB_21      0.0202639000
_diffrn_orient_matrix_UB_22      0.0391371000
_diffrn_orient_matrix_UB_23      -0.1113238000
_diffrn_orient_matrix_UB_31      0.1379311000
_diffrn_orient_matrix_UB_32      -0.0531831000
_diffrn_orient_matrix_UB_33      0.0213486000
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10061
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         4.898
_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    0.684
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79605
_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    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.4580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2375
_reflns_number_total             2836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03806_si_006.cif
_cod_data_source_block           190124c
_cod_original_cell_volume        1746.60(13)
_cod_database_code               4128715
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 90.42
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C3(H3), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C12(H12), C11(H11), C14(H14)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              58279
_shelx_hkl_checksum              32069
_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 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.658