Three-Component Regio- and Stereoselective Polymerizations toward Functional Chalcogen-Rich Polymers with AIE-Activities.
Gao, Qingqing; Xiong, Ling-Hong; Han, Ting; Qiu, Zijie; He, Xuewen; Sung, Herman H. Y.; Kwok, Ryan T. K.; Williams, Ian D.; Lam, Jacky W. Y.; Tang, Ben Zhong; Journal of the American Chemical Society 141 (2019) 14712–14719; doi:10.1021/jacs.9b06493

data_4127615
_publ_section_title
;
 Three-Component Regio- and Stereoselective Polymerizations toward
 Functional Chalcogen-Rich Polymers with AIE-Activities.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14712
_journal_page_last               14719
_journal_paper_doi               10.1021/jacs.9b06493
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C20 H16 O2 S Se'
_chemical_formula_sum            'C20 H16 O2 S Se'
_chemical_formula_weight         399.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.278(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9736(3)
_cell_length_b                   5.31980(10)
_cell_length_c                   20.0252(4)
_cell_measurement_reflns_used    2686
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.6320
_cell_measurement_theta_min      4.4450
_cell_volume                     1691.46(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    100.00 165.00   1.00    3.00    --  110.57 111.00-150.00   65
  2  \w    -70.00  31.00   1.00    1.00    --  -40.20  57.00 -30.00  101
  3  \w    -95.00  -2.00   1.00    1.00    --  -40.20 125.00   0.00   93
  4  \w     94.00 175.00   1.00    3.00    --  110.57  77.00 -90.00   81
  5  \w     91.00 157.00   1.00    3.00    --  110.57  45.00   0.00   66
  6  \w     61.00 100.00   1.00    3.00    --  110.57 -94.00 120.00   39
  7  \w     40.00 138.00   1.00    3.00    --  110.57 -45.00 120.00   98
  8  \w     76.00 108.00   1.00    3.00    --  110.57 -94.00-180.00   32
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0212890000
_diffrn_orient_matrix_UB_12      0.2778000000
_diffrn_orient_matrix_UB_13      0.0118935000
_diffrn_orient_matrix_UB_21      -0.0088021000
_diffrn_orient_matrix_UB_22      -0.0586805000
_diffrn_orient_matrix_UB_23      0.0743378000
_diffrn_orient_matrix_UB_31      0.0941020000
_diffrn_orient_matrix_UB_32      0.0573467000
_diffrn_orient_matrix_UB_33      0.0183711000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4902
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.416
_diffrn_reflns_theta_min         4.443
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2989
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.1448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2668
_reflns_number_total             2989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06493_si_002.cif
_cod_data_source_block           gao2cult
_cod_database_code               4127615
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.816
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C12-C11 \\sim C13-C12 \\sim C14-C13 \\sim C15-C14 \\sim C16-C15 \\sim C16-C11
 with sigma of 0.02
 C12A-C11A \\sim C13A-C12A \\sim C14A-C13A \\sim C15A-C14A \\sim C16A-C15A
\\sim C16A-C11A
 with sigma of 0.02
3. Restrained planarity
 C11, C12, C13, C14, C15, C16
 with sigma of 0.02
 C11A, C12A, C13A, C14A, C15A, C16A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C35)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C16A) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 C11, C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11A, C12A, C13A, C14A, C15A, C16A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C11(0.5) C11A(0.5) C12(0.5) H12(0.5) C12A(0.5) H12A(0.5) C13(0.5)
 H13(0.5) C13A(0.5) H13A(0.5) C14(0.5) H14(0.5) C14A(0.5) H14A(0.5) C15(0.5)
 H15(0.5) C15A(0.5) H15A(0.5) C16(0.5) H16(0.5) C16A(0.5) H16A(0.5) C32(0.5)
 H32(0.5) C32A(0.5) H32A(0.5) C33(0.5) H33(0.5) C33A(0.5) H33A(0.5) H34(0.5)
 H34A(0.5) C35(0.5) H35(0.5) C35A(0.5) H35A(0.5) C36(0.5) H36(0.5) C36A(0.5)
 H36A(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C12(H12), C12A(H12A), C13(H13), C13A(H13A), C14(H14), C14A(H14A),
 C15(H15), C15A(H15A), C16(H16), C16A(H16A), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C34(H34),
 C34(H34A), C35(H35), C35A(H35A), C36(H36), C36A(H36A)
;
_shelx_res_checksum              3816
_shelx_hkl_checksum              12556
_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 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.889