Sign inversions of circularly polarized luminescence for helical compounds by chemically fine-tuning operations.
Lin, Wei-Bin; He, Dong-Qiang; Lu, Hai-Yan; Hu, Zhi-Qiang; Chen, Chuan-Feng; Chemical communications (Cambridge, England) 56 (2020) 1863–1866; doi:10.1039/c9cc08573d

data_7126127
_publ_section_title
;
 Sign inversions of circularly polarized luminescence for helical
 compounds by chemically fine-tuning operations.
;
_journal_issue                   12
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1863
_journal_page_last               1866
_journal_paper_doi               10.1039/c9cc08573d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C40 H30 Cl2 O2'
_chemical_formula_sum            'C40 H30 Cl2 O2'
_chemical_formula_weight         613.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-22 deposited with the CCDC.	2020-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.676(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4619(3)
_cell_length_b                   16.5737(4)
_cell_length_c                   15.2124(3)
_cell_measurement_reflns_used    6852
_cell_measurement_temperature    299.9(3)
_cell_measurement_theta_max      74.9240
_cell_measurement_theta_min      4.0110
_cell_volume                     3052.89(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.952
_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    -17.00   8.00   0.50    0.50    --  -47.20  39.00 156.00   50
  2  \w    -96.00 -34.00   0.50    0.50    --  -47.20 -39.00   2.00  124
  3  \w     52.00 115.00   0.50    0.50    --   47.20  39.00 156.00  126
  4  \w    -10.00  60.00   0.50    0.50    --   47.20 -39.00   2.00  140
  5  \w    -93.00 -68.00   0.50    1.50    --  -99.00  39.00 156.00   50
  6  \w   -151.00-126.00   0.50    1.50    --  -99.00 -39.00   2.00   50
  7  \w     91.00 155.00   0.50    1.50    --  103.25  39.00 156.00  128
  8  \w     31.00 116.00   0.50    1.50    --  103.25 -39.00   2.00  170
  9  \w     16.00  95.00   0.50    0.50    --   47.20-125.00-120.00  158
 10  \w   -112.00 -29.00   0.50    1.50    --  -99.00  30.00 -30.00  166
 11  \w   -111.00 -28.00   0.50    1.50    --  -99.00  45.00   0.00  166
 12  \w   -167.00 -88.00   0.50    1.50    --  -99.00 -30.00  30.00  158
 13  \w     34.00  60.00   0.50    1.50    --  103.25 -45.00 150.00   52
 14  \w    111.00 169.00   0.50    1.50    --  103.25  45.00 -90.00  116
 15  \w     93.00 130.00   0.50    1.50    --  103.25  45.00-150.00   74
 16  \w     60.00  96.00   0.50    1.50    --  103.25 -94.00-150.00   72
 17  \w     72.00 108.00   0.50    1.50    --  103.25 -45.00 150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0242594000
_diffrn_orient_matrix_UB_12      -0.0046470000
_diffrn_orient_matrix_UB_13      0.0946419000
_diffrn_orient_matrix_UB_21      0.1099481000
_diffrn_orient_matrix_UB_22      -0.0447333000
_diffrn_orient_matrix_UB_23      0.0357556000
_diffrn_orient_matrix_UB_31      0.0591755000
_diffrn_orient_matrix_UB_32      0.0813505000
_diffrn_orient_matrix_UB_33      0.0251909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10170
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.317
_diffrn_reflns_theta_min         4.007
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0717P)^2^+1.4868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2635
_reflns_number_total             3000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08573d2.cif
_cod_data_source_block           tx1102
_cod_database_code               7126127
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOCl
_reflns_odcompleteness_completeness 99.31
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C9(H9), C10(H10), C15(H15), C16(H16), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              34043
_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 1.439
_oxdiff_exptl_absorpt_empirical_full_min 0.872