Chiral cyclic architectonics with tetraphenylethylenes: conformation immobilization, optical resolution and circularly polarized luminescence
Meng, Qi; Cui, Liwen; Liao, Qi; Xu, Jian; Wang, Yuxiang; Chemical Communications  (2022) –; doi:10.1039/D2CC04139A

data_7130558
_publ_section_title
;
 Chiral cyclic architectonics with tetraphenylethylenes: conformation
 immobilization, optical resolution and circularly polarized luminescence
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04139A
_journal_year                    2022
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '0.5(C H2 Cl2), C48 H34 O2'
_chemical_formula_sum            'C48.5 H35 Cl O2'
_chemical_formula_weight         685.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-29 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7146(7)
_cell_length_b                   9.8698(5)
_cell_length_c                   25.4906(12)
_cell_measurement_reflns_used    5379
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.203
_cell_measurement_theta_min      2.505
_cell_volume                     3608.9(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.1207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38856
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_min         1.914
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1614 before and 0.0740 after correction. The Ratio of minimum to maximum transmission is 0.7520. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.656
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 2504 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         12767
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0829
_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^)+(0.1253P)^2^+2.7386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2438
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                8400
_reflns_number_total             12767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04139a2.cif
_cod_data_source_block           12081_0m
_cod_depositor_comments
;

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C97 H70 Cl2 O4'
_cod_original_formula_weight         1370.43
_cod_original_formula_moiety         'C H2 Cl2, 2(C48 H34 O2)'
_cod_original_formula_units_Z            2
_cod_database_code               7130558
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.981
_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:
 C84(H84A,H84B), C63(H63A,H63B), C21(H21A,H21B), C42(H42A,H42B), C49(H49A,H49B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C14(H14), C16(H16), C29(H29), C93(H93), C6(H6), C94(H94), C79(H79),
 C48(H48), C17(H17), C5(H5), C90(H90), C51(H51), C89(H89), C4(H4), C23(H23),
 C55(H55), C3(H3), C59(H59), C58(H58), C34(H34), C87(H87), C24(H24), C20(H20),
 C81(H81), C2(H2), C85(H85), C76(H76), C97(H97), C61(H61), C39(H39), C66(H66),
 C13(H13), C82(H82), C53(H53), C45(H45), C28(H28), C10(H10), C95(H95), C47(H47),
  C65(H65), C44(H44), C40(H40), C77(H77), C26(H26), C54(H54), C78(H78),
 C62(H62), C12(H12), C96(H96), C52(H52), C35(H35), C71(H71), C27(H27), C37(H37),
  C70(H70), C36(H36), C11(H11), C68(H68), C69(H69)
;
_olex2_submission_special_instructions 'No special instructions were received'