Solvent and Temperature Effects on Dynamics and Chiroptical Properties of Propeller Chirality and Toroidal Interaction of Hexaarylbenzenes.
Kosaka, Tomoyo; Iwai, Satono; Inoue, Yoshihisa; Moriuchi, Toshiyuki; Mori, Tadashi; The journal of physical chemistry. A 122 (2018) 7455–7463; doi:10.1021/acs.jpca.8b06535

data_1552783
_publ_section_title
;
 Solvent and Temperature Effects on Dynamics and Chiroptical Properties of
 Propeller Chirality and Toroidal Interaction of Hexaarylbenzenes.
;
_journal_issue                   37
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              7455
_journal_page_last               7463
_journal_paper_doi               10.1021/acs.jpca.8b06535
_journal_volume                  122
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C54 H54 O6'
_chemical_formula_sum            'C54 H54 O6'
_chemical_formula_weight         798.97
_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             2018-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5859(3)
_cell_length_b                   20.1144(4)
_cell_length_c                   18.9328(4)
_cell_measurement_reflns_used    30720
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      60.06
_cell_measurement_theta_min      3.835
_cell_volume                     4389.44(17)
_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      123.15
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29775
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.917
_diffrn_reflns_theta_max         30.917
_diffrn_reflns_theta_min         3.214
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Abscore (Rigaku)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 902 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1095
_refine_ls_number_reflns         2735
_refine_ls_number_restraints     1740
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1283P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2214
_reflns_number_total             2735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp8b06535_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               1552783
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.914
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed X: C24(1.340549)
 Fixed Y: C3(0.549029)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C37(H37), C67(H67), C91(H91)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C38(H38A,H38B), C68(H68A,H68B), C92(H92A,H92B)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C18(H18), C19(H19), C21(H21), C22(H22),
 C25(H25), C26(H26), C28(H28), C29(H29), C32(H32), C33(H33), C35(H35), C36(H36),
  C42(H42), C43(H43), C45(H45), C46(H46), C49(H49), C50(H50), C52(H52),
 C53(H53), C62(H62), C63(H63), C65(H65), C66(H66), C72(H72), C73(H73), C75(H75),
  C76(H76), C79(H79), C80(H80), C82(H82), C83(H83), C86(H86), C87(H87),
 C89(H89), C90(H90), C96(H96), C97(H97), C99(H99), C100(H100), C103(H103),
 C104(H104), C106(H106), C107(H107)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C30(H30A,H30B,
 H30C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C54(H54A,
 H54B,H54C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C77(H77A,H77B,H77C),
 C84(H84A,H84B,H84C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C101(H10A,H10B,
 H10C), C108(H10D,H10E,H10F)
;
_olex2_submission_special_instructions 'No special instructions were received'