Inducing configurational stability in inherently flexible expanded heterohelicenes and unlocking stimuli-responsive chiroptical switching
Pal, Manisha; Karak, Pirudhan; Hati, Debranjan; Giri, Mrityunjay; George, Subi J.; Choudhury, Joyanta; Chemical Science  (2026) –; doi:10.1039/D6SC02610A

data_1577092
_publ_section_title
;
 Inducing configurational stability in inherently flexible expanded
 heterohelicenes and unlocking stimuli-responsive chiroptical switching
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D6SC02610A
_journal_year                    2026
_chemical_formula_moiety         'C71 H77 N5, C H Cl'
_chemical_formula_sum            'C71 H77 Cl0.5 N5 O0.5'
_chemical_formula_weight         1026.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-09-04 deposited with the CCDC.	2026-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                79.736(12)
_cell_angle_beta                 78.645(9)
_cell_angle_gamma                66.662(10)
_cell_formula_units_Z            2
_cell_length_a                   13.162(3)
_cell_length_b                   14.991(4)
_cell_length_c                   16.491(4)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      2.25
_cell_volume                     2911.0(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            158115
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.127
_diffrn_reflns_theta_min         1.975
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1149 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.8878.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       needle
_exptl_crystal_F_000             1101
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.549
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         17080
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.1120
_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^)+(0.1406P)^2^+7.6485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3035
_refine_ls_wR_factor_ref         0.3218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13179
_reflns_number_total             17080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc02610a7.cif
_cod_data_source_block           final1_a
_cod_original_formula_sum        'C71 H77 Cl0.50 N5 O0.50'
_cod_database_code               1577092
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.997
_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
Uanis(C11) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C0AA(H1)
3.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C71(H71A,H71B), C67(H67A,H67B), C70(H70A,H70B), C63(H63A,
 H63B), C72(H72A,H72B), C64(H64A,H64B), C73(H73A,H73B)
3.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C26(H26), C58(H58), C8(H8), C43(H43), C22(H22), C19(H19), C39(H39),
 C21(H21), C33(H33), C31(H31), C38(H38), C41(H41)
3.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C69(H69A,H69B,H69C), C62(H62A,H62B,
 H62C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C), C68(H68A,H68B,H68C), C61(H61A,
 H61B,H61C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C47(H47A,H47B,H47C), C74(H74A,H74B,
 H74C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              19985
_shelx_fab_checksum              15037
_olex2_submission_special_instructions 'No special instructions were received'