Conformationally flexible heterohelicenes as stimuli-controlled soft molecular springs
Karak, Pirudhan; Choudhury, Joyanta; Chemical Science 13 (2022) 11163–11173; doi:10.1039/D2SC04006A

data_1567618
_publ_section_title
;
 Conformationally flexible heterohelicenes as stimuli-controlled soft
 molecular springs
;
_journal_issue                   37
_journal_name_full               'Chemical Science'
_journal_page_first              11163
_journal_page_last               11173
_journal_paper_doi               10.1039/D2SC04006A
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C51 H45 N5'
_chemical_formula_sum            'C51 H45 N5'
_chemical_formula_weight         727.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-04-12 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.655(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4766(9)
_cell_length_b                   15.6816(16)
_cell_length_c                   28.099(2)
_cell_measurement_reflns_used    7654
_cell_measurement_temperature    140.01
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.45
_cell_volume                     3716.9(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      140.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1350
_diffrn_reflns_av_unetI/netI     0.1134
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            45331
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.452
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6676
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1274 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.8948.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_recrystallization_method 'slow evaporation of dichloromethane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0525P)^2^+1.9771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4308
_reflns_number_total             7602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04006a2.cif
_cod_data_source_block           final2_a
_cod_depositor_comments
'Adding full bibliography for 1567617--1567621.cif.'
_cod_original_cell_volume        3717.0(6)
_cod_database_code               1567618
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00B), C00S(H00C,H00D), C00W(H00E,H00F), C014(H01D,H01E), C016(H01F,
 H01G), C017(H01H,H01I), C01C(H01J,H01K), C01J(H01U,H01V)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C44(H44), C11(H11), C20(H20), C17(H17), C19(H19), C14(H14), C18(H18),
 C43(H43), C12(H12), C13(H13), C35(H35), C41(H41), C36(H36), C42(H42), C38(H38),
  C37(H37)
2.c Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C01D(H01L,H01M,H01N), C01E(H01O,H01P,H01Q), C01I(H01R,
 H01S,H01T)
;
_shelx_res_checksum              49480
_shelx_hkl_checksum              14325
_olex2_submission_special_instructions 'No special instructions were received'