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

data_1567619
_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         'C55 H45 N5, 2(C H2 Cl2)'
_chemical_formula_sum            'C57 H49 Cl4 N5'
_chemical_formula_weight         945.81
_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
_atom_sites_solution_primary     dual
_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                 113.674(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0926(14)
_cell_length_b                   16.4670(12)
_cell_length_c                   17.5046(13)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.47
_cell_volume                     4512.3(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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.1167
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            98282
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.183
_diffrn_reflns_theta_min         2.153
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1220 before and 0.0734 after correction.
The Ratio of minimum to maximum transmission is 0.9467.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       needle
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         10026
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.0789
_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^)+(0.0428P)^2^+13.4405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6498
_reflns_number_total             10026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04006a2.cif
_cod_data_source_block           f1_a
_cod_depositor_comments
'Adding full bibliography for 1567617--1567621.cif.'
_cod_database_code               1567619
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.943
_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. Restrained distances
 Cl3-C28 \\sim Cl3A-C28A
 with sigma of 0.02
 Cl1-C28 \\sim Cl1A-C28A
 with sigma of 0.02
 Cl3-Cl1 \\sim Cl3A-Cl1A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 Cl1, Cl3, C28, H28A, H28B, Cl3A, C28A, H28D, Cl1A, H28C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(Cl3A)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl1)=Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C013(H01A,H01B), C014(H01C,H01D), C01H(H01E,H01F), C01I(H01G,H01H), C01J(H01I,
 H01J), C01M(H01K,H01L), C01O(H01P,H01Q), C01Q(H01U,H01V), C29(H29A,H29B),
 C28(H28A,H28B), C28A(H28C,H28D)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C6(H6), C43(H43), C19(H19), C41(H41), C20(H20), C36(H36), C14(H14),
 C17(H17), C16(H16), C34(H34), C13(H13), C12(H12), C42(H42), C35(H35), C38(H38),
  C39(H39)
5.c Idealised Me refined as rotating group:
 C01N(H01M,H01N,H01O), C01P(H01R,H01S,H01T), C01R(H01W,H01X,H01Y), C01S(H01Z,H,
 HA)
;
_shelx_res_checksum              16258
_shelx_hkl_checksum              6995
_olex2_submission_special_instructions 'No special instructions were received'