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

data_1567617
_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         '2(C F3 O3 S), C57 H51 N5'
_chemical_formula_sum            'C59 H51 F6 N5 O6 S2'
_chemical_formula_weight         1104.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-15 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.116(7)
_cell_length_b                   17.029(5)
_cell_length_c                   16.379(8)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.24
_cell_volume                     5098(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.992
_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  0.0702
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58133
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.598
_diffrn_reflns_theta_min         2.229
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6944
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1141 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.9311.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6474
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0824P)^2^+8.8132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5069
_reflns_number_total             6474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04006a2.cif
_cod_data_source_block           f2_a
_cod_depositor_comments
'Adding full bibliography for 1567617--1567621.cif.'
_cod_database_code               1567617
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Restrained distances
 S001-O00M \\sim S0-O00N
 with sigma of 0.02
 S001-O00S \\sim S0-O00T
 with sigma of 0.02
 C013-O1 \\sim C0-O1A
 with sigma of 0.04
 S001-C013 \\sim S0-C0
 with sigma of 0.02
 S001-O1 \\sim S0-O1A
 with sigma of 0.02
 F00R-C013 \\sim F00S-C0
 with sigma of 0.02
 F00R-F00T \\sim F00S-F00U
 with sigma of 0.04
 O00S-O1 \\sim O00T-O1A
 with sigma of 0.04
 F00T-C013 \\sim F00U-C0
 with sigma of 0.02
 F00Y-C013 \\sim F00Z-C0
 with sigma of 0.02
 F00R-F00Y \\sim F00S-F00Z
 with sigma of 0.04
 O00S-C013 \\sim O00T-C0
 with sigma of 0.04
 F00T-F00Y \\sim F00U-F00Z
 with sigma of 0.04
 S001-F00R \\sim S0-F00S
 with sigma of 0.04
 S001-F00T \\sim S0-F00U
 with sigma of 0.04
 S001-F00Y \\sim S0-F00Z
 with sigma of 0.04
 O00M-O00S \\sim O00N-O00T
 with sigma of 0.04
 O00M-C013 \\sim O00N-C0
 with sigma of 0.04
 O00M-O1 \\sim O00N-O1A
 with sigma of 0.04
2. Rigid body (RIGU) restrains
 O00T, O00N, S0, C0, O1A, F00S, F00U, F00Z, O00S, S001, O00M, C013, O1, F00R,
 F00T, F00Y
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: S001(0.85) O00M(0.85) F00R(0.85) O00S(0.85) F00T(0.85) F00Y(0.85)
 C013(0.85) O1(0.85) O00N(0.15) S0(0.15) O00T(0.15) C0(0.15) O1A(0.15)
 F00S(0.15) F00U(0.15) F00Z(0.15)
4.a Secondary CH2 refined with riding coordinates:
 C00O(H00D,H00E), C00W(H00F,H00G), C010(H01A,H01B), C011(H01C,H01D)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C14(H14), C7(H7), C9(H9), C12(H12), C22(H22), C13(H13),
 C10(H10)
4.c Idealised Me refined as rotating group:
 C00G(H00A,H00B,H00C), C00Z(H00H,H00I,H00J), C012(H01E,H01F,H01G)
;
_shelx_res_checksum              80740
_shelx_hkl_checksum              50255
_olex2_submission_special_instructions 'No special instructions were received'