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

data_1567620
_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         'C57 H53 I2 N5 Rh2, 2(C H Cl3)'
_chemical_formula_sum            'C59 H55 Cl6 I2 N5 Rh2'
_chemical_formula_weight         1506.40
_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                 91.779(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6999(9)
_cell_length_b                   18.4945(10)
_cell_length_c                   20.4988(11)
_cell_measurement_reflns_used    7494
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.547
_cell_measurement_theta_min      2.587
_cell_volume                     5949.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.977
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25663
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.702
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1001 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.7968.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       plate
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         7506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+8.2472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6401
_reflns_number_total             7506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04006a2.cif
_cod_data_source_block           f2
_cod_depositor_comments
'Adding full bibliography for 1567617--1567621.cif.'
_cod_database_code               1567620
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C201(H201)
1.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
 C20(H20), C6(H6)
1.c Idealised Me refined as rotating group:
 C150(H15A,H15B,H15C), C154(H15D,H15E,H15F), C151(H15G,H15H,H15I), C152(H15J,
 H15K,H15L), C153(H15M,H15N,H15O), C301(H30A,H30B,H30C)
;
_shelx_res_checksum              60935
_shelx_hkl_checksum              74198
_olex2_submission_special_instructions 'No special instructions were received'