Tether-entangled conjugated helices.
Jin, Ke; Xiao, Zuo; Xie, Huidong; Shen, Xingxing; Wang, Jizheng; Chen, Xiangyu; Wang, Zhijie; Zhao, Zujin; Yan, Keyou; Ding, Yong; Ding, Liming; Chemical science 15 (2024) 17128–17149; doi:10.1039/d4sc04796f

data_1572705
_publ_section_title
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 Tether-entangled conjugated helices.
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_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              17128
_journal_page_last               17149
_journal_paper_doi               10.1039/d4sc04796f
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         '3(C0.5 H Cl), C46 H44 F2 N4, 0.5(C1 H2 Cl1)'
_chemical_formula_sum            'C48 H48 Cl3.5 F2 N4'
_chemical_formula_weight         842.98
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-25
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2024-05-11 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9463(3)
_cell_length_b                   15.9463(3)
_cell_length_c                   35.1878(11)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.51
_cell_volume                     8947.7(4)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            123102
_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         27.125
_diffrn_reflns_theta_min         1.897
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1136 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.9478.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             3532
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 3171 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9906
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1650P)^2^+3.1716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2383
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8353
_reflns_number_total             9906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04796f2.cif
_cod_data_source_block           mo_220824_c8f_0m
_cod_depositor_comments
'Adding full bibliography for 1572702--1572708.cif.'
_cod_original_formula_sum        'C48 H48 Cl3.50 F2 N4'
_cod_database_code               1572705
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H41A-H50D
 2 with sigma of 0.001
 Cl2-C47 \\sim Cl2A-C47A
 with sigma of 0.02
 Cl1-C47 \\sim Cl1A-C47A
 with sigma of 0.02
 Cl2-Cl1 \\sim Cl2A-Cl1A
 with sigma of 0.04
 Cl5-C50 \\sim Cl5A-C50A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C47 \\sim Cl1A \\sim Cl2A \\sim C47A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Cl5 \\sim C50 \\sim Cl5A \\sim C50A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C47) = Uanis(C47A)
Uanis(C50) = Uanis(C50A)
4. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(C47A)=Sof(H47C)=Sof(H47D)=0.5*(1-FVAR(2))
 Sof(Cl1)=Sof(Cl2)=Sof(C47)=Sof(H47A)=Sof(H47B)=0.5*FVAR(2)
 Sof(Cl5A)=Sof(C50A)=Sof(H50C)=Sof(H50D)=0.5*(1-FVAR(3))
 Sof(Cl5)=Sof(C50)=Sof(H50A)=Sof(H50B)=0.5*FVAR(3)
 Fixed Sof: H48A(0.5) H48B(0.5) H49B(0.5) H49A(0.5)
 Fixed X: C50A(0.55148)
 Fixed Y: C50A(0.56099)
 Fixed Z: C50A(0.5298)
5.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49B,H49A), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C50(H50A,H50B), C47A(H47C,H47D), C50A(H50C,H50D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C9(H9), C12(H12), C15(H15), C18(H18), C21(H21),
 C24(H24), C27(H27), C29(H29), C30(H30)
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_shelx_res_checksum              82441
_olex2_submission_special_instructions 'No special instructions were received'