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_1572707
_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_formula_moiety         'C102 H102 Br4 N10 O8, 2(C H4 O)'
_chemical_formula_sum            'C104 H110 Br4 N10 O10'
_chemical_formula_weight         1979.65
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2024-05-11 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                112.136(4)
_cell_angle_beta                 107.694(4)
_cell_angle_gamma                95.621(4)
_cell_formula_units_Z            2
_cell_length_a                   15.9913(15)
_cell_length_b                   19.7892(19)
_cell_length_c                   21.961(2)
_cell_measurement_reflns_used    9597
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      49.928
_cell_measurement_theta_min      2.160
_cell_volume                     5952.5(10)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            141007
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         61.052
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0783 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.8387.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 11809 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.093(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2311
_refine_ls_number_reflns         52897
_refine_ls_number_restraints     1871
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                32303
_reflns_number_total             52897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04796f2.cif
_cod_data_source_block           230505_j2_zwj_0m
_cod_depositor_comments
'Adding full bibliography for 1572702--1572708.cif.'
_cod_original_cell_volume        5952.6(10)
_cod_database_code               1572707
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.792
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C37-C7FA
 2.55 with sigma of 0.01
 C06I-C7FA
 2.65 with sigma of 0.01
 C47-C37
 2.65 with sigma of 0.01
 C99-C7FA
 1.45 with sigma of 0.01
 C6FA-C47
 1.55 with sigma of 0.01
 C6FA-C37
 1.55 with sigma of 0.01
 C99-C37
 1.55 with sigma of 0.01
 C4FA-C3FA
 1.55 with sigma of 0.01
 C43-C06I
 1.55 with sigma of 0.01
 C8EA-C7EA \\sim C9EA-C8EA \\sim C7EA-C05B \\sim C6EA-C05B \\sim C6EA-C5EA
\\sim C5EA-C4EA \\sim C4EA-
 C2DA
 with sigma of 0.02
3. Rigid bond restraints
 C6DA, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C06I, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within -2.3A with sigma of 0.01 and
sigma for terminal atoms of 0.02
5.a Riding coordinates:
 N053(H053), N12(H12), O4(H4), O2AA(H2AA)
5.b Secondary CH2 refined with riding coordinates:
 C017(H01A,H01B), C018(H01C,H01D), C03D(H03A,H03B), C03H(H03L,H03M), C03J(H03O,
 H03P), C03T(H03D,H03E), C03V(H03F,H03G), C03W(H03H,H03I), C03Y(H03J,H03K),
 C044(H04G,H04H), C04F(H04A,H04B), C04G(H04C,H04D), C04K(H04I,H04K), C04L(H04L,
 H04M), C04R(H04E,H04F), C04S(H04N,H04O), C04Y(H04Q,H04R), C054(H05G,H05H),
 C056(H05A,H05B), C05B(H05I,H05J), C05E(H05K,H05L), C05J(H05C,H05D), C05K(H05M,
 H05N), C05N(H05O,H05P), C05U(H05R,H05S), C05W(H05E,H05F), C060(H06A,H06B),
 C064(H06I,H06J), C065(H06C,H06D), C06D(H06E,H06F), C06E(H06K,H06L), C06I(H06G,
 H06H), C22(H22A,H22B), C4(H4A,H4B), C23(H23A,H23B), C28(H28A,H28B), C5AA(H5AA,
 H5AB), C7AA(H7AA,H7AB), C5BA(H5BA,H5BB), C11(H11A,H11B), C6AA(H6AA,H6AB),
 C8AA(H8AA,H8AB), C7BA(H7BA,H7BB), C19(H19A,H19B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C29(H29A,H29B), C2BA(H2BA,H2BB), C0CA(H0CA,H0CB),
 C1CA(H1CA,H1CB), C9BA(H9BA,H9BB), C20(H20A,H20B), C1DA(H1DA,H1DB), C9CA(H9CA,
 H9CB), C4DA(H4DA,H4DB), C3DA(H3DA,H3DB), C9DA(H9DA,H9DB), C5DA(H5DA,H5DB),
 C7DA(H7DA,H7DB), C2DA(H2DA,H2DB), C0EA(H0EA,H0EB), C1EA(H1EA,H1EB), C3EA(H3EA,
 H3EB), C7EA(H7EA,H7EB), C9EA(H9EA,H9EB), C5EA(H5EA,H5EB), C8EA(H8EA,H8EB),
 C6EA(H6EA,H6EB), C4EA(H4EA,H4EB), C43(H43A,H43B), C47(H47A,H47B), C3FA(H3FA,
 H3FB), C4FA(H4FA,H4FB), C36(H36A,H36B), C40(H40A,H40B), C7FA(H7FA,H7FB),
 C6FA(H6FA,H6FB), C37(H37A,H37B), C99(H99A,H99B)
5.c Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00Z(H00Z), C012(H012), C019(H019), C01B(H01E), C01H(H01H),
 C01J(H01J), C020(H020), C029(H029), C02C(H02C), C02F(H02F), C02H(H02H),
 C02I(H02I), C02V(H02V), C02X(H02X), C033(H033), C03C(H03C), C03I(H03N),
 C03N(H03Q), C03R(H03R), C03X(H03X), C048(H048), C04J(H04J), C04P(H04P),
 C04U(H04U), N058(H058), C05P(H05Q), C16(H16), C8(H8), C2EA(H2EA), C6DA(H6DA),
 C30(H30), C6(H6), C7(H7), C10(H10), C18(H18), C0BA(H0BA), C9AA(H9AA),
 C4CA(H4CA), C2CA(H2CA), C6CA(H6CA), N0DA(H0DA)
5.d Idealised Me refined as rotating group:
 C0DA(H0DB,H0DC,H0DD), C1FA(H1FA,H1FB,H1FC), C2FA(H2FA,H2FB,H2FC), C5FA(H5FA,
 H5FB,H5FC)
5.e Idealised tetrahedral OH refined as rotating group:
 O0AA(H0AA), O4AA(H4AA)
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_olex2_submission_special_instructions 'No special instructions were received'