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_1572708
_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, C H2 Cl2'
_chemical_formula_sum            'C103 H104 Br4 Cl2 N10 O8'
_chemical_formula_weight         2000.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-30
_audit_creation_method
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Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
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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                90
_cell_angle_beta                 110.733(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.326(2)
_cell_length_b                   20.5209(11)
_cell_length_c                   16.0320(9)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      47.242
_cell_measurement_theta_min      2.564
_cell_volume                     12407.7(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0500
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            86570
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.709
_diffrn_reflns_theta_min         2.038
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           3.57
_diffrn_source_power             0.2495787
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           69.91
_exptl_absorpt_coefficient_mu    1.599
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.8134.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       block
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 5330 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.089(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1132
_refine_ls_number_reflns         26967
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1308P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.888
_reflns_number_gt                15529
_reflns_number_total             26967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04796f2.cif
_cod_data_source_block           230505_j1_zwj_0m
_cod_depositor_comments
'Adding full bibliography for 1572702--1572708.cif.'
_cod_database_code               1572708
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.762
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 Cl0A-Cl2
 2.8 with sigma of 0.01
 Cl2-C33 = Cl0A-C33
 1.7 with sigma of 0.01
 C8-N03H
 2.5 with sigma of 0.01
 N03H-C6
 1.47 with sigma of 0.01
 C5-C1
 2.3 with sigma of 0.01
 C8-C1
 1.49 with sigma of 0.003
 C0AA-C8
 2.35 with sigma of 0.003
 C5-C0AA = C5-C4 = C4-C3 = C3-C11 = C1-C0AA = C8-C6
 1.45 with sigma of 0.003
 C5-C3
 2.45 with sigma of 0.003
 C6-C1
 2.45 with sigma of 0.003
 C4-C0AA
 2.45 with sigma of 0.01
 C1-C0AA
 1.47 with sigma of 0.01
 C8-C5
 3.12 with sigma of 0.01
 H4B-H03D_$1
 2.1 with sigma of 0.01
 Cl2-C33 \\sim Cl0A-C33
 with sigma of 0.02
3. Rigid bond restraints
 C8, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C8 \\sim C1 \\sim C0AA \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim N03H \\sim C11
\\sim C33 \\sim Cl0A \\sim Cl2 \\sim Br03 \\sim Br04 \\sim N029 \\sim C02Z
\\sim C03E \\sim C7 \\sim C2 \\sim C03A \\sim C034 \\sim N03H \\sim C8 \\sim
C11: within -3.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within -3.5A
5.a Secondary CH2 refined with riding coordinates:
 C023(H02A,H02B), C025(H02C,H02D), C028(H02E,H02F), C02A(H02G,H02H), C02B(H02I,
 H02J), C02C(H02K,H02L), C02E(H02M,H02N), C02F(H02O,H02P), C02G(H02Q,H02R),
 C02H(H02S,H02T), C02I(H02U,H02V), C02J(H02W,H02X), C02K(H02Y,H), C02L(H02Z,HA),
  C02N(H1,HB), C02O(H2,HC), C02P(H3,HD), C02Q(H4,HE), C02R(H5,HF), C02S(H6,HG),
 C02T(H7,HH), C02U(H8,HI), C02V(H9,HJ), C02W(H10,HK), C02X(H11,HL), C02Y(H12,
 HM), C030(H03A,H03B), C031(H03C,H03D), C033(H03E,H03F), C035(H03G,H03H),
 C036(H03I,H03J), C037(H03K,H03L), C8(H8A,H8B), C11(H11A,H11B), C33(H33A,H33B),
 C1(H1A,H1B), C0AA(H0AA,H0AB), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,
 H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00R(H00R), C00X(H00X), C011(H011), C018(H018), C01E(H01E),
 C01I(H01I), C01J(H01J), C01K(H01K), C01M(H01M), C01N(H01N), C01P(H01P),
 C01Q(H01Q), N01S(H01S), C01V(H01V), C01X(H01X), C01Z(H01Z), C024(H024),
 C02M(H02), C7(H7A), C034(H034), N03H(H03M)
5.c Fitted hexagon refined as free rotating group:
 C02Z(C03E,C7,C2,C03A,C034)
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_olex2_submission_special_instructions 'No special instructions were received'