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_1572704
_publ_section_title
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 Tether-entangled conjugated helices.
;
_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         'C32 H36 Br2 N2 O4'
_chemical_formula_sum            'C32 H36 Br2 N2 O4'
_chemical_formula_weight         672.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-19
_audit_creation_method
; 
Olex2 1.3 
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) 
;
_audit_update_record
;
2024-05-11 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6760(5)
_cell_length_b                   9.3251(4)
_cell_length_c                   13.9069(5)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.25
_cell_measurement_theta_min      2.77
_cell_volume                     1512.06(11)
_computing_cell_refinement
'SAINT V8.40B Bruker-AXS, Madison WI for PHOTON III'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction
'SAINT V8.40B Bruker-AXS, Madison WI for PHOTON III'
_computing_molecular_graphics
'Bruker SHELXTL Bruker-AXS, Madison WI and local programs'
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon III 28 detector'
_diffrn_detector_area_resol_mean ' 7.39 for PHOTON III'
_diffrn_detector_type            'Bruker Photon III 28'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  'Bruker Photon III'
_diffrn_measurement_method       'Profile data from \q/2\q scans'
_diffrn_radiation_monochromator  'Metaljet Helios MX'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_xray_symbol    'Ga K\a'
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37233
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         72.518
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'METALJET liquid metal X-ray source'
_diffrn_source_current           3.58
_diffrn_source_power             0.250421
_diffrn_source_target            Ga
_diffrn_source_type              'Sealed X-ray tube'
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS, Madison WI for PHOTON III'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
; 
 Flack x determined using 3855 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.053(8)
_refine_ls_extinction_coef       0.0185(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8909
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0300P)^2^+0.5545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                8665
_reflns_number_total             8909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04796f2.cif
_cod_data_source_block           220919a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1572702--1572708.cif.
;
_cod_database_code               1572704
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Restrained distances 
 C4-C5 \\sim C4-C5A 
 with sigma of 0.02 
 C5-C6 \\sim C5A-C6A 
 with sigma of 0.02 
 C7-N2 \\sim C7A-N2 
 with sigma of 0.04 
 C6-C7 \\sim C6A-C7A 
 with sigma of 0.02 
 C7-C8 \\sim C7A-C8A 
 with sigma of 0.02 
 C6-C8 \\sim C6A-C8A 
 with sigma of 0.04 
 C8-N2 \\sim C8A-N2 
 with sigma of 0.02 
 C4-C6 \\sim C4-C6A 
 with sigma of 0.04 
 C5-C7 \\sim C5A-C7A 
 with sigma of 0.04 
3. Others 
 Sof(H4BC)=Sof(H4BD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)= 
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(1) 
 Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)= 
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=FVAR(1) 
4.a Ternary CH refined with riding coordinates: 
 C15(H15), C24(H24) 
4.b Secondary CH2 refined with riding coordinates: 
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A, 
 H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C5A(H5AA,H5AB), C6A(H6AA,H6AB), 
 C7A(H7AA,H7AB), C8A(H8AA,H8AB) 
4.c Aromatic/amide H refined with riding coordinates: 
 C10(H10), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), 
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31) 
4.d Idealised Me refined as rotating group: 
 C16(H16A,H16B,H16C), C25(H25A,H25B,H25C) 
;
_olex2_submission_special_instructions 'No special instructions were received'