Anion-coordination-driven single-double helix switching and chiroptical molecular switch based on oligoureas
Li, Hongfei; Kou, Lei; Liang, Lin; Li, Boyang; Zhao, Wei; Yang, Xiao-Juan; Wu, Biao; Chemical Science  (2022) –; doi:10.1039/D2SC00876A

data_1566773
_publ_section_title
;
 Anion-coordination-driven single-double helix switching and chiroptical
 molecular switch based on oligoureas
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00876A
_journal_year                    2022
_chemical_formula_moiety         '2(Cl), C45 H44 N10 O5, 2(C16 H36 N)'
_chemical_formula_sum            'C77 H44 Cl2 N12 O5'
_chemical_formula_weight         1288.14
_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             2021-01-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-12-24 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.9750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9428(5)
_cell_length_b                   25.5121(9)
_cell_length_c                   12.5127(4)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.40
_cell_volume                     3807.3(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0596
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47493
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         1.707
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4343
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1502 before and 0.1040 after correction.
The Ratio of minimum to maximum transmission is 0.5827.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.4343
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 6027 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.042(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.732
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         13393
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.732
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1171P)^2^+1.9219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                12926
_reflns_number_total             13393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00876a2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1566773
_shelx_shelxl_version_number     2018/3
_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
2.a Ternary CH refined with riding coordinates:
 C38(H38), C7(H7A)
2.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C75(H75A,H75B), C66(H66A,H66B), C67(H67A,H67B), C70(H70A,
 H70B), C46(H46A,H46B), C62(H62A,H62B), C47(H47A,H47B), C64(H64A,H64B),
 C58(H58A,H58B), C54(H54A,H54B), C50(H50A,H50B), C76(H76A,H76B), C71(H71A,H71B),
  C68(H68A,H68B), C51(H51A,H51B), C48(H48A,H48B), C72(H72A,H72B), C59(H59A,
 H59B), C60(H60A,H60B), C52(H52A,H52B), C63(H63A,H63B), C55(H55A,H55B),
 C56(H56A,H56B)
2.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N3(H3), N9(H9), N1(H1), N7(H7), N10(H10), N2(H2), N4(H4), N6(H6),
 N5(H5), C14(H14), C26(H26), C35(H35), C32(H32), C27(H27), C18(H18), C28(H28),
 C5(H5A), C21(H21), C25(H25), C19(H19), C45(H45), C13(H13), C20(H20), C41(H41),
 C11(H11), C1(H1A), C33(H33), C4(H4A), C34(H34), C12(H12), C44(H44), C42(H42),
 C43(H43), C3(H3A), C2(H2A)
2.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C8(H8A,H8B,H8C), C65(H65A,H65B,H65C), C49(H49A,H49B,
 H49C), C73(H73A,H73B,H73C), C53(H53A,H53B,H53C), C77(H77A,H77B,H77C), C61(H61A,
 H61B,H61C), C69(H69A,H69B,H69C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              71001
_shelx_hkl_checksum              5490
_olex2_submission_special_instructions 'No special instructions were received'