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_1566772
_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
'O4 P, C52 H50 N12 O6, 2(H2 O), 3(C4 H12 N), C3 H6 O'
_chemical_formula_sum            'C67 H96 N15 O13 P'
_chemical_formula_weight         1350.55
_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   mixed
_audit_creation_date             2021-11-30
_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                 106.566(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0070(12)
_cell_length_b                   20.8259(16)
_cell_length_c                   13.9625(14)
_cell_measurement_reflns_used    3429
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.48
_cell_volume                     3625.2(6)
_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      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.1460
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23229
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.338
_diffrn_reflns_theta_min         1.956
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6384
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1268 before and 0.0772 after correction.
The Ratio of minimum to maximum transmission is 0.8567.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.6384
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 1983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         12829
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0954
_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^)+(0.1252P)^2^+2.7352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2734
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                6942
_reflns_number_total             12829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00876a2.cif
_cod_data_source_block           complex6
_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               1566772
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O11(H11B,H11C), O12(H12B,H12C)
2.b Ternary CH refined with riding coordinates:
 C45(H45), C7(H7A)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N12(H12), N7(H7), N2(H2), N4(H4), N3(H3), N6(H6), N1(H1), N8(H8),
 N11(H11), N9(H9), N10(H10), C25(H25), C48(H48), C28(H28), C21(H21), C20(H20),
 C51(H51), C11(H11A), C52(H52), C27(H27), C14(H14), C19(H19), C18(H18), C1(H1A),
  C50(H50), C26(H26), C12(H12A), C49(H49), C5(H5A), C40(H40), C39(H39),
 C13(H13), C3(H3A), C42(H42), C34(H34), C32(H32), C41(H41), C33(H33), C4(H4A),
 C2(H2A), C35(H35)
2.d Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C46(H46A,H46B,H46C), C56(H56A,H56B,H56C), C55(H55A,H55B,
 H55C), C8(H8A,H8B,H8C), C57(H57A,H57B,H57C), C53(H53A,H53B,H53C), C59(H59A,
 H59B,H59C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C),
 C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C65(H65A,H65B,
 H65C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              3367
_shelx_hkl_checksum              62313
_olex2_submission_special_instructions 'No special instructions were received'