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_1566770
_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), 2(C19 H19 N4 O2), 2(C8 H20 N)'
_chemical_formula_sum            'C54 H78 Cl2 N10 O4'
_chemical_formula_weight         1002.16
_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
_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                 114.8810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7990(5)
_cell_length_b                   14.2717(4)
_cell_length_c                   20.0159(6)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.7175
_cell_measurement_theta_min      2.4320
_cell_volume                     5390.0(3)
_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 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'SSRF BL17B Beamline'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32045
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         1.121
_exptl_absorpt_coefficient_mu    0.175
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Block
_exptl_crystal_F_000             2152
_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   0.6256
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 4181 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.051(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8941
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0743P)^2^+1.3448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                8832
_reflns_number_total             8941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00876a2.cif
_cod_data_source_block           complex1
_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               1566770
_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:
 C26(H26), C7(H7A)
2.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C45(H45A,H45B), C49(H49A,H49B), C39(H39A,H39B), C51(H51A,
 H51B), C43(H43A,H43B), C53(H53A,H53B), C47(H47A,H47B)
2.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N3(H3), N7(H7), N4(H4), N2(H2), N5(H5), N6(H6), N1(H1), C30(H30),
 C37(H37), C1(H1A), C31(H31), C33(H33), C38(H38), C32(H32), C11(H11), C18(H18),
 C5(H5A), C2(H2A), C14(H14), C12(H12), C20(H20), C19(H19), C3(H3A), C24(H24),
 C13(H13), C4(H4A), C23(H23), C21(H21), C22(H22)
2.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C52(H52A,H52B,H52C), C46(H46A,H46B,H46C), C40(H40A,H40B,
 H40C), C54(H54A,H54B,H54C), C27(H27A,H27B,H27C), C8(H8A,H8B,H8C), C48(H48A,
 H48B,H48C), C44(H44A,H44B,H44C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              12936
_shelx_hkl_checksum              25691
_olex2_submission_special_instructions 'No special instructions were received'