Anion binding and fluoride ion induced conformational changes in bisurea receptors
Shu, Xi; Fan, Yu; Li, Shoujian; Jin, Yongdong; Xia, Chuanqin; Huang, Chao; New Journal of Chemistry 44 (2020) 2033–2045; doi:10.1039/C9NJ05785D

data_7059208
_publ_section_title
;
 Anion binding and fluoride ion induced conformational changes in bisurea
 receptors
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2033
_journal_page_last               2045
_journal_paper_doi               10.1039/C9NJ05785D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '2(C13 H17 N5 O4)'
_chemical_formula_sum            'C26 H34 N10 O8'
_chemical_formula_weight         614.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-05 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                92.323(4)
_cell_angle_beta                 106.840(4)
_cell_angle_gamma                110.178(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0672(4)
_cell_length_b                   13.1124(7)
_cell_length_c                   14.5279(7)
_cell_measurement_reflns_used    5122
_cell_measurement_temperature    293.52(10)
_cell_measurement_theta_max      72.5420
_cell_measurement_theta_min      4.4790
_cell_volume                     1532.65(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.52(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -99.0000 -120.0000 74

  2 omega   19.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   57.0000  120.0000 84

  3 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -57.0000  -60.0000 84

  4 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671 -125.0000  120.0000 67

  5 omega    9.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   77.0000    0.0000 95

  6 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -38.0000  120.0000 88

  7 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -38.0000 -150.0000 88

  8 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -99.0000 -180.0000 74

  9 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -77.0000   60.0000 94

 10 omega   39.00  109.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 70

 11 omega   38.00   91.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

 12 omega   38.00   91.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 13 omega   38.00  116.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 78

 14 omega   40.00   98.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 58

 15 omega   38.00   91.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

 16 omega   37.00  146.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000  -90.0000 109

 17 omega   38.00   91.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

 18 omega   41.00  126.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -180.0000 85

 19 omega   41.00  126.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -30.0000 85

 20 omega   38.00   91.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 21 omega   39.00  109.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 70

 22 omega   38.00   91.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 23 omega   41.00  126.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 85

 24 omega   70.00  178.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 108

 25 omega   39.00   64.00   1.0000    3.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0814738000
_diffrn_orient_matrix_UB_12      -0.0985561000
_diffrn_orient_matrix_UB_13      -0.0831695000
_diffrn_orient_matrix_UB_21      0.0477395000
_diffrn_orient_matrix_UB_22      -0.0747625000
_diffrn_orient_matrix_UB_23      0.0726205000
_diffrn_orient_matrix_UB_31      -0.1663961000
_diffrn_orient_matrix_UB_32      -0.0275310000
_diffrn_orient_matrix_UB_33      0.0197920000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13339
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.425
_diffrn_reflns_theta_min         5.339
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1460P)^2^+0.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2038
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4798
_reflns_number_total             5849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05785d2.cif
_cod_data_source_block           hc-sx-l1
_cod_depositor_comments
;Adding full bibliography for 7059208--7059212.cif.

 Adding full bibliography for 7059208--7059212.cif.
;
_cod_original_cell_volume        1532.64(14)
_cod_database_code               7059208
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Secondary CH2 refined with riding coordinates:
 C00W(H00B,H00J), C012(H01A,H01B), C014(H01C,H01D), C017(H01N,H01O)
2.b Aromatic/amide H refined with riding coordinates:
 N00A(H00A), N00C(H00C), N00D(H00D), N00E(H00E), N00F(H00F), N00G(H00G),
 N00H(H00H), N00I(H00I), C00O(H00O), C00V(H00V), C00X(H00X), C00Y(H00Y),
 C010(H010), C013(H013)
2.c Idealised Me refined as rotating group:
 C011(H01K,H01L,H01M), C015(H01E,H01F,H01G), C016(H01H,H01I,H01J), C018(H01P,
 H01Q,H01R)
;
_shelx_res_checksum              98428
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-01-13
_olex2_submission_special_instructions 'No special instructions were received'