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_7059211
_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         'C13 H17 N5 O4, H2 O'
_chemical_formula_sum            'C13 H19 N5 O5'
_chemical_formula_weight         325.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-07-31 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.934(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9330(3)
_cell_length_b                   21.6567(7)
_cell_length_c                   9.2173(3)
_cell_measurement_reflns_used    4213
_cell_measurement_temperature    294.33(10)
_cell_measurement_theta_max      72.3190
_cell_measurement_theta_min      5.3830
_cell_volume                     1522.71(10)
_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      294.33(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   23.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0421 -125.0000   30.0000 66

  2 omega   17.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0421   38.0000   30.0000 88

  3 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -57.0000 -150.0000 84

  4 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -57.0000  150.0000 84

  5 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -57.0000  -90.0000 84

  6 omega   38.00   91.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

  7 omega   38.00   91.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

  8 omega   40.00  135.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -120.0000 95

  9 omega   40.00   98.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 58

 10 omega   40.00   98.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

 11 omega   39.00  109.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 70

 12 omega   38.00   91.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 13 omega   40.00   98.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

 14 omega   40.00   98.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 58

 15 omega   90.00  175.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000    0.0000 85

 16 omega   19.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0421   57.0000  120.0000 84

 17 omega   17.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0421   38.0000 -120.0000 88
;
_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      -0.1433603000
_diffrn_orient_matrix_UB_12      0.0500795000
_diffrn_orient_matrix_UB_13      -0.0287932000
_diffrn_orient_matrix_UB_21      -0.1262861000
_diffrn_orient_matrix_UB_22      -0.0433821000
_diffrn_orient_matrix_UB_23      -0.1111359000
_diffrn_orient_matrix_UB_31      -0.0654995000
_diffrn_orient_matrix_UB_32      -0.0259233000
_diffrn_orient_matrix_UB_33      0.1304286000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8364
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.453
_diffrn_reflns_theta_min         5.393
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45037
_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    1.419
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0910P)^2^+0.3280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2719
_reflns_number_total             2967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05785d2.cif
_cod_data_source_block           lsj-sx
_cod_depositor_comments
;Adding full bibliography for 7059208--7059212.cif.

 Adding full bibliography for 7059208--7059212.cif.
;
_cod_original_cell_volume        1522.70(9)
_cod_database_code               7059211
_reflns_odcompleteness_completeness 99.89
_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, All O(H,H) groups
2.a Free rotating group:
 O003(H00O,H00P)
2.b Secondary CH2 refined with riding coordinates:
 C00J(H00B,H00C), C00M(H00I,H00J)
2.c Aromatic/amide H refined with riding coordinates:
 N006(H006), N007(H007), N009(H009), N00A(H00A), C00E(H00E), C00H(H00H),
 C00K(H00K)
2.d Idealised Me refined as rotating group:
 C00L(H00D,H00F,H00G), C00N(H00L,H00M,H00N)
;
_shelx_res_checksum              5208
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-14
_olex2_submission_special_instructions 'No special instructions were received'