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_7059209
_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         'C21 H17 N5 O4, C16 H36 N, F'
_chemical_formula_sum            'C37 H53 F N6 O4'
_chemical_formula_weight         664.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-07-31 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.634(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2710(3)
_cell_length_b                   17.4802(4)
_cell_length_c                   19.5368(4)
_cell_measurement_reflns_used    6119
_cell_measurement_temperature    296.31(10)
_cell_measurement_theta_max      71.9360
_cell_measurement_theta_min      4.7370
_cell_volume                     3993.72(17)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.31(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega   20.00  104.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -       36.4171   57.0000   60.0000 84

  2 omega   20.00  104.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -       36.4171   57.0000  -90.0000 84

  3 omega   20.00  104.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -       36.4171   57.0000    0.0000 84

  4 omega  -31.00   53.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -57.0000  150.0000 84

  5 omega    1.00   75.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -99.0000  -90.0000 74

  6 omega   23.00   90.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -       36.4171 -125.0000  150.0000 67

  7 omega  -31.00   53.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -57.0000  -30.0000 84

  8 omega   40.00   98.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

  9 omega  100.00  178.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 78

 10 omega   39.00  109.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 70

 11 omega   39.00  109.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 70

 12 omega   38.00   91.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 13 omega   39.00  109.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 70

 14 omega   38.00   91.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

 15 omega  133.00  177.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 44

 16 omega   50.00   87.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 37

 17 omega   45.00   91.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 46

 18 omega   40.00   90.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 50

 19 omega   42.00   97.00   1.0000   11.0200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 55
;
_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      -0.0979322000
_diffrn_orient_matrix_UB_12      0.0511841000
_diffrn_orient_matrix_UB_13      -0.0446966000
_diffrn_orient_matrix_UB_21      0.0820952000
_diffrn_orient_matrix_UB_22      0.0689509000
_diffrn_orient_matrix_UB_23      0.0134899000
_diffrn_orient_matrix_UB_31      0.0320654000
_diffrn_orient_matrix_UB_32      -0.0198922000
_diffrn_orient_matrix_UB_33      -0.0682669000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22804
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.825
_diffrn_reflns_theta_min         4.549
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64242
_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    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0641
_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^)+(0.1260P)^2^+0.3581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5888
_reflns_number_total             7792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05785d2.cif
_cod_data_source_block           hc-sx-l3-3_sq
_cod_depositor_comments
;Adding full bibliography for 7059208--7059212.cif.

 Adding full bibliography for 7059208--7059212.cif.
;
_cod_original_cell_volume        3993.72(16)
_cod_database_code               7059209
_shelx_shelxl_version_number     2014/7
_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
2.a Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00E(H00C,H00D), C00H(H00E,H00F), C00L(H00G,H00H), C00M(H00I,
 H00J), C00N(H00K,H00L), C00O(H00M,H00N), C00Q(H00O,H00P), C00S(H00Q,H00R),
 C00T(H00S,H00T), C00U(H00U,H00V), C010(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 N006(H006), N009(H009), N00A(H00), N00B(H0AA), C00V(H1AA), C00W(H2AA),
 C00Y(H3AA), C011(H011), C012(H012), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019), C01A(H01I), C01B(H01J)
2.c Idealised Me refined as rotating group:
 C00X(H00W,H00X,H00Y), C00Z(H00Z,H,HA), C013(H01C,H01D,H01E), C01C(H01F,H01G,
 H01H)
;
_shelx_res_checksum              24778
_shelx_fab_checksum              93851
_olex2_date_sample_data_collection 2017-06-16
_olex2_submission_special_instructions 'No special instructions were received'