Anion binding with biphenyl-bis-urea derivatives: solution and solid-state studies
Grgurić, Toni; Cetina, Mario; Petroselli, Manuel; Bacchiocchi, Corrado; Dzolić, Zoran; Cametti, Massimo; New Journal of Chemistry 44 (2020) 16294–16301; doi:10.1039/D0NJ03670F

data_7059911
_publ_section_title
;
 Anion binding with biphenyl-bis-urea derivatives: solution and
 solid-state studies
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16294
_journal_page_last               16301
_journal_paper_doi               10.1039/D0NJ03670F
_journal_volume                  44
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C26 H22 N4 O2, 2(C16 H36 N), 2(C2 H3 O2), H2 O'
_chemical_formula_sum            'C62 H102 N6 O7'
_chemical_formula_weight         1043.49
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-17T19:16:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.772(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0943(7)
_cell_length_b                   16.7406(10)
_cell_length_c                   18.7190(12)
_cell_measurement_reflns_used    2465
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      22.4710
_cell_measurement_theta_min      4.7190
_cell_volume                     3161.7(4)
_computing_cell_refinement
'CrysAlisPro 1.171.37.35 (Agilent Technologies, 2014)'
_computing_data_collection
'CrysAlisPro 1.171.37.35 (Agilent Technologies, 2014)'
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'CrysAlisPro 1.171.37.35 (Agilent Technologies, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      295(1)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13957
_diffrn_reflns_point_group_measured_fraction_full 0.851
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         4.329
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50098
_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            yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethylformamide'
_exptl_crystal_size_max          0.793
_exptl_crystal_size_mid          0.471
_exptl_crystal_size_min          0.203
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1991 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         10473
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1070P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1991
_reflns_Friedel_coverage         0.635
_reflns_Friedel_fraction_full    0.697
_reflns_Friedel_fraction_max     0.679
_reflns_number_gt                6486
_reflns_number_total             10473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03670f2.cif
_cod_data_source_block           1-((TBA)AcO)2-H2O
_cod_depositor_comments
'Adding full bibliography for 7059910--7059921.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7059911
_shelx_shelxl_version_number     2014/7