Crystal structure of a host‒guest complex of the tris-urea receptor, 3-(4-nitrophenyl)-1,1-bis{2-[3-(4-nitrophenyl)ureido]ethyl}urea, that encapsulates hydrogen-bonded chains of dihydrogen phosphate anions with separate tetra-<i>n</i>-butylammonium counter-ions
Wang, Ruyu; Shu, Xi; Fan, Yu; Li, Shoujian; Jin, Yongdong; Xia, Chuanqin; Huang, Chao; Acta Crystallographica Section E 75 (2019) 319–323; doi:10.1107/S2056989019001336

data_2242842
_publ_section_title
;
 Crystal structure of a host--guest complex of the tris-urea receptor,
 3-(4-nitrophenyl)-1,1-bis{2-[3-(4-nitrophenyl)ureido]ethyl}urea, that
 encapsulates hydrogen-bonded chains of dihydrogen phosphate anions with
 separate tetra-<i>n</i>-butylammonium counter-ions
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              319
_journal_page_last               323
_journal_paper_doi               10.1107/S2056989019001336
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C25 H25 N9 O9, C16 H36 N + , H2 P O4 -'
_chemical_formula_moiety         'C25 H25 N9 O9, C16 H36 N, H2 O4 P'
_chemical_formula_sum            'C41 H63 N10 O13 P'
_chemical_formula_weight         934.98
_chemical_name_systematic
;
3-(4-Nitrophenyl)-1,1-bis{2-[3-(4-nitrophenyl)ureido]ethyl}urea
tetrabutylammonium dihydrogen phosphate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                83.797(2)
_cell_angle_beta                 79.818(2)
_cell_angle_gamma                89.191(2)
_cell_formula_units_Z            4
_cell_length_a                   15.2043(3)
_cell_length_b                   17.4555(5)
_cell_length_c                   18.1232(4)
_cell_measurement_reflns_used    22142
_cell_measurement_temperature    179(2)
_cell_measurement_theta_max      72.61
_cell_measurement_theta_min      4.17
_cell_volume                     4706.3(2)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009) and Mercury (Macrae <i>et
al.</i>,  2008)
;
_computing_publication_material
;
ShelXL (Sheldrick, 2015b), PLATON (Spek, 2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      179(2)
_diffrn_detector_area_resol_mean 15.9595
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Agilent New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50539
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.719
_diffrn_reflns_theta_min         4.486
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlisPro</i>; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.848
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         18359
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0652
_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^)+(0.06P)^2^+6P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1603
_reflns_number_gt                15323
_reflns_number_total             18359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            kq2020sup1.cif
_cod_data_source_block           I
_cod_database_code               2242842
_shelx_estimated_absorpt_t_min   0.661
_shelx_estimated_absorpt_t_max   0.895
_shelx_hkl_checksum              86190
_shelx_res_checksum              98815
_shelxl_version_number           .2013
_cod_database_fobs_code 2242842