Supramolecular chemistry of amine–phenol adducts; novel three-dimensional framework structures in adducts of bis(2-aminoethyl)amine with 4,4'-sulfonyldiphenol, 1,1,1-tris(4-hydroxyphenyl)ethane and 3,5-dihydroxybenzoic acid, and in the methanol-solvated adduct of tris(2-aminoethyl)amine with 4,4'-biphenol
Glidewell, Christopher; Ferguson, George; Gregson, Richard M.; Campana, Charles F.; Acta Crystallographica Section B 56 (2000) 68–84; doi:10.1107/S0108768199009714

data_2101994
_publ_section_title
;
 Supramolecular chemistry of amine--phenol adducts; novel
 three-dimensional framework structures in adducts of
 bis(2-aminoethyl)amine with 4,4'-sulfonyldiphenol,
 1,1,1-tris(4-hydroxyphenyl)ethane and 3,5-dihydroxybenzoic acid, and
 in the methanol-solvated adduct of tris(2-aminoethyl)amine with
 4,4'-biphenol
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              68
_journal_page_last               84
_journal_paper_doi               10.1107/S0108768199009714
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C4 H15 N3, 2(C7 H5 O4)'
_chemical_formula_sum            'C18 H25 N3 O8'
_chemical_formula_weight         411.41
_chemical_name_systematic
;
Bis(2-aminoethyl)amine-3,5-dihydroxybenzoic acid (1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.144(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2469(7)
_cell_length_b                   10.527(2)
_cell_length_c                   23.052(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      15.06
_cell_measurement_theta_min      9.95
_cell_volume                     1981.1(5)
_computing_cell_refinement       'SET4 & CELDIM (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD-4-PC Software (Enraf-Nonius, 1992)'
_computing_data_reduction        'DATRD2 in NRCVAX96 (Gabe et al., 1989)'
_computing_molecular_graphics
'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1998)'
_computing_publication_material
'NRCVAX96, SHELXL97  and WordPerfect macro PREP8 (Ferguson, 1998)'
_computing_structure_refinement  'NRCVAX96 and SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .014
_diffrn_reflns_av_sigmaI/netI    .1478
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3807
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        'no decay, variation  0.6'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .109
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             872
_exptl_crystal_size_max          .41
_exptl_crystal_size_mid          .41
_exptl_crystal_size_min          .22
_refine_diff_density_max         .282
_refine_diff_density_min         -.209
_refine_ls_extinction_coef       .0042(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   .831
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .831
_refine_ls_R_factor_all          .1528
_refine_ls_R_factor_gt           .0561
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0198P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0826
_reflns_number_gt                1536
_reflns_number_total             3555
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            na0096.cif
_cod_data_source_block           9828
_cod_original_cell_volume        1981.0(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2101994
_cod_database_fobs_code          2101994