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_2101992
_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         '2(C12 H10 O4 S), C12 H8 O4 S, C4 H15 N3'
_chemical_formula_sum            'C40 H43 N3 O12 S3'
_chemical_formula_weight         853.95
_chemical_name_systematic
;
Bis(2-aminoethyl)amine-4,4'-sulfonyldiphenol (1/3)
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7305(5)
_cell_length_b                   14.9948(6)
_cell_length_c                   19.4209(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      21.42
_cell_measurement_theta_min      10.56
_cell_volume                     3998.5(3)
_computing_cell_refinement       'SET4 & CELDIM (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1992)'
_computing_data_reduction
'DATRD2 in NRCVAX96 (Gabe, Le Page, Charland, Lee & White, 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 .99
_diffrn_measured_fraction_theta_max .99
_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     .7107
_diffrn_reflns_av_R_equivalents  .000
_diffrn_reflns_av_sigmaI/netI    .0226
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4595
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        'no decay, variation 1.0'
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .253
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          .41
_exptl_crystal_size_mid          .41
_exptl_crystal_size_min          .40
_refine_diff_density_max         .284
_refine_diff_density_min         -.234
_refine_ls_extinction_coef       .0020(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4595
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          .0646
_refine_ls_R_factor_gt           .0391
_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^)+(0.0551P)^2^+0.6244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1077
_reflns_number_gt                3159
_reflns_number_total             4595
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            na0096.cif
_cod_data_source_block           9810
_cod_database_code               2101992
_cod_database_fobs_code          2101992