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_2101995
_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(C6 H19 N4), 5(C12 H10 O2), C12 H8 O2, 2(C H4 O)'
_chemical_formula_sum            'C86 H104 N8 O14'
_chemical_formula_weight         1473.77
_chemical_name_systematic
;
Tris(2-aminoethyl)amine-4,4'-biphenol-methanol (1/3/1)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 112.7460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0041(2)
_cell_length_b                   41.5502(7)
_cell_length_c                   10.27150(10)
_cell_measurement_reflns_used    23654
_cell_measurement_temperature    293.0(10)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      .98
_cell_volume                     3937.52(11)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics
'NRCVAX-96, ORTEP (Johnson, 1976), PLATON (Spek, 1999)'
_computing_publication_material
'NRCVAX-96, SHELXL-97  and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'NRCVAX-96 and SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293.0(10)
_diffrn_measured_fraction_theta_full .991
_diffrn_measured_fraction_theta_max .929
_diffrn_measurement_device_type  Siemens-CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0397
_diffrn_reflns_av_sigmaI/netI    .0427
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23654
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         .98
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .15
_refine_diff_density_max         .175
_refine_diff_density_min         -.209
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_extinction_coef       .0021(6)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         9156
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          .0837
_refine_ls_R_factor_gt           .0572
_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^)+(0.0627P)^2^+0.8778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1433
_reflns_number_gt                6625
_reflns_number_total             9156
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            na0096.cif
_cod_data_source_block           9733frav
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2101995
_cod_database_fobs_code          2101995