<i>meso</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane as a building block in supramolecular chemistry; salts formed with 2,2'-biphenol, 4,4'-biphenol, 4,4'-thiodiphenol, 4,4'-sulfonyldiphenol, 3- and 4-hydroxybenzoic acids, 3,5-dihydroxybenzoic acid and phenylphosphonic acid; supramolecular structures in zero, one, two and three dimensions
Gregson, Richard M.; Glidewell, Christopher; Ferguson, George; Lough, Alan J.; Acta Crystallographica Section B 56 (2000) 39–57; doi:10.1107/S0108768199006072

data_2101981
_publ_section_title
;
 <i>meso</i>-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane
 as a building block in supramolecular chemistry; salts formed with
 2,2'-biphenol, 4,4'-biphenol, 4,4'-thiodiphenol,
 4,4'-sulfonyldiphenol, 3- and 4-hydroxybenzoic acids,
 3,5-dihydroxybenzoic acid and phenylphosphonic acid; supramolecular
 structures in zero, one, two and three dimensions
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              39
_journal_page_last               57
_journal_paper_doi               10.1107/S0108768199006072
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C16 H40 N4 4+, 4(C6 H6 O3 P -), 2(H2 O)'
_chemical_formula_sum            'C40 H68 N4 O14 P4'
_chemical_formula_weight         952.86
_chemical_name_systematic
;
Meso-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazayclotetradecane-
phenylphosphonic acid-water (1/4/2)
;
_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                 107.267(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7391(2)
_cell_length_b                   26.1558(7)
_cell_length_c                   10.7871(2)
_cell_measurement_reflns_used    22140
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      4.1
_cell_volume                     2354.57(19)
_computing_cell_refinement       'DENZO (Nonius, 1998)'
_computing_data_collection       'KappaCCD (Nonius, 1998)'
_computing_data_reduction        'DENZO (Nonius, 1998)'
_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      100.0(10)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       \w
_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  .065
_diffrn_reflns_av_sigmaI/netI    .0490
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22140
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         4.09
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .227
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .15
_refine_diff_density_max         .300
_refine_diff_density_min         -.499
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4796
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          .0563
_refine_ls_R_factor_gt           .0402
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+1.8098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1011
_reflns_number_gt                3777
_reflns_number_total             4796
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            na0090.cif
_cod_data_source_block           6
_cod_original_cell_volume        2354.57(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2101981