Crystal Engineering Using Bis- and Tris-phenols. Adducts with 1,4,8,11-Tetraazacyclotetradecane (Cyclam): Isolated Ladders in the Adduct with 4,4'-Thiodiphenol, Tethered Ladders in the Adduct with 4,4'-Sulfonyldiphenol and Two Interwoven Three-Dimensional Networks in the Adduct with 1,1,1-Tris(4-hydroxyphenyl)ethane
Ferguson, G.; Glidewell, C.; Gregson, R. M.; Meehan, P. R.; Acta Crystallographica Section B 54 (1998) 139–150; doi:10.1107/S0108768197010136

data_2105513
_publ_section_title
;
 Crystal Engineering Using Bis- and Tris-phenols. Adducts with
 1,4,8,11-Tetraazacyclotetradecane (Cyclam): Isolated Ladders in the
 Adduct with 4,4'-Thiodiphenol, Tethered Ladders in the Adduct with
 4,4'-Sulfonyldiphenol and Two Interwoven Three-Dimensional Networks in
 the Adduct with 1,1,1-Tris(4-hydroxyphenyl)ethane
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              139
_journal_page_last               150
_journal_paper_doi               10.1107/S0108768197010136
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C51 H64 N4 O7 '
_chemical_formula_sum            'C51 H64 N4 O7'
_chemical_formula_weight         845.06
_chemical_name_systematic
;
1,1,1-Tris(4-hydroxyphenyl)ethane-1,4,8,11-tetraazacyclotetradecane-methanol
(2/1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.694(13)
_cell_angle_beta                 89.656(14)
_cell_angle_gamma                86.468(12)
_cell_formula_units_Z            2
_cell_length_a                   8.2208(11)
_cell_length_b                   16.245(2)
_cell_length_c                   17.337(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      18.00
_cell_measurement_theta_min      10.05
_cell_volume                     2286.7(5)
_computing_cell_refinement       'SET4 and CELDIM (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1992)'
_computing_data_reduction        'DATRD2 in NRCVAX96 (Gabe et al., 1989)'
_computing_molecular_graphics
'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1996a), PLUTON (Spek 1996b)'
_computing_publication_material
'NRCVAX96, SHELXL93  and WordPerfect macro PRPCIF97 (Ferguson, 1997)'
_computing_structure_refinement  'NRCVAX96 and SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SOLVER in NRCVAX96'
_diffrn_ambient_temperature      294.0(10)
_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           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8108
_diffrn_reflns_theta_full        27.20
_diffrn_reflns_theta_max         27.20
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        'no decay, variation 1.0'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         8108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(Fo^2^) + (0.0569P)^2^], where P = (Fo^2^ +
2Fc^2^)/3
;
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                4835
_reflns_number_total             8108
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ab0380.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2286.6(5)
_cod_database_code               2105513