Calix[4]arene-5,17-dicarboxylic acids and their interactions with aliphatic amines. Part 2. A crystal engineering approach
Krebs, Frederik C.; Jørgensen, Mikkel; Journal of the Chemical Society, Perkin Transactions 2  (2000) 1935–; doi:10.1039/b002409k

data_7213330
_publ_section_title
;
 Calix[4]arene-5,17-dicarboxylic acids and their interactions with
 aliphatic amines. Part 2. A crystal engineering approach
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1935
_journal_paper_doi               10.1039/b002409k
_journal_year                    2000
_chemical_formula_sum            'C72 H87 N5 O8'
_chemical_formula_weight         1150.47
_chemical_name_systematic
; 
11,23-bis((E)-(2-phenyl-1-ethenyl)-
 25,26,27,28-tetrapropoxycalix[4]arene-5,17-
 dicarboxylic acid bis-
 1,4-diaza[2,2,2]bicyclooctane salt  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.75(3)
_cell_angle_beta                 93.04(3)
_cell_angle_gamma                110.93(3)
_cell_formula_units_Z            2
_cell_length_a                   13.062(3)
_cell_length_b                   13.325(3)
_cell_length_c                   20.365(4)
_cell_measurement_temperature    120(2)
_cell_volume                     3270.4(14)
_computing_cell_refinement       'SAINT Siemens'
_computing_data_collection       'SMART Siemens'
_computing_data_reduction        'SAINT Siemens'
_computing_molecular_graphics    'SHELXTL (Sheldrick)'
_computing_publication_material  'XCIF (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega scan, frame data integration'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3159
_diffrn_reflns_av_sigmaI/netI    0.5490
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34859
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         13338
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.4304
_refine_ls_R_factor_gt           0.1352
_refine_ls_shift/su_max          0.466
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1893P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3159
_refine_ls_wR_factor_ref         0.4616
_reflns_number_gt                2682
_reflns_number_total             13338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002409ksup1.cif
_cod_data_source_block           11(dabco)2
_cod_original_cell_volume        3270.4(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213330