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_7213334
_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            'C51.5 H70.5 Br2 Cl N2.5 O8'
_chemical_formula_weight         1047.87
_chemical_name_systematic
; 
11,23-dibromo-
 25,26,27,28-tetrapropoxycalix[4]arene-
 5,17-dicarboxylic acid-
 bis-diethylamine salt
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.394(6)
_cell_length_b                   23.820(6)
_cell_length_c                   27.882(7)
_cell_measurement_temperature    120(2)
_cell_volume                     11552(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.2705
_diffrn_reflns_av_sigmaI/netI    0.2966
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41459
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.479
_refine_diff_density_min         -1.829
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         11780
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      2.349
_refine_ls_R_factor_all          0.3482
_refine_ls_R_factor_gt           0.1662
_refine_ls_shift/su_max          4.021
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1205P)^2^+171.6719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3302
_refine_ls_wR_factor_ref         0.4240
_reflns_number_gt                3936
_reflns_number_total             11780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002409ksup1.cif
_cod_data_source_block           4(Et2NH)2,II
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C51.50 H70.50 Br2 Cl N2.50 O8'
_cod_database_code               7213334