A cylindrical cavity with two different hydrogen-binding boundaries: the calix[4]arene skeleton screwed onto the meso-positions of the calix[4]pyrrole†
Bonomo, Lucia; Solari, Euro; Toraman, Gülsen; Scopelliti, Rosario; Floriani, Carlo; Latronico, Mario; Chemical Communications  (1999) 2413–; doi:10.1039/a907563a

data_7110724
_publ_section_title
;
 A cylindrical cavity with two different hydrogen-binding boundaries: the
 calix[4]arene skeleton screwed onto the meso-positions of the
 calix[4]pyrrole&#x2020;
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2413
_journal_paper_doi               10.1039/a907563a
_journal_year                    1999
_chemical_formula_moiety         'C48 H44 N4 O4, C4 H8 O, 3(C2 H4 O2)'
_chemical_formula_sum            'C58 H64 N4 O11'
_chemical_formula_weight         993.13
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.054(5)
_cell_length_b                   20.054(5)
_cell_length_c                   11.079(3)
_cell_measurement_reflns_used    '87 spots from the first image'
_cell_measurement_temperature    143(2)
_cell_volume                     3858.6(17)
_computing_cell_refinement       'marresearch, marHKL, release 1.9.1'
_computing_data_collection       'marresearch, mar345, release 1.2.11'
_computing_data_reduction        'marresearch, marHKL'
_computing_molecular_graphics    'Bruker, SHELXTL, release 5.1'
_computing_publication_material  'Bruker, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measurement_device_type  'mar345 IPDS'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13929
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(13)
_refine_ls_extinction_coef       0.0140(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         5796
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.4040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                4394
_reflns_number_total             5796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907563asup1.cif
_cod_data_source_block           1a.MeCOOH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P3(2)
_cod_database_code               7110724