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_7110725
_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         'C76 H64 N8 O8, 5(C3 H6 O)'
_chemical_formula_sum            'C91 H94 N8 O13'
_chemical_formula_weight         1507.74
_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'
_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                 94.400(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3580(19)
_cell_length_b                   19.927(3)
_cell_length_c                   35.860(4)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      5.0
_cell_volume                     8092(2)
_computing_cell_refinement       'Kuma, CrysAlis, release 1.6.0'
_computing_data_collection       'Kuma, KM4CCD, release 1.5.9'
_computing_data_reduction        'Kuma, CrysAlis'
_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
'Kuma diffractometer equipped with CCD area detector'
_diffrn_measurement_method
'2 runs (110 frames each) using omega scan, 1 run (300 frames) using phi scan'
_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  0.1889
_diffrn_reflns_av_sigmaI/netI    0.1348
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            37534
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         9923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.2190
_refine_ls_R_factor_gt           0.1119
_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^)+(0.1122P)^2^+34.0475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2542
_refine_ls_wR_factor_ref         0.3308
_reflns_number_gt                4534
_reflns_number_total             9923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907563asup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        8093(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110725