Calix[4]pyrroles Containing Deep Cavities and Fixed Walls. Synthesis, Structural Studies, and Anion Binding Properties of the Isomeric Products Derived from the Condensation of p-Hydroxyacetophenone and Pyrrole
Pavel Anzenbacher; Karolina Jursíková; Vincent M. Lynch; Philip A. Gale; Jonathan L. Sessler; Journal of the American Chemical Society 121 (1999) 11020–11021; doi:10.1021/ja993195n

data_4116607
_publ_section_title
;
 Calix[4]pyrroles Containing Deep Cavities and Fixed Walls. Synthesis,
 Structural Studies, and Anion Binding Properties of the Isomeric Products
 Derived from the Condensation of p-Hydroxyacetophenone and Pyrrole
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11020
_journal_page_last               11021
_journal_paper_doi               10.1021/ja993195n
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C50 H52 N4 O6'
_chemical_formula_weight         804.96
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.134(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8820(5)
_cell_length_b                   20.2050(6)
_cell_length_c                   19.7400(6)
_cell_measurement_temperature    153(2)
_cell_volume                     4189.7(3)
_computing_cell_refinement       'DENZO-SMN V0.93.0'
_computing_data_collection       'Collect, Nonius B.V., 1998'
_computing_data_reduction
;
  DENZO-SMN V0.93.0, Z. Otwinoski and W. Minor, "Processing of X-ray
  Diffraction Data Collected in Oscillation Mode", Methods in
  Enzymology, Volume 276, Macromolecular Crystallography, part A,
  307-326, 1997, C.W. Carter, jr. and R. W. Sweet, Eds., Academic
  Press.
;
_computing_molecular_graphics
;
Shelxtl-Plus V5.03, Siemens Analytical, 1994, Madison, WI
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14882
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       needles
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0028(5)
_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_all   1.079
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.151
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_obs          0.0582
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+2.3751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1288
_refine_ls_wR_factor_obs         0.1107
_reflns_number_observed          6309
_reflns_number_total             9391
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja993195n_2.cif
_cod_data_source_block
ethanol_adduct_of_the_alpha,alpha,alpha,alpha_adduct_of_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+2.3751P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+2.3751P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116607