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_4116606
_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            'C56 H58 N6 O4'
_chemical_formula_weight         879.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.288(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0292(4)
_cell_length_b                   19.0713(6)
_cell_length_c                   16.8933(5)
_cell_measurement_temperature    153(2)
_cell_volume                     4811.9(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17592
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.077
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             1872
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0048(4)
_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   1.030
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         10888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+2.5706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1141
_refine_ls_wR_factor_obs         0.0991
_reflns_number_observed          7782
_reflns_number_total             10888
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja993195n_1.cif
_cod_data_source_block           methcalx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+2.5706P] 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^)+(0.0316P)^2^+2.5706P] 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               4116606