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_4116609
_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            'C70 H95 F N6 O6'
_chemical_formula_weight         1135.52
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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                 92.901(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1593(4)
_cell_length_b                   11.2873(4)
_cell_length_c                   25.7805(7)
_cell_measurement_temperature    153(2)
_cell_volume                     3243.11(19)
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12926
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       lathes
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          .12
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .20
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.43(130)
_refine_ls_extinction_coef       0.0075(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_all   1.063
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         12919
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_obs          0.0785
_refine_ls_shift/esd_max         -0.045
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+3.0506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1751
_refine_ls_wR_factor_obs         0.1492
_reflns_number_observed          8207
_reflns_number_total             12919
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja993195n_4.cif
_cod_data_source_block           C70H95FN6O6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+3.0506P] 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^)+(0.0442P)^2^+3.0506P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3243.1(2)
_cod_database_code               4116609