Selective anion binding and solid-state host‒guest chemistry of an extended cavity calix[6]pyrrole
Turner, Boaz; Shterenberg, Alexander; Kapon, Moshe; Eichen, Yoav; Suwinska, Kinga; Chemical Communications  (2001) 13–; doi:10.1039/b007788g

data_7111147
_publ_section_title
;
 Selective anion binding and solid-state host--guest chemistry of an
 extended cavity calix[6]pyrrole
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              13
_journal_paper_doi               10.1039/b007788g
_journal_year                    2001
_chemical_formula_sum            'C82.5 H89 Cl12 N6 O9.5'
_chemical_formula_weight         1742.00
_chemical_melting_point          248
_chemical_name_systematic
; 
 1,1,3,3,5,5- meso- hexaphenyl- 2,2,4,4,6,6- meso- hexamethyl- calix[6]pyrrole
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.730(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7730(10)
_cell_length_b                   20.2090(10)
_cell_length_c                   26.2590(10)
_cell_measurement_reflns_used    82763
_cell_measurement_temperature    170.0(1)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.0
_cell_volume                     8983.6(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius (1997), KappaCCD Collect Program'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
; 
 Molecular Structure Corporation (1999). 
 ORTEP. TEXRAY Structure Analysis Package. 
 MSC, 3200 Research Forest Drive, The 
 Woodlands,TX 77381, USA.  
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170.0(1)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1739
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14385
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.426
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0061(7)
_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     1054
_refine_ls_number_reflns         14385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.2231
_refine_ls_R_factor_gt           0.1168
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1969P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3188
_refine_ls_wR_factor_ref         0.3653
_reflns_number_gt                5318
_reflns_number_total             14385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007788gsup1.cif
_cod_data_source_block           hexapyr170
_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_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C82.50 H89 Cl12 N6 O9.50'
_cod_database_code               7111147