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_7111148
_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            'C90.5 H81.5 N9 O6'
_chemical_formula_weight         1391.15
_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                 115.405(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.4550(5)
_cell_length_b                   19.7620(8)
_cell_length_c                   22.0270(8)
_cell_measurement_temperature    293(2)
_cell_volume                     7649.8(5)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       KappaCCD
_computing_data_reduction        maXus
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method
;
'114 frames via \f rotation and 183 frames via \o rotation 
(rotation angle 1.5\%) and 2 x 150s per \%'
;
_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  0.038
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16018
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2942
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0013(2)
_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   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         7929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+6.1157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                5823
_reflns_number_total             15694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007788gsup1.cif
_cod_data_source_block           yoav18
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C90.50 H81.50 N9 O6'
_cod_database_code               7111148