Calix[6]arene Derivatives Selectively Functionalized at Alternate Sites on the Smaller Rim with 2-Phenylpyridine and 2-Fluorenylpyridine Substituents to Provide Deep Cavities
Xianshun Zeng; Andrei S. Batsanov; Martin R. Bryce; Journal of Organic Chemistry 71 (2006) 9589–9594; doi:10.1021/jo0614341

data_4022175
_publ_contact_author             'Andrei S.Batsanov'
_publ_contact_author_email       a.s.batsanov@durham.ac.uk
_publ_section_title
;
 Calix[6]arene Derivatives Selectively Functionalized at Alternate
 Sites on the Smaller Rim with 2-Phenylpyridine and
 2-Fluorenylpyridine Substituents to Provide Deep Cavities
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9589
_journal_page_last               9594
_journal_paper_doi               10.1021/jo0614341
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C105 H117 N3 O6,2.75(C H2 Cl2),2(C2 H6 O)'
_chemical_formula_sum            'C111.75 H134.5 Cl5.5 N3 O8'
_chemical_formula_weight         1842.70
_chemical_name_systematic
; 5,11,17,23,29,35-hexa-tert-butyl-37,39,41-
tris{4-(2-pyridyl)phenoxy}-38,40,42-trimethoxycalix[6]arene 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.85(1)
_cell_angle_beta                 94.80(1)
_cell_angle_gamma                119.60(1)
_cell_formula_units_Z            4
_cell_length_a                   21.979(2)
_cell_length_b                   22.020(2)
_cell_length_c                   26.603(3)
_cell_measurement_reflns_used    7110
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.21
_cell_volume                     10217.2(17)
_computing_cell_refinement       'SAINT version 6.02A (Bruker, 2001)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_solution    'OLEX 2 (Dolomanov & Puschman, 2006)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 6K CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.1118
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            118524
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             3934
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2337
_refine_ls_number_reflns         46985
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1870
_refine_ls_R_factor_gt           0.1029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1780P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2869
_refine_ls_wR_factor_ref         0.3302
_reflns_number_gt                22231
_reflns_number_total             46985
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo0614341si20060710_081211.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4022175