Controllable selective functionalization of a cavitand via solid state photolysis of an encapsulated phenyl azide.
Wagner, Gerald; Arion, Vladimir B.; Brecker, Lothar; Krantz, Carsten; Mieusset, Jean-Luc; Brinker, Udo H.; Organic letters 11 (2009) 3056–3058; doi:10.1021/ol901122h

data_1504008
_publ_section_title
;
 Controllable selective functionalization of a cavitand via solid state
 photolysis of an encapsulated phenyl azide.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3056
_journal_page_last               3058
_journal_paper_doi               10.1021/ol901122h
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C84 H80 N8 O8, C6 H5 N3'
_chemical_formula_sum            'C90 H85 N11 O8'
_chemical_formula_weight         1448.69
_chemical_name_systematic
; 
C-Hexyl-6,10:12,16:18,22:24,4-O,O'-tetrakis(quinoxaline-
2,3-diyl)calix[4]resorcinarene phenyl azide adduct 
;
_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                70.524(2)
_cell_angle_beta                 88.842(3)
_cell_angle_gamma                77.787(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5021(9)
_cell_length_b                   15.7541(8)
_cell_length_c                   18.9376(11)
_cell_measurement_reflns_used    1419
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      2.32
_cell_volume                     3706.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD'
_diffrn_measurement_method       '\f-scan and \w-scan'
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62200
_diffrn_reflns_theta_full        25.58
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         13771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                9336
_reflns_number_total             13771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol901122h_si_001.cif
_cod_data_source_block           GEWAV101
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1504008