Photochemical Cycloisomerizations via 7-exo-dig Reactions on a Calix[4]arene Scaffold
Hassan Al-Saraierh; David O. Miller; Paris E. Georghiou; Journal of Organic Chemistry 72 (2007) 4532–4535; doi:10.1021/jo070236m

data_4022916
_publ_section_title
;
 Photochemical Cycloisomerizations via 7-exo-dig Reactions
 on a Calix[4]arene Scaffold
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4532
_journal_page_last               4535
_journal_paper_doi               10.1021/jo070236m
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C61 H64 Cl3 O2'
_chemical_formula_weight         935.47
_chemical_name_systematic
; 
 ? 
;
_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                 106.986(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.008(3)
_cell_length_b                   24.042(4)
_cell_length_c                   17.079(3)
_cell_measurement_temperature    113(2)
_cell_volume                     5108.4(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0916
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24970
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.8969
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0019(9)
_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   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.2157
_refine_ls_R_factor_gt           0.1636
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1286P)^2^+18.9073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3557
_refine_ls_wR_factor_ref         0.3895
_reflns_number_gt                5940
_reflns_number_total             8989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070236msi20070204_123326.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4022916