Unexpected Single-Step Formation of 1,2-anti-Heterodisubstituted Calix[4]arenes upon Alkylation of a Tribenzoyl Precursor
Arjan W. Kleij; Beatriz Souto; César J. Pastor; Pilar Prados; Javier de Mendoza; Journal of Organic Chemistry 68 (2003) 8711–8714; doi:10.1021/jo035150h

data_4022558
_publ_section_title
;
 Unexpected Single-Step Formation of 1,2-anti-Heterodisubstituted
 Calix[4]arenes upon Alkylation of a Tribenzoyl Precursor
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8711
_journal_page_last               8714
_journal_paper_doi               10.1021/jo035150h
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C58 H65 I O5'
_chemical_formula_weight         969.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.0333(10)
_cell_length_b                   19.0258(11)
_cell_length_c                   28.1843(13)
_cell_measurement_temperature    296(2)
_cell_volume                     10206.2(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1191
_diffrn_reflns_av_sigmaI/netI    0.1293
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32087
_diffrn_reflns_theta_full        70.43
_diffrn_reflns_theta_max         70.43
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    5.289
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisma
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         12650
_refine_ls_number_restraints     1185
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.1759
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0972P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.2082
_reflns_number_gt                5196
_reflns_number_total             12650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo035150hsi20030807_060313.cif
_cod_data_source_block           orto_abs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
;
_cod_database_code               4022558