Efficient fragment coupling approaches toward large oxacalix[n]arenes (n = 6, 8).
Van Rossom, Wim; Ovaere, Margriet; Van Meervelt, Luc; Dehaen, Wim; Maes, Wouter; Organic letters 11 (2009) 1681–1684; doi:10.1021/ol900116h

data_1503814
_publ_section_title
;
 Efficient fragment coupling approaches toward large oxacalix[n]arenes (n
 = 6, 8).
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1681
_journal_page_last               1684
_journal_paper_doi               10.1021/ol900116h
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C68 H48 N8 O8'
_chemical_formula_sum            'C68 H48 N8 O8'
_chemical_formula_weight         1105.14
_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
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_cell_angle_beta                 104.689(7)
_cell_angle_gamma                91.598(8)
_cell_formula_units_Z            1
_cell_length_a                   10.2187(11)
_cell_length_b                   10.7224(12)
_cell_length_c                   12.9364(13)
_cell_measurement_reflns_used    1215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.30
_cell_measurement_theta_min      3.56
_cell_volume                     1358.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Pluton
_computing_publication_material  Platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'crossed Goebel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23684
_diffrn_reflns_theta_full        71.30
_diffrn_reflns_theta_max         71.30
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0000P)^2^+0.3014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                4046
_reflns_number_total             5186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol900116h_si_002.cif
_cod_data_source_block           wim57
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