Odd-numbered oxacalix[n]arenes (n = 5, 7): synthesis and solid-state structures.
Van Rossom, Wim; Robeyns, Koen; Ovaere, Magriet; Van Meervelt, Luc; Dehaen, Wim; Maes, Wouter; Organic letters 13 (2011) 126–129; doi:10.1021/ol1026969

data_1501889
_publ_section_title
;
 Odd-numbered oxacalix[n]arenes (n = 5, 7): synthesis and solid-state
 structures.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              126
_journal_page_last               129
_journal_paper_doi               10.1021/ol1026969
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C49 H32 N6 O7 S'
_chemical_formula_sum            'C49 H32 N6 O7 S'
_chemical_formula_weight         848.87
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.311(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0733(13)
_cell_length_b                   19.7051(16)
_cell_length_c                   14.1933(11)
_cell_measurement_reflns_used    1735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.05
_cell_measurement_theta_min      16.17
_cell_volume                     4084.9(6)
_computing_cell_refinement       'Bruker SAINT (SAINT, 1997)'
_computing_data_collection       'Bruker SMART (SMART, 1997)'
_computing_data_reduction        'Bruker SAINT (SAINT, 1997)'
_computing_molecular_graphics    'PLUTON (Spek, 1998)'
_computing_publication_material  'PLATON (Spek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       'omega and phi scan'
_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  0.1312
_diffrn_reflns_av_sigmaI/netI    0.0908
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27921
_diffrn_reflns_theta_full        50.54
_diffrn_reflns_theta_max         50.54
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            translucent
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     594
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1093P)^2^+0.0362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1875
_reflns_number_gt                2826
_reflns_number_total             4266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol1026969_si_002.cif
_cod_data_source_block           wim132
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1501889