Synthesis and Structure of Oxacalix[2]arene[2]triazines of an Expanded π-Electron-Deficient Cavity and Their Interactions with Anions
Sen Li; Shi-Xin Fa; Qi-Qiang Wang; De-Xian Wang; Mei-Xiang Wang; Journal of Organic Chemistry 77 (2012) 1860–1867; doi:10.1021/jo2024448

data_4026974
_publ_section_title
;
 Synthesis and Structure of Oxacalix[2]arene[2]triazines of an Expanded
 \p-Electron-Deficient Cavity and Their Interactions with Anions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1860
_journal_page_last               1867
_journal_paper_doi               10.1021/jo2024448
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C44 H30 Cl2 N12 O12'
_chemical_formula_sum            'C44 H30 Cl2 N12 O12'
_chemical_formula_weight         989.70
_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                 95.313(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.809(3)
_cell_length_b                   17.516(3)
_cell_length_c                   20.801(4)
_cell_measurement_reflns_used    817
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.17
_cell_volume                     5009.7(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18865
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.9278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         9079
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0966
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2366
_refine_ls_wR_factor_ref         0.2598
_reflns_number_gt                5328
_reflns_number_total             9079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2024448_si_002.cif
_cod_data_source_block           sa959
_cod_original_cell_volume        5009.8(17)
_cod_database_code               4026974