Formation and conformational conversion of flattened partial cone oxygen bridged calix[2]arene[2]triazines.
Wang, Qi-Qiang; Wang, De-Xian; Zheng, Qi-Yu; Wang, Mei-Xiang; Organic letters 9 (2007) 2847–2850; doi:10.1021/ol0710008

data_1505444
_publ_section_title
;
 Formation and conformational conversion of flattened partial cone oxygen
 bridged calix[2]arene[2]triazines.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              2847
_journal_page_last               2850
_journal_paper_doi               10.1021/ol0710008
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C48 H54 N6 O6'
_chemical_formula_weight         810.97
_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
_cell_angle_alpha                89.89(3)
_cell_angle_beta                 107.15(3)
_cell_angle_gamma                90.21(3)
_cell_formula_units_Z            4
_cell_length_a                   14.451(3)
_cell_length_b                   17.782(4)
_cell_length_c                   19.083(4)
_cell_measurement_reflns_used    30835
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      1.12
_cell_volume                     4685.6(19)
_computing_cell_refinement       'Rapid Auto(Rigaku 2001)'
_computing_data_collection       'Rapid Auto(Rigaku 2001)'
_computing_data_reduction        'Rapid Auto(Rigaku 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Rigaku raxis Rapid IP'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30835
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9678
_exptl_absorpt_correction_T_min  0.9405
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.0097(11)
_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   1.236
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         20044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.2244
_refine_ls_R_factor_gt           0.1513
_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^)+(0.1361P)^2^+14.6725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4055
_refine_ls_wR_factor_ref         0.4439
_reflns_number_gt                12194
_reflns_number_total             20044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0710008si20070429_041126.cif
_cod_data_source_block           a
_cod_original_cell_volume        4685.7(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1505444