Synthesis, Structure and Metal Binding Property of Internally 1,3-Arylene-Bridged Azacalix[6]aromatics
Yi-Xin Fang; Liang Zhao; De-Xian Wang; Mei-Xiang Wang; Journal of Organic Chemistry 77 (2012) 10073–10082; doi:10.1021/jo301528f

data_4027686
_publ_section_title
;
 Synthesis, Structure and Metal Binding Property of Internally
 1,3-Arylene-Bridged Azacalix[6]aromatics
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              10073
_journal_page_last               10082
_journal_paper_doi               10.1021/jo301528f
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C40.25 H34.5 Cl0.5 N12'
_chemical_formula_weight         704.02
_chemical_name_systematic
; 
 ? 
;
_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                109.330(8)
_cell_angle_beta                 101.227(7)
_cell_angle_gamma                98.434(7)
_cell_formula_units_Z            2
_cell_length_a                   10.6023(9)
_cell_length_b                   13.3109(12)
_cell_length_c                   13.4391(12)
_cell_measurement_temperature    100
_cell_volume                     1709.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8335
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9697
_exptl_absorpt_correction_T_min  0.9407
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             737
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0500P)^2^+2.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                6515
_reflns_number_total             8335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301528f_si_002_2.cif
_cod_data_source_block           Compound2
_cod_original_formula_sum        'C40.25 H34.50 Cl0.50 N12'
_cod_database_code               4027686