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_4027688
_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_moiety         'C41 H41 Co N13 O2, 3(C H4 O), Cl4 Co'
_chemical_formula_sum            'C44 H53 Cl4 Co2 N13 O5'
_chemical_formula_weight         1103.65
_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                101.482(3)
_cell_angle_beta                 91.641(4)
_cell_angle_gamma                99.266(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2033(19)
_cell_length_b                   13.486(3)
_cell_length_c                   18.280(4)
_cell_measurement_reflns_used    7630
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.56
_cell_volume                     2428.1(9)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19420
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.9357
_exptl_absorpt_correction_T_min  0.8234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0647P)^2^+4.2772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                8493
_reflns_number_total             9791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301528f_si_002_4.cif
_cod_data_source_block           1-CoCl2
_cod_original_cell_volume        2428.2(9)
_cod_database_code               4027688