Synthesis of 9,10-Bis-ketoenaminoanthryl and 9,10-Bis-isoxazolylanthryl Linked Biscalix[4]arenes: Atropisomers and Molecular Recognitions
Chia-Chen Tsai; I-Ting Ho; Jean-Ho Chu; Li-Ching Shen; Shou-Ling Huang; Wen-Sheng Chung; Journal of Organic Chemistry 77 (2012) 2254–2262; doi:10.1021/jo2024784

data_4027018
_publ_section_title
;
 Synthesis of 9,10-Bis-ketoenaminoanthryl and 9,10-Bis-isoxazolylanthryl
 Linked Biscalix[4]arenes: Atropisomers and Molecular Recognitions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2254
_journal_page_last               2262
_journal_paper_doi               10.1021/jo2024784
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C137 H155 Cl3 N4 O16'
_chemical_formula_weight         2220.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.311(4)
_cell_angle_beta                 81.842(5)
_cell_angle_gamma                78.038(5)
_cell_formula_units_Z            1
_cell_length_a                   11.9430(8)
_cell_length_b                   16.0684(10)
_cell_length_c                   16.8946(8)
_cell_measurement_reflns_used    8254
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.2436
_cell_measurement_theta_min      2.8269
_cell_volume                     3121.4(3)
_computing_cell_refinement
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_collection
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_reduction
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29213
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         68.00
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.774
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.333
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.333
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.1173
_refine_ls_shift/su_max          0.008
_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          0.3066
_refine_ls_wR_factor_ref         0.3222
_reflns_number_gt                8416
_reflns_number_total             11277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2024784_si_002.cif
_cod_data_source_block           ic13467
_cod_database_code               4027018