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_4027690
_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            'C43 H46.5 Cl5 N13 Ni O11'
_chemical_formula_weight         1157.39
_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                96.018(3)
_cell_angle_beta                 93.271(3)
_cell_angle_gamma                92.071(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7471(5)
_cell_length_b                   13.9306(5)
_cell_length_c                   15.8655(6)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.11
_cell_volume                     2794.70(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
XP, Shelxtl-Plus Version 5.1, Bruker AXS, 1998.
;
_computing_publication_material
;
XCIF, Shelxtl-Plus Version 5.1, Bruker AXS, 1998.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      104(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_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    0.0803
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9818
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.9378
_exptl_absorpt_correction_T_min  0.8808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       prism
_exptl_crystal_F_000             1193
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         9818
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0677
_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^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1633
_reflns_number_gt                6904
_reflns_number_total             9818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301528f_si_002_6.cif
_cod_data_source_block           1-Ni(ClO4)2
_cod_original_formula_sum        'C43 H46.50 Cl5 N13 Ni O11'
_cod_database_code               4027690