Synthesis of Upper-Rim Allyl- and p-Methoxyphenylazocalix[4]arenes and Their Efficiencies in Chromogenic Sensing of Hg^2+^ Ion
I-Ting Ho; Gene-Hsiang Lee; Wen-Sheng Chung; Journal of Organic Chemistry 72 (2007) 2434–2442; doi:10.1021/jo062280s

data_4022739
_publ_section_title
;
 Synthesis of Upper-Rim Allyl- and p-Methoxyphenylazocalix[4]arenes
 and Their Efficiencies in Chromogenic Sensing of Hg^2+^ Ion
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2434
_journal_page_last               2442
_journal_paper_doi               10.1021/jo062280s
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C52 H52 Cl3 N4 O8 S2'
_chemical_formula_weight         1031.45
_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                67.770(1)
_cell_angle_beta                 70.213(1)
_cell_angle_gamma                74.126(1)
_cell_formula_units_Z            2
_cell_length_a                   12.7090(5)
_cell_length_b                   13.4048(5)
_cell_length_c                   16.4736(6)
_cell_measurement_reflns_used    5944
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.19
_cell_volume                     2410.16(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31834
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_correction_T_min  0.8882
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange-yello
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         11046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+3.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2048
_reflns_number_gt                8887
_reflns_number_total             11046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo062280ssi20061104_013334.cif
_cod_data_source_block           ic11545
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4022739