Synthesis of a Calix[4]arene Derivative for Isolation of a Stable Cation Radical Salt for Use as a Colorimetric Sensor of Nitric Oxide
Rajendra Rathore; Sameh H. Abdelwahed; Ilia A. Guzei; Journal of the American Chemical Society 126 (2004) 13582–13583; doi:10.1021/ja0454900

data_4113081
_publ_section_title
;
 Synthesis of a Calix[4]arene Derivative for Isolation of a Stable Cation
 Radical Salt for Use as a Colorimetric Sensor of Nitric Oxide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13582
_journal_page_last               13583
_journal_paper_doi               10.1021/ja0454900
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C77 H90 Cl2 O12'
_chemical_formula_weight         1278.39
_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                94.4670(10)
_cell_angle_beta                 92.1880(10)
_cell_angle_gamma                107.8300(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8595(7)
_cell_length_b                   16.9450(10)
_cell_length_c                   17.3999(10)
_cell_measurement_temperature    173(2)
_cell_volume                     3590.7(4)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26830
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.9621
_exptl_absorpt_correction_T_min  0.9425
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         12608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0775P)^2^+0.8051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                8669
_reflns_number_total             12608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0454900si20040727_115711.cif
_cod_data_source_block           rathf
_cod_database_code               4113081