New Fluorogenic Dansyl-Containing Calix[4]arene in the Partial Cone Conformation for Highly Sensitive and Selective Recognition of Lead(II)
Nicole M. Buie; Vladimir S. Talanov; Raymond J. Butcher; Galina G. Talanova; Inorganic Chemistry 47 (2008) 3549–3558; doi:10.1021/ic7018346

data_4304348
_publ_section_title
;
New Fluorogenic Dansyl-Containing Calix[4]arene in the Partial
Cone Conformation for Highly Sensitive and Selective Recognition of Lead(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3549
_journal_page_last               3558
_journal_paper_doi               10.1021/ic7018346
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C246 H298 N8 O40 Pb4 S4,4(C2 H3 N), 2(C H3)'
_chemical_formula_sum            'C256 H316 N12 O40 Pb4 S4'
_chemical_formula_weight         5158.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2504(6)
_cell_length_b                   30.5529(7)
_cell_length_c                   41.1767(10)
_cell_measurement_reflns_used    18323
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      30.6768
_cell_measurement_theta_min      4.5525
_cell_volume                     27992.5(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_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      203(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f and \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  0.1701
_diffrn_reflns_av_sigmaI/netI    0.2150
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            113411
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         4.56
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             10592
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.117
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1375
_refine_ls_number_reflns         23504
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.2038
_refine_ls_R_factor_gt           0.0849
_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^)+(0.0519P)^2^+411.3542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.2191
_reflns_number_gt                10830
_reflns_number_total             23504
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic7018346-file015.cif
_cod_data_source_block           dfpb1
_cod_database_code               4304348