Metal Complexes with a New N4O3 Amine Pendant-Armed Macrocyclic Ligand: Synthesis, Characterization, Crystal Structures, and Fluorescence Studies
Manuel Vicente; Rufina Bastida; Carlos Lodeiro; Alejandro Macías; A. Jorge Parola; Laura Valencia; Sharon E. Spey; Inorganic Chemistry 42 (2003) 6768–6779; doi:10.1021/ic034245z

data_4312322
_publ_section_title
;
 Metal Complexes with a New N4O3 Amine Pendant-Armed Macrocyclic Ligand:
 Synthesis, Characterization, Crystal Structures, and Fluorescence Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6768
_journal_page_last               6779
_journal_paper_doi               10.1021/ic034245z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[PbL](ClO4)2'
_chemical_formula_sum            'C24 H36 Cl2 N4 O11 Pb'
_chemical_formula_weight         834.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.254(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6686(15)
_cell_length_b                   13.225(2)
_cell_length_c                   23.633(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3021.9(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6121
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    5.823
_exptl_absorpt_correction_T_max  0.3889
_exptl_absorpt_correction_T_min  0.2283
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs, Sheldrick, 1996'
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.3638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                4904
_reflns_number_total             6121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034245zsi20030306_112308_2.cif
_cod_data_source_block           '[PbL](ClO4)2'
_cod_original_cell_volume        3022.0(8)
_cod_database_code               4312322