Synthesis, Characterization, and X-ray Crystal Structures of Cyclam Derivatives. 8. Thermodynamic and Kinetic Appraisal of Lead(II) Chelation by Octadentate Carbamoyl-Armed Macrocycles1
François Cuenot; Michel Meyer; Enrique Espinosa; Roger Guilard; Inorganic Chemistry 44 (2005) 7895–7910; doi:10.1021/ic0508019

data_4309854
_publ_contact_author
; Pr. Roger Guilard,
  LIMSAG, CNRS UMR 5633, 
  Universit\'e de Bourgogne, Facult\'e des Sciences, 
  6 boulevard Gabriel, 21100 Dijon, 
  France 
;
_publ_contact_author_email       Roger.Guilard@u-bourgogne.fr
_publ_contact_author_fax         '+33 3 80 39 61 17'
_publ_contact_author_phone       '+33 3 80 39 61 11'
_publ_section_title
;
Synthesis, Characterization, and X-ray Crystal Structures of Cyclam
Derivatives. 8. Thermodynamic and Kinetic Appraisal of Lead(II) Chelation
by Octadentate Carbamoyl-Armed Macrocycles1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7895
_journal_page_last               7910
_journal_paper_doi               10.1021/ic0508019
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C18 H38 N8 O4, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C18 H42 N10 O12'
_chemical_formula_weight         590.62
_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                98.904(2)
_cell_angle_beta                 108.550(2)
_cell_angle_gamma                111.047(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5200(3)
_cell_length_b                   8.8830(3)
_cell_length_c                   10.6060(4)
_cell_measurement_reflns_used    5365
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.13
_cell_volume                     676.60(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5365
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.2490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                2728
_reflns_number_total             3446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0508019si20050804_090712_2.cif
_cod_data_source_block           ab126
_cod_database_code               4309854