Synthesis, Characterization, and X-ray Crystal Structures of Cyclam Derivatives. 5. Copper(II) Binding Studies of a Pyridine-Strapped 5,12-Dioxocyclam-Based Macrobicycle1
Michel Meyer; Laurent Frémond; Enrique Espinosa; Roger Guilard; Zhongping Ou; Karl M. Kadish; Inorganic Chemistry 43 (2004) 5572–5587; doi:10.1021/ic049518k

data_4311500
_publ_contact_author
;
  Pr. Roger Guilard,
  LIMSAG, CNRS UMR 5633, 
  Universite de Bourgogne, Faculte 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. 5. Copper(II) Binding Studies of a Pyridine-Strapped
 5,12-Dioxocyclam-Based Macrobicycle1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5572
_journal_page_last               5587
_journal_paper_doi               10.1021/ic049518k
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C17 H24 Cu N5 O2,Cl O4,H2 O'
_chemical_formula_sum            'C17 H26 Cl Cu N5 O7'
_chemical_formula_weight         511.42
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.0150(3)
_cell_length_b                   13.6120(5)
_cell_length_c                   18.6620(6)
_cell_measurement_reflns_used    13042
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      33.29
_cell_measurement_theta_min      1.85
_cell_volume                     2036.03(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13042
_diffrn_reflns_theta_full        33.29
_diffrn_reflns_theta_max         33.29
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         7067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+2.1942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                6039
_reflns_number_total             7067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049518ksi20040616_110903_1.cif
_cod_data_source_block           lf084
_cod_database_code               4311500