Synthesis, Crystal Structure, and Magnetic Properties of the First Nonanuclear Lanthanide(III)-Copper(II) Complexes of Macrocyclic Oxamide [NaLn2Cu6] (Macrocyclic Oxamide = 1,4,8,11-Tetraazacyclotradecanne-2,3-dione, Ln = Pr, Nd)
Jin-Kui Tang; Yi-Zhi Li; Qing-Lun Wang; En-Qing Gao; Dai-Zheng Liao; Zong-Hui Jiang; Shi-Ping Yan; Peng Cheng; Liu-Fang Wang; Geng-Lin Wang; Inorganic Chemistry 41 (2002) 2188–2192; doi:10.1021/ic010674q

data_4317840
_publ_contact_author
;
  Dai-Zheng Liao
  Department of Chemistry, Nankai University, Tianjin 300071,China
;
_publ_contact_author_email       ' coord@nankai.edu.cn '
_publ_section_title
;
 Synthesis, Crystal Structure, and Magnetic Properties of the First
 Nonanuclear Lanthanide(III)-Copper(II) Complexes of Macrocyclic Oxamide
 [NaLn2Cu6] (Macrocyclic Oxamide =
 1,4,8,11-Tetraazacyclotradecanne-2,3-dione, Ln = Pr, Nd)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2188
_journal_page_last               2192
_journal_paper_doi               10.1021/ic010674q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C60 H136 Cl7 Cu6 N24 Na Nd2 O50'
_chemical_formula_weight         2934.79
_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                98.195(4)
_cell_angle_beta                 96.602(4)
_cell_angle_gamma                114.109(4)
_cell_formula_units_Z            1
_cell_length_a                   13.892(3)
_cell_length_b                   14.477(3)
_cell_length_c                   16.213(4)
_cell_measurement_temperature    298(2)
_cell_volume                     2891.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0074
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26192
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    2.221
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          1.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.354
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         13098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.354
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+1.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                12614
_reflns_number_total             13098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010674q_2.cif
_cod_data_source_block           2
_cod_database_code               4317840