New Types of Heterospin Complexes from trans-Oxamido-Bridged Copper(II) Binuclear Units and Nitronyl Nitroxide Radicals: Crystal Structure and Magnetic Characterization
Zhiliang Liu; Zhengliang Lü; Deqing Zhang; Zonghui Jiang; Licun Li; Caiming Liu; Daoben Zhu; Inorganic Chemistry 43 (2004) 6620–6627; doi:10.1021/ic049247d

data_4311755
_publ_section_title
;
 New Types of Heterospin Complexes from trans-Oxamido-Bridged Copper(II)
 Binuclear Units and Nitronyl Nitroxide Radicals: Crystal Structure and
 Magnetic Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6620
_journal_page_last               6627
_journal_paper_doi               10.1021/ic049247d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C17 H26 Cl Cu N5 O9'
_chemical_formula_weight         543.42
_chemical_name_systematic
; 
 ? 
;
_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                 98.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.040(3)
_cell_length_b                   23.159(5)
_cell_length_c                   7.572(2)
_cell_measurement_reflns_used    18786
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      1.56
_cell_volume                     2262.9(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.624
_diffrn_measured_fraction_theta_max 0.624
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       'phi and omega 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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9185
_diffrn_reflns_theta_full        32.02
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  1.1663
_exptl_absorpt_correction_T_min  0.7901
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            darkblue
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.291
_refine_ls_extinction_coef       0.0104(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          9.310
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                2857
_reflns_number_total             4910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049247dsi20040610_073414_1.cif
_cod_data_source_block           1(complex1)
_cod_database_code               4311755