Oxamato-Bridged Trinuclear NiIICuIINiII Complexes with Irregular Spin State Structures and a Binuclear NiIICuII Complex with an Unusual Supramolecular Structure: Crystal Structure and Magnetic Properties
En-Qing Gao; Jin-Kui Tang; Dai-Zheng Liao; Zong-Hui Jiang; Shi-Ping Yan; Geng-Lin Wang; Inorganic Chemistry 40 (2001) 3134–3140; doi:10.1021/ic001023h

data_4319816
_publ_contact_author
;
 Dai-Zheng Liao
 Department of Chemistry, Nankai University, Tianjin 300071,China
;
_publ_contact_author_email       ' coord@sun.nankai.edu.cn '
_publ_section_title
;
 Oxamato-Bridged Trinuclear NiIICuIINiII Complexes with Irregular Spin
 State Structures and a Binuclear NiIICuII Complex with an Unusual
 Supramolecular Structure: Crystal Structure and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3134
_journal_page_last               3140
_journal_paper_doi               10.1021/ic001023h
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C39 H78 Cl2 Cu N10 Ni2 O14'
_chemical_formula_weight         1162.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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                   35.376(4)
_cell_length_b                   10.7433(11)
_cell_length_c                   14.3949(14)
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.03
_cell_measurement_theta_min      2.22
_cell_volume                     5470.9(10)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       \w
_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  0.1041
_diffrn_reflns_av_sigmaI/netI    0.1273
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18723
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        4.7
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.8089
_exptl_absorpt_correction_T_min  0.7092
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         7773
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1458
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                3849
_reflns_number_total             7773
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001023h_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        5470.8(10)
_cod_database_code               4319816