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_4319814
_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            'C27 H44 Cu N6 Ni O7'
_chemical_formula_weight         686.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.622(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.159(4)
_cell_length_b                   15.210(5)
_cell_length_c                   17.271(6)
_cell_measurement_reflns_used    4873
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.36
_cell_volume                     3193.9(19)
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12950
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        4.75
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_T_max  0.8281
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refinement
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0856P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                3852
_reflns_number_total             5632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001023h_1.cif
_cod_data_source_block           5
_cod_original_cell_volume        3193.8(19)
_cod_database_code               4319814