Tetranuclear Copper(II) and Nickel(II) Cluster Complexes Derived by Self-Assembly from a Series of Tetradentate Diazine Ligands: Structural and Magnetic Studies
Craig J. Matthews; Karen Avery; Zhiqiang Xu; Laurence K. Thompson; Liang Zhao; David O. Miller; Kumar Biradha; Karen Poirier; Michael J. Zaworotko; Claire Wilson; Andrés E. Goeta; Judith A. K. Howard; Inorganic Chemistry 38 (1999) 5266–5276; doi:10.1021/ic990598f

data_4322401
_publ_section_title
;
 Tetranuclear Copper(II) and Nickel(II) Cluster Complexes Derived by
 Self-Assembly from a Series of Tetradentate Diazine Ligands: Structural
 and Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5266
_journal_page_last               5276
_journal_paper_doi               10.1021/ic990598f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C44 H54 Cl4 N24 Ni4 O28'
_chemical_formula_weight         1743.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   14.368(4)
_cell_length_b                   25.469(7)
_cell_length_c                   18.479(5)
_cell_measurement_reflns_used    614
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      14.42
_cell_volume                     6762(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT''
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       /w-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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43201
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   del-F
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8867
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0583P)^2^+5.5686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                5809
_reflns_number_total             8867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990598f_5.cif
_cod_data_source_block           zl39ab
_cod_database_code               4322401