Synthesis and Structure of [2 x 2] Molecular Grid Copper(II) and Nickel(II) Complexes with a New Polydentate Oxime-Containing Schiff Base Ligand
Yurii S. Moroz; Kinga Kulon; Matti Haukka; Elżbieta Gumienna-Kontecka; Henryk Kozłowski; Franc Meyer; Igor O. Fritsky; Inorganic Chemistry 47 (2008) 5656–5665; doi:10.1021/ic702375h

data_4305178
_publ_contact_author             'Igor O.Fritsky'
_publ_contact_author_email       ifritsky@univ.kiev.ua
_publ_section_title
;
Synthesis and Structure of [2 x 2] Molecular Grid Copper(II) and
Nickel(II) Complexes with a New Polydentate Oxime-Containing Schiff Base
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5656
_journal_page_last               5665
_journal_paper_doi               10.1021/ic702375h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C44 H48 Cu4 N16 O16, 2(H2 O)'
_chemical_formula_sum            'C11 H13 Cu N4 O4.5'
_chemical_formula_weight         336.79
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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            8
_cell_length_a                   15.4644(10)
_cell_length_b                   15.4644(10)
_cell_length_c                   11.4200(4)
_cell_measurement_reflns_used    16074
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2731.1(3)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25942
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_T_max  0.8771
_exptl_absorpt_correction_T_min  0.7076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+3.9982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                2196
_reflns_number_total             3116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702375h-file003.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C11 H13 Cu N4 O4.50'
_cod_database_code               4305178