Ni(II), Cu(II), and Zn(II) Dinuclear Metal Complexes with an Aza-Phenolic Ligand: Crystal Structures, Magnetic Properties, and Solution Studies
Elisabetta Berti; Andrea Caneschi; Carole Daiguebonne; Paolo Dapporto; Mauro Formica; Vieri Fusi; Luca Giorgi; Annalisa Guerri; Mauro Micheloni; Paola Paoli; Roberto Pontellini; Patrizia Rossi; Inorganic Chemistry 42 (2003) 348–357; doi:10.1021/ic0204070

data_4312917
_publ_contact_author             'Fusi Vieri'
_publ_contact_author_address
;
   Institute of Chemical Science
   University of Urbino
   P.zza Rinascimento, 6
   61029 Urbino, ITALY
;
_publ_contact_author_email       vieri@chim.uniurb.it
_publ_section_title
;
 Ni(II), Cu(II), and Zn(II) Dinuclear Metal Complexes with an Aza-Phenolic
 Ligand: Crystal Structures, Magnetic Properties, and Solution Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              348
_journal_page_last               357
_journal_paper_doi               10.1021/ic0204070
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
'(Ni 2+)2, (C11 H18 N3 O1 1-)2, (Cl O4 1-)2, (H2 O)'
_chemical_formula_sum            'C22 H38 Cl2 N6 Ni2 O11'
_chemical_formula_weight         750.90
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2ac 2a'
_symmetry_space_group_name_H-M   'P 21 c a'
_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                   15.242(2)
_cell_length_b                   10.593(2)
_cell_length_c                   19.072(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3079.3(10)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'Siemens P4'
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare,1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2891
_diffrn_reflns_theta_full        64.17
_diffrn_reflns_theta_max         64.17
_diffrn_reflns_theta_min         4.17
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.687
_exptl_absorpt_correction_type   'REFDELF (WALKER and STUART, 1983)'
_exptl_crystal_colour            greenblue
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.00003(8)
_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   0.1097
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.1097
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+2.4757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                2690
_reflns_number_total             2891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0204070_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P c 21 b'
_cod_database_code               4312917