Synthesis of a Flexible Ligand for Assembling Two Metal Ions in Close Proximity. Crystal Structures of Binuclear Nickel and Copper Complexes
Paolo Dapporto; Mauro Formica; Vieri Fusi; Mauro Micheloni; Paola Paoli; Roberto Pontellini; Patrizia Rossi; Inorganic Chemistry 39 (2000) 4663–4665; doi:10.1021/ic0000799

data_4321381
_publ_contact_author             'Vieri Fusi'
_publ_contact_author_address
;
  Instiute of Chemical Sciences
  Univerity of Urbino
  P.za Rinascimento 6
  I-61029 Urbino, ITALY
;
_publ_contact_author_email       vieri@chim.uniurb.it
_publ_section_title
;
 Synthesis of a Flexible Ligand for Assembling Two Metal Ions in Close
 Proximity. Crystal Structures of Binuclear Nickel and Copper Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4663
_journal_page_last               4665
_journal_paper_doi               10.1021/ic0000799
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety
;
 (Cu 2+)2, C16 H31 N6 O1 1-, (H O 1-), (Cl O4 1-)2, H2 O
;
_chemical_formula_sum            'C16 H34 Cl2 Cu2 N6 O11'
_chemical_formula_weight         684.47
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.009(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.368(1)
_cell_length_b                   14.099(1)
_cell_length_c                   26.116(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_volume                     5250.9(8)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'Siemens P4'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_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 0.787
_diffrn_measured_fraction_theta_max 0.787
_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    0.0396
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6901
_diffrn_reflns_theta_full        64.20
_diffrn_reflns_theta_max         64.20
_diffrn_reflns_theta_min         3.41
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.458
_exptl_absorpt_correction_type   'REFDELF (WALKER and STUART, 1983)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00000(3)
_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   1.027
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         6901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          1.045
_refine_ls_shift/su_mean         0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+11.1719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                6153
_reflns_number_total             6901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0000799_1.cif
_cod_data_source_block           '[Cu2(L-O)(OH)](ClO4)2.H2O'
_cod_original_sg_symbol_H-M      ' P 21/a'
_cod_database_code               4321381