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_4321382
_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
;
 (Ni 2+)2, C16 H31 N6 O1 1-, (Cl 1-)3
;
_chemical_formula_sum            'C16 H31 Cl3 N6 Ni2 O'
_chemical_formula_weight         547.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.142(5)
_cell_length_b                   10.307(4)
_cell_length_c                   18.692(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_volume                     2146.2(16)
_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
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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    0.0605
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3416
_diffrn_reflns_theta_full        64.22
_diffrn_reflns_theta_max         64.22
_diffrn_reflns_theta_min         3.97
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.785
_exptl_absorpt_correction_type   'refdelf (Walker and Stuart, 1983)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00000(12)
_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   0.743
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.743
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+35.7468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.1974
_reflns_number_gt                2859
_reflns_number_total             3416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0000799_2.cif
_cod_data_source_block           '[Ni2(LO)]Cl3'
_cod_original_sg_symbol_H-M      ' P 1 21/c 1'
_cod_database_code               4321382