New Dinuclear Nickel(II) Complexes: Synthesis, Structure, Electrochemical, and Magnetic Properties
Dmitry Yakhvarov; Ekaterina Trofimova; Oleg Sinyashin; Olga Kataeva; Yulia Budnikova; Peter Lönnecke; Evamarie Hey-Hawkins; Andreas Petr; Yulia Krupskaya; Vladislav Kataev; Rüdiger Klingeler; Bernd Büchner; Inorganic Chemistry 50 (2011) 4553–4558; doi:10.1021/ic2002546

data_4325078
_publ_section_title
;
 New Dinuclear Nickel(II) Complexes: Synthesis, Structure,
 Electrochemical, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4553
_journal_page_last               4558
_journal_paper_doi               10.1021/ic2002546
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C58 H56 Br2 N8 Ni2 O4 P2'
_chemical_formula_weight         1268.29
_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                 109.31(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.908(1)
_cell_length_b                   15.051(1)
_cell_length_c                   16.906(1)
_cell_measurement_reflns_used    362
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      22.44
_cell_measurement_theta_min      3.66
_cell_volume                     2859.6(4)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Schakal-99 (E.Keller 1999)'
_computing_publication_material  'XCIF 6.12 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.806
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39701
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    2.165
_exptl_absorpt_correction_T_max  0.4934
_exptl_absorpt_correction_T_min  0.3126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03.(Sheldrick,Bruker AXS Inc.,2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.67
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0284P)^2^+2.5105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                4468
_reflns_number_total             5829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2002546_si_004.cif
_cod_data_source_block           bud2
_cod_original_cell_volume        2859.6(3)
_cod_database_code               4325078