Binuclear nickel complexes with an edge sharing bis(square-pyramidal) N3Ni(μ-S2)NiN3 core: synthesis, characterization, crystal structure and magnetic properties.
Lehmann, Ulrike; Lach, Jochen; Loose, Claudia; Hahn, Torsten; Kersting, Berthold; Kortus, Jens; Dalton transactions (Cambridge, England : 2003) 42 (2013) 987–996; doi:10.1039/c2dt31973j

data_7022183
_publ_section_title
;
 Binuclear nickel complexes with an edge sharing bis(square-pyramidal)
 N3Ni(\m-S2)NiN3 core: synthesis, characterization, crystal structure and
 magnetic properties.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              987
_journal_page_last               996
_journal_paper_doi               10.1039/c2dt31973j
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source
;
Crystals were obtained by recrystallization from MeCN/MeOH.
;
_chemical_formula_structural
;
[Ni2L2][BPh4]2(MeOH)
;
_chemical_formula_sum            'C85 H104 B2 N6 Ni2 O S2'
_chemical_formula_weight         1428.90
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   constr
_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                   16.917(3)
_cell_length_b                   23.635(5)
_cell_length_c                   19.856(4)
_cell_measurement_temperature    200(2)
_cell_volume                     7939(3)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       hemisphere
_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  0.1091
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25062
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.9718
_exptl_absorpt_correction_T_min  0.9036
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   STOE-X-AREA
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00041(14)
_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   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                3725
_reflns_number_total             7156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31973j.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7022183