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_7022182
_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_formula_structural
;
[Ni2L2][ClO4]2n(EtOH)n(MECN)
;
_chemical_formula_sum            'C36 H60 Cl2 N6 Ni2 O8 S2'
_chemical_formula_weight         957.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.23(3)
_cell_angle_beta                 97.53(3)
_cell_angle_gamma                99.30(3)
_cell_formula_units_Z            2
_cell_length_a                   12.800(3)
_cell_length_b                   14.108(3)
_cell_length_c                   16.996(3)
_cell_measurement_temperature    203(2)
_cell_volume                     2822.3(13)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20993
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.9574
_exptl_absorpt_correction_T_min  0.8236
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0087(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   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9885
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.1987
_reflns_number_gt                6491
_reflns_number_total             9885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31973j.txt
_cod_data_source_block           4
_cod_original_cell_volume        2822.2(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7022182