New dinuclear nickel(II) and iron(II) complexes with a macrocyclic ligand containing a N6S2 donor-set: synthesis, structural, MALDI-TOF-MS, magnetic and spectroscopic studies.
Núñez, Cristina; Bastida, Rufina; Macías, Alejandro; Valencia, Laura; Ribas, Joan; Capelo, José Luis; Lodeiro, Carlos; Dalton transactions (Cambridge, England : 2003) 39 (2010) 7673–7683; doi:10.1039/c0dt00182a

data_7026078
_publ_section_title
;
 New dinuclear nickel(II) and iron(II) complexes with a macrocyclic ligand
 containing a N6S2 donor-set: synthesis, structural, MALDI-TOF-MS,
 magnetic and spectroscopic studies.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7673
_journal_page_last               7683
_journal_paper_doi               10.1039/c0dt00182a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety
'[Ni2 (C22 H34 N6 S2) (CH3CN)4](BF4)4 . 3.5 (CH3CN)'
_chemical_formula_sum            'C18.5 H28.25 B2 F8 N6.75 Ni S'
_chemical_formula_weight         609.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.84
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.079
_cell_length_b                   18.517
_cell_length_c                   13.181
_cell_measurement_reflns_used    1805
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.62
_cell_measurement_theta_min      2.88
_cell_volume                     2896.895
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_computing_data_reduction        'BRUKER SHELXTL'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  'Wingx publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR-92 (Altornare, Cascarano, Giacovazzo, and Gualardi, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24504
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.7584
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            mauve
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1250
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         5899
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                3613
_reflns_number_total             5899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00182a.txt
_cod_data_source_block           ba19cn2n
_cod_original_cell_volume        2897.0
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C18.50 H28.25 B2 F8 N6.75 Ni S'
_cod_database_code               7026078