Two new salts containing bis(maleonitriledithiolate)nickel(III)/copper(II) anion and substituted N,N'-dibenzylpiperidinium: Syntheses, crystal structures and magnetic properties
Ya-Lan Hu; Li-Bo Liang; Le-Min Yang; Jin-Fang Liu; Wei-Qiang Chen; Jia-Rong Zhou; Xiao-Ping Liu; Chun-Lin Ni; Inorganica Chimica Acta 392 (2012) 410–416; doi:10.1016/j.ica.2012.05.022

data_1512637
_publ_section_title
;
 Two new salts containing
 bis(maleonitriledithiolate)nickel(III)/copper(II) anion and substituted
 N,N'-dibenzylpiperidinium: Syntheses, crystal structures and magnetic
 properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              410
_journal_page_last               416
_journal_paper_doi               10.1016/j.ica.2012.05.022
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         '2(C19 H24 N), C8 Cu N4 S4'
_chemical_formula_sum            'C46 H48 Cu N6 S4'
_chemical_formula_weight         876.68
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.1710(10)
_cell_angle_beta                 89.7270(10)
_cell_angle_gamma                82.2810(10)
_cell_formula_units_Z            1
_cell_length_a                   9.0632(12)
_cell_length_b                   11.0030(14)
_cell_length_c                   11.4379(15)
_cell_measurement_reflns_used    5125
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.27
_cell_volume                     1106.0(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART(Bruker, 2000)'
_computing_data_reduction        'SAINT(Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL(Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w 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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7958
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_correction_T_min  0.8573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             459
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+0.7280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                3459
_reflns_number_total             3867
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2012-392-410-416-1.cif
_cod_data_source_block           Cu(mnt)
_cod_database_code               1512637