Synthesis and Magnetic Properties of Four New (Cu-Ni)2 Tetranuclear Complexes of General Formula [Cu(oxpn)Ni(μ-NCS)(H2O)(aa)]2(X)2 (oxpn =N,N'-Bis(3-aminopropyl)oxamide; aa = Bidentate Amine; X = ClO4- or PF6-). Ferro- and Antiferromagnetic Alternation
Joan Ribas; Carmen Diaz; Ramon Costa; Javier Tercero; Xavier Solans; Mercé Font-Bardía; Helen Stoeckli-Evans; Inorganic Chemistry 37 (1998) 233–239; doi:10.1021/ic970899u

data_4322617
_publ_section_title
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 Synthesis and Magnetic Properties of Four New (Cu-Ni)2 Tetranuclear
 Complexes of General Formula [Cu(oxpn)Ni(\m-NCS)(H2O)(aa)]2(X)2 (oxpn
 =N,N'-Bis(3-aminopropyl)oxamide; aa = Bidentate Amine; X = ClO4- or
 PF6-). Ferro- and Antiferromagnetic Alternation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              233
_journal_page_last               239
_journal_paper_doi               10.1021/ic970899u
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_sum            'C15 H34 Cu F6 N7 Ni O3 P S'
_chemical_formula_weight         659.77
_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
_cell_angle_alpha                95.27(6)
_cell_angle_beta                 99.22(2)
_cell_angle_gamma                108.86(7)
_cell_formula_units_Z            2
_cell_length_a                   9.059(8)
_cell_length_b                   12.604(2)
_cell_length_c                   12.743(4)
_cell_measurement_reflns_used    13
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      16.6
_cell_measurement_theta_min      14.0
_cell_volume                     1342.9(14)
_computing_cell_refinement       'STADI4 (Stoe Cie GmbH, Darmstadt, Germany)'
_computing_data_collection       'STADI4 (Stoe Cie GmbH, Darmstadt, Germany)'
_computing_data_reduction        'X-RED (Stoe Cie GmbH, Darmstadt, Germany)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1995)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measurement_device       'Stoe AED2 4-circle diffractometer'
_diffrn_measurement_method       \w/2\Q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0417
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_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3518
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.702
_exptl_absorpt_correction_T_max  1.382
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   'empirical - DIFABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    none
_exptl_crystal_description       plates
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.413
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     320
_refine_ls_number_reflns         3518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.370
_refine_ls_restrained_S_obs      1.413
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_obs          0.0949
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+12.1570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1703
_refine_ls_wR_factor_obs         0.1674
_reflns_number_observed          3223
_reflns_number_total             3518
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970899u_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+12.1570P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+12.1570P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1342.9(13)
_cod_database_code               4322617