Dinuclear Cu(II) Complexes of Isomeric Bis-(3-acetylacetonate)benzene Ligands: Synthesis, Structure, and Magnetic Properties
Marzio Rancan; Alessandro Dolmella; Roberta Seraglia; Simonetta Orlandi; Silvio Quici; Lorenzo Sorace; Dante Gatteschi; Lidia Armelao; Inorganic Chemistry 51 (2012) 5409–5416; doi:10.1021/ic3003806

data_4329129
_publ_contact_author_address
;
CNR-ISTM, 
Dipartimento di Scienze Chimiche, 
Universita degli Studi di Padova, 
Via Marzolo 1, 35131 Padova, Italy
;
_publ_contact_author_email       marzio.rancan@unipd.it
_publ_contact_author_name        'Marzio Rancan'
_publ_contact_author_phone       '+39 0498275188'
_publ_section_title
;
 Dinuclear Cu(II) Complexes of Isomeric Bis-(3-acetylacetonate)benzene
 Ligands: Synthesis, Structure, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5409
_journal_page_last               5416
_journal_paper_doi               10.1021/ic3003806
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '2(Cl O4), 2(C2 H6 O S), C40 H44 Cu2 N4 O6 S2'
_chemical_formula_sum            'C44 H56 Cl2 Cu2 N4 O16 S4'
_chemical_formula_weight         1223.15
_chemical_name_common            'compound 2'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                78.327(4)
_cell_angle_beta                 81.739(4)
_cell_angle_gamma                64.461(4)
_cell_formula_units_Z            2
_cell_length_a                   12.3340(6)
_cell_length_b                   13.2732(5)
_cell_length_c                   18.3581(10)
_cell_measurement_reflns_used    6540
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      51.1173
_cell_measurement_theta_min      3.7308
_cell_volume                     2650.3(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140.0
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega -102.00   -6.00   1.0000    4.4500
omega____ theta____ kappa____ phi______ frames
    -      -31.1115  -38.0000   90.0000 96

  2 omega -111.00  -39.00   1.0000    4.4500
omega____ theta____ kappa____ phi______ frames
    -      -31.1115  179.0000  -90.0000 72

  3 omega  -62.00   36.00   1.0000    4.4500
omega____ theta____ kappa____ phi______ frames
    -      -31.1115   38.0000  -90.0000 98

  4 omega   44.00  143.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093   45.0000    0.0000 99

  5 omega   -1.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -45.0000  -90.0000 27

  6 omega    5.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -45.0000    0.0000 27

  7 omega   -2.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -45.0000   60.0000 28

  8 omega  102.00  129.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  125.0000  -60.0000 27

  9 omega   20.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -77.0000    0.0000 83

 10 omega    3.00   28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -45.0000 -180.0000 25

 11 omega   12.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -77.0000 -120.0000 92

 12 omega    3.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -77.0000  120.0000 100

 13 omega   -2.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -15.0000   90.0000 60

 14 omega   90.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -15.0000   90.0000 44

 15 omega   85.00  141.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093   45.0000  -90.0000 56

 16 omega    1.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093  -45.0000   30.0000 32

 17 omega   78.00  132.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093 -149.0000  -53.0000 54

 18 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       71.2093 -124.0000  -69.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0586140699
_diffrn_orient_matrix_UB_12      0.0270325015
_diffrn_orient_matrix_UB_13      -0.0745812813
_diffrn_orient_matrix_UB_21      0.1245631903
_diffrn_orient_matrix_UB_22      -0.0293209195
_diffrn_orient_matrix_UB_23      -0.0426566706
_diffrn_orient_matrix_UB_31      0.0183402403
_diffrn_orient_matrix_UB_32      -0.1239938432
_diffrn_orient_matrix_UB_33      0.0078712104
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10223
_diffrn_reflns_theta_full        51.15
_diffrn_reflns_theta_max         51.15
_diffrn_reflns_theta_min         3.74
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     645
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0718
_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^)+(0.1618P)^2^+6.5502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2240
_reflns_number_gt                4555
_reflns_number_total             5695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3003806_si_002_4.cif
_cod_data_source_block           exp_82
_cod_database_code               4329129