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_4329128
_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         'C40 H44 Cu2 N4 O6 S2, 2(Cl O4)'
_chemical_formula_sum            'C40 H44 Cl2 Cu2 N4 O14 S2'
_chemical_formula_weight         1066.93
_chemical_name_common            'compound 1'
_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                104.425(2)
_cell_angle_beta                 103.075(2)
_cell_angle_gamma                108.667(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0255(3)
_cell_length_b                   11.1307(3)
_cell_length_c                   12.0879(3)
_cell_measurement_reflns_used    33245
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      40.9440
_cell_measurement_theta_min      3.5725
_cell_volume                     1283.20(7)
_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
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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
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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      123.15
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -73.00   30.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000   60.0000 103

  2 omega  -12.00   14.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -150.0000 26

  3 omega  -23.00    3.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -53.0000  -42.0000 26

  4 omega   35.00   82.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000  179.0000  -60.0000 47

  5 omega   49.00   76.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000  179.0000  120.0000 27

  6 omega   22.00   62.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -150.0000 40

  7 omega   -4.00   21.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567   53.0000 -137.0000 25

  8 omega  -64.00  -38.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567   53.0000 -137.0000 26

  9 omega -108.00  -26.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  125.0000 -180.0000 82

 10 omega -122.00  -15.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -77.0000   90.0000 107

 11 omega   80.00  111.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567   77.0000   90.0000 31

 12 omega   15.00   42.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567   77.0000   90.0000 27

 13 omega   81.00  113.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567  125.0000   30.0000 32

 14 omega  -20.00   56.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567  -38.0000  -30.0000 76

 15 omega   38.00   84.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567  -77.0000  -60.0000 46

 16 omega   26.00  106.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567   77.0000  -60.0000 80

 17 omega   73.00  101.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567  125.0000  -30.0000 28

 18 omega  -10.00   61.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567  -38.0000  120.0000 71

 19 omega   41.00   73.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   60.0000 32

 20 omega  -30.00   36.00   1.0000    1.6500
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   60.0000 66

 21 omega  -43.00  -17.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -77.0000 -120.0000 26

 22 omega  -34.00   -8.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -90.0000  113.0000 26

 23 omega  -34.00   -8.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -90.0000   41.0000 26

 24 omega  -36.00  -10.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -86.0000 -144.0000 26

 25 omega  -40.00  -10.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -86.0000  -54.0000 30

 26 omega  -28.00   10.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567   38.0000   90.0000 38

 27 omega  -99.00  -20.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -38.0000  -30.0000 79

 28 omega  -83.00  -33.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  125.0000   60.0000 50

 29 omega  -55.00   22.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567   77.0000  -60.0000 77

 30 omega  -39.00   -9.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -88.0000    0.0000 30

 31 omega -104.00  -20.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -46.0000  143.0000 84

 32 omega  -39.00   -9.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -88.0000  169.0000 30

 33 omega -122.00  -80.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -      -49.5567  -77.0000 -120.0000 42

 34 omega   15.00  115.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567   77.0000 -120.0000 100

 35 omega   73.00  112.00   1.0000   20.8200
omega____ theta____ kappa____ phi______ frames
    -       49.5567  125.0000 -120.0000 39
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0635299753
_diffrn_orient_matrix_UB_12      0.0052135256
_diffrn_orient_matrix_UB_13      0.0358854895
_diffrn_orient_matrix_UB_21      0.0343075775
_diffrn_orient_matrix_UB_22      0.0508343469
_diffrn_orient_matrix_UB_23      -0.0210544220
_diffrn_orient_matrix_UB_31      -0.0001174230
_diffrn_orient_matrix_UB_32      0.0506220301
_diffrn_orient_matrix_UB_33      0.0494445234
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65960
_diffrn_reflns_theta_full        41.18
_diffrn_reflns_theta_max         41.18
_diffrn_reflns_theta_min         3.58
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_F_000             548
_exptl_crystal_recrystallization_method 'DMSO + EtOH '
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         16557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                12515
_reflns_number_total             16557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3003806_si_002_3.cif
_cod_data_source_block           exp_83_s
_cod_original_cell_volume        1283.20(6)
_cod_database_code               4329128