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_4329130
_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         'C36 H36 Cu2 N4 O6, 2(Cl O4), 3(C3 H6 O)'
_chemical_formula_sum            'C45 H54 Cl2 Cu2 N4 O17'
_chemical_formula_weight         1120.90
_chemical_name_common            'compound 3'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.1413(2)
_cell_length_b                   17.7925(2)
_cell_length_c                   28.3123(3)
_cell_measurement_reflns_used    14560
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      60.8608
_cell_measurement_theta_min      3.3084
_cell_volume                     10146.11(19)
_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      150.15
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega -104.00   -6.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4133  -77.0000   90.0000 98

  2 omega  -88.00  -57.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4133 -158.0000  172.0000 31

  3 omega  -41.00   15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       31.4133  -38.0000  150.0000 56

  4 omega  -92.00  -67.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   45.0000  150.0000 25

  5 omega   58.00  149.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.9232  179.0000   60.0000 91

  6 omega  113.00  164.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.9232  111.0000 -150.0000 51

  7 omega   91.00  117.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.9232  -45.0000   90.0000 26

  8 omega   65.00  141.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.9232   45.0000  150.0000 76

  9 omega  100.00  139.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.9232  111.0000   30.0000 39

 10 omega   90.00  115.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.9232  -46.0000   16.0000 25

 11 omega   90.00  117.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.9232  -45.0000  120.0000 27

 12 omega  -56.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4133   54.0000   40.0000 49

 13 omega -104.00    2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4133  -77.0000  -90.0000 106
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0846934745
_diffrn_orient_matrix_UB_12      0.0158238876
_diffrn_orient_matrix_UB_13      0.0004918097
_diffrn_orient_matrix_UB_21      0.0142273489
_diffrn_orient_matrix_UB_22      0.0614423868
_diffrn_orient_matrix_UB_23      -0.0312054209
_diffrn_orient_matrix_UB_31      -0.0107969672
_diffrn_orient_matrix_UB_32      -0.0427224186
_diffrn_orient_matrix_UB_33      -0.0446282694
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21879
_diffrn_reflns_theta_full        60.96
_diffrn_reflns_theta_max         60.96
_diffrn_reflns_theta_min         3.66
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18138
_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    1.468
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             4640
_exptl_crystal_recrystallization_method 'acetone; slow evaporation'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         7650
_refine_ls_number_restraints     652
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0595
_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^)+(0.1246P)^2^+5.3638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                6531
_reflns_number_total             7650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3003806_si_002_5.cif
_cod_data_source_block           exp_41
_cod_database_code               4329130