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_4329126
_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         'C16 H18 O4'
_chemical_formula_sum            'C16 H18 O4'
_chemical_formula_weight         274.30
_chemical_name_common            p-LH2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   13.2257(3)
_cell_length_b                   12.6283(3)
_cell_length_c                   8.78833(18)
_cell_measurement_reflns_used    1326
_cell_measurement_temperature    298.3
_cell_measurement_theta_max      50.9460
_cell_measurement_theta_min      3.3389
_cell_volume                     1467.81(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      298.3
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -51.00   -1.00   0.2500    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.5383  -77.0000  -30.0000 200

  2 omega  -62.00  -35.00   0.2500    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.5383  179.0000   60.0000 108

  3 omega -103.00  -54.00   0.2500    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.5383  -77.0000  -30.0000 196

  4 omega  -99.00  -73.00   0.2500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000    0.0000   60.0000 104

  5 omega  113.00  141.00   0.2500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.8450  158.0000   30.0000 112

  6 omega   77.00  106.00   0.2500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.8450  158.0000   30.0000 116

  7 omega   50.00  142.00   0.2500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.8450   15.0000 -180.0000 368

  8 omega    2.00   28.00   0.2500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.8450  -45.0000  -30.0000 104

  9 omega  101.00  141.00   0.2500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.8450  125.0000   90.0000 160

 10 omega -104.00    2.00   0.2500    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.5383  -77.0000   90.0000 424

 11 omega -104.00  -52.00   0.2500    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.5383 -158.0000  -30.0000 208

 12 omega   -2.00   34.00   0.2500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.8450  -45.0000  150.0000 144
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0220132000
_diffrn_orient_matrix_UB_12      0.1171970000
_diffrn_orient_matrix_UB_13      0.0355939000
_diffrn_orient_matrix_UB_21      -0.1076718000
_diffrn_orient_matrix_UB_22      0.0297575000
_diffrn_orient_matrix_UB_23      -0.0513922000
_diffrn_orient_matrix_UB_31      -0.0386507000
_diffrn_orient_matrix_UB_32      -0.0161407000
_diffrn_orient_matrix_UB_33      0.1637538000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2566
_diffrn_reflns_theta_full        51.00
_diffrn_reflns_theta_max         51.00
_diffrn_reflns_theta_min         6.05
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       needle
_exptl_crystal_F_000             584
_exptl_crystal_recrystallization_method 'solvent MeOH'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.134
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0012(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.3394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                702
_reflns_number_total             832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3003806_si_002_1.cif
_cod_data_source_block           exp_255
_cod_original_cell_volume        1467.80(6)
_cod_database_code               4329126