Structural and Magnetic Characterization of a Tetranuclear Copper(II) Cubane Stabilized by Intramolecular Metal Cation-π Interactions
Raffaello Papadakis; Eric Rivière; Michel Giorgi; Hélène Jamet; Pierre Rousselot-Pailley; Marius Réglier; A. Jalila Simaan; Thierry Tron; Inorganic Chemistry 52 (2013) 5824–5830; doi:10.1021/ic3027545

data_4334824
_publ_contact_author_email
;
jalila.simaan@univ-amu.fr
;
_publ_section_title
;
 Structural and Magnetic Characterization of a Tetranuclear Copper(II)
 Cubane Stabilized by Intramolecular Metal Cation-\p Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5824
_journal_page_last               5830
_journal_paper_doi               10.1021/ic3027545
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H30 Cl2 Cu N4 O9'
_chemical_formula_sum            'C28 H30 Cl2 Cu N4 O9'
_chemical_formula_weight         701.01
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-04-15T09:37:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2012-10-15 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8464(5)
_cell_length_b                   8.4305(2)
_cell_length_c                   17.6443(4)
_cell_measurement_reflns_used    21902
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.31
_cell_measurement_wavelength     0.71073
_cell_volume                     3100.91(13)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'Omega + Phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.07
_diffrn_reflns_av_unetI/netI     0.044
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21902
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       prism
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+2.5867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.2313
_reflns_number_gt                2206
_reflns_number_total             3475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3027545_si_002_2.cif
_cod_data_source_block           complex3
_cod_database_code               4334824