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_4334825
_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         'C14 H17 Cl1 Cu1 N2 O6'
_chemical_formula_sum            'C14 H17 Cl Cu N2 O6'
_chemical_formula_weight         408.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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             2011-11-28T13:33:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2012-10-15 # Formatted by publCIF
;
_cell_angle_alpha                94.190(1)
_cell_angle_beta                 98.429(1)
_cell_angle_gamma                97.648(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0049(3)
_cell_length_b                   9.0910(2)
_cell_length_c                   10.3035(3)
_cell_measurement_reflns_used    12162
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      3.17
_cell_measurement_wavelength     0.71073
_cell_volume                     823.25(4)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_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  0.028
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12162
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         3.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       prism
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4133
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.046
_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^)+(0.0718P)^2^+0.7550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                3502
_reflns_number_total             4133
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3027545_si_002_3.cif
_cod_data_source_block           complex2
_cod_original_formula_sum        'C14 H17 Cl1 Cu1 N2 O6'
_cod_database_code               4334825