Ligand Influence over the Formation of Dinuclear [2+2] versus Trinuclear [3+3] CuI Schiff Base Macrocyclic Complexes
Arnau Arbuse; Sukanta Mandal; Somnath Maji; Ma Angeles Martínez; Xavier Fontrodona; Diana Utz; Frank W. Heinemann; Sandra Kisslinger; Siegfried Schindler; Xavier Sala; Antoni Llobet; Inorganic Chemistry 50 (2011) 6878–6889; doi:10.1021/ic102185y

data_4325716
_publ_section_title
;
 Ligand Influence over the Formation of Dinuclear [2+2] versus Trinuclear
 [3+3] CuI Schiff Base Macrocyclic Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6878
_journal_page_last               6889
_journal_paper_doi               10.1021/ic102185y
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C54 H60 Cu3 N12, 3(F6 Sb)'
_chemical_formula_sum            'C54 H60 Cu3 F18 N12 Sb3'
_chemical_formula_weight         1775.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.82(3)
_cell_angle_beta                 104.97(3)
_cell_angle_gamma                97.76(3)
_cell_formula_units_Z            2
_cell_length_a                   12.008(18)
_cell_length_b                   15.72(2)
_cell_length_c                   20.01(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3328(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1404
_diffrn_reflns_av_sigmaI/netI    0.2796
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42888
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       needle
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.582
_refine_diff_density_min         -2.086
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         17338
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.2401
_refine_ls_R_factor_gt           0.1076
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2784
_refine_ls_wR_factor_ref         0.3216
_reflns_number_gt                5607
_reflns_number_total             17338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102185y_si_002_3.cif
_cod_data_source_block           4(SbF6)3
_cod_original_cell_volume        3328(9)
_cod_database_code               4325716