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_4325715
_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         'C42 H48 Cu2 N8 O2, 2(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C46 H51 Cu2 F6 N9 O8 S2'
_chemical_formula_weight         1163.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.371(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.203(3)
_cell_length_b                   18.211(3)
_cell_length_c                   19.084(3)
_cell_measurement_temperature    100(2)
_cell_volume                     5213.1(16)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        SAINT+"
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79370
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       plate
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         12917
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+4.5101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                9650
_reflns_number_total             12917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102185y_si_002_2.cif
_cod_data_source_block           2(CF3SO3)2
_cod_original_cell_volume        5213.3(16)
_cod_database_code               4325715