Trinuclear, Tetranuclear, and Polymeric CuII Complexes from the First Use of 2-Pyridylcyanoxime in Transition Metal Chemistry: Synthetic, Structural, and Magnetic Studies
Albert Escuer; Gina Vlahopoulou; Spyros P. Perlepes; Franz A. Mautner; Inorganic Chemistry 50 (2011) 2468–2478; doi:10.1021/ic102286r

data_4324656
_publ_section_title
;
 Trinuclear, Tetranuclear, and Polymeric CuII Complexes from the First Use
 of 2-Pyridylcyanoxime in Transition Metal Chemistry: Synthetic,
 Structural, and Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2468
_journal_page_last               2478
_journal_paper_doi               10.1021/ic102286r
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '3(C42 H30 Cu4 N6 O12), 2(C H1.50 N0.50)'
_chemical_formula_sum            'C128 H93 Cu12 N19 O36'
_chemical_formula_weight         3235.82
_chemical_name_common            '[Cu4(C5H5CO2)4(CN-py-NO)2(OH)2]3(CH3CN)'
_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
_cell_angle_alpha                80.00(3)
_cell_angle_beta                 78.65(3)
_cell_angle_gamma                77.25(2)
_cell_formula_units_Z            1
_cell_length_a                   13.546(2)
_cell_length_b                   15.635(2)
_cell_length_c                   16.036(3)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.50
_cell_volume                     3217.5(10)
_computing_cell_refinement       'Bruker SAINT (1998)'
_computing_data_collection       'Bruker SMART (1998)'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'SHELXTL/PC v.5.03 (Sheldrick, 1995)'
_computing_publication_material  'SHELXTL/PC v.5.03 (Sheldrick, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'Bruker P4'
_diffrn_measurement_method       \w-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  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25410
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    2.027
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.114
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         12918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_gt       1.281
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+8.2753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2002
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                9122
_reflns_number_total             12919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102286r_si_001_3.cif
_cod_data_source_block           tz4k
_cod_database_code               4324656