Reactivity of Nickel(II) and Copper(II) Complexes of a β-Aminohydrazone Ligand with Pyridine-2-aldehyde: Macrocyclization vs Unprecedented Pyrazole Ring Synthesis via C-C Bond-Forming Reaction
Oindrila Das; Ennio Zangrando; Tapan Kanti Paine; Inorganic Chemistry 50 (2011) 8012–8019; doi:10.1021/ic200261j

data_4326000
_publ_section_title
;
 Reactivity of Nickel(II) and Copper(II) Complexes of a \b-Aminohydrazone
 Ligand with Pyridine-2-aldehyde: Macrocyclization vs Unprecedented
 Pyrazole Ring Synthesis via C-C Bond-Forming Reaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8012
_journal_page_last               8019
_journal_paper_doi               10.1021/ic200261j
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C36 H30 Cu2 N8 O2 2+, 2(Cl O4 1-)'
_chemical_formula_sum            'C36 H30 Cl2 Cu2 N8 O10'
_chemical_formula_weight         932.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
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_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.521(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.147(3)
_cell_length_b                   24.849(4)
_cell_length_c                   13.631(3)
_cell_measurement_temperature    150(2)
_cell_volume                     7838(2)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'APEX2 v2.1-0 (Bruker AXS)'
_computing_data_reduction        'Bruker Apex II'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.80.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'w/ and f/ scan'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
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_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            49625
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.8970
_exptl_absorpt_correction_T_min  0.7536
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7713
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0742P)^2^+6.6800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                5977
_reflns_number_total             7713
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200261j_si_005.cif
_cod_data_source_block           tkp-o12
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4326000