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_4325997
_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         'C20 H35 N7 Ni 2+, 2(Cl O4 1-)'
_chemical_formula_sum            'C20 H35 Cl2 N7 Ni O8'
_chemical_formula_weight         631.16
_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                 94.58(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.433(3)
_cell_length_b                   15.889(4)
_cell_length_c                   20.827(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2781.7(14)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Xpress'
_computing_data_reduction        'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.70.00 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'image plate dip1030'
_diffrn_measurement_method       'laser scanner'
_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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.1378
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32862
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .12
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.791
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                2154
_reflns_number_total             5327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200261j_si_002.cif
_cod_data_source_block           tk5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4325997