First-Transition-Metal Complexes Containing the Ligands 6-Amino-6-methylperhydro-1,4-diazepine (AAZ) and a New Functionalized Derivative: Can AAZ Act as a Mimetic Ligand for 1,4,7-Triazacyclononane?
Rosely A. Peralta; Ademir Neves; Adailton J. Bortoluzzi; Annelise Casellato; Ademir dos Anjos; Alessandra Greatti; Fernando R. Xavier; Bruno Szpoganicz; Inorganic Chemistry 44 (2005) 7690–7692; doi:10.1021/ic050755c

data_4309840
_publ_section_title
;
First-Transition-Metal Complexes Containing the Ligands
6-Amino-6-methylperhydro-1,4-diazepine (AAZ) and a New Functionalized
Derivative: Can AAZ Act as a Mimetic Ligand for 1,4,7-Triazacyclononane?
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7690
_journal_page_last               7692
_journal_paper_doi               10.1021/ic050755c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H30 Cl2 N6 Ni O8'
_chemical_formula_weight         516.03
_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                 119.673(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3031(7)
_cell_length_b                   13.7491(11)
_cell_length_c                   9.3830(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.05
_cell_measurement_theta_min      6.73
_cell_volume                     1042.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1967
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.8513
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0331P)^2^+1.0724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                1553
_reflns_number_total             1851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050755csi20050512_011941_2.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        1042.79(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4309840