Ferromagnetic CuII4, CoII4, and NiII6 Azido Complexes Derived from Metal-Assisted Methanolysis of Di-2,6-(2-pyridylcarbonyl)pyridine
Anastasia N. Georgopoulou; Catherine P. Raptopoulou; Vassilis Psycharis; Rafael Ballesteros; Belén Abarca; Athanassios K. Boudalis; Inorganic Chemistry 48 (2009) 3167–3176; doi:10.1021/ic900115c

data_4301886
_publ_section_title
;
Ferromagnetic CuII4, CoII4, and NiII6 Azido Complexes Derived from
Metal-Assisted Methanolysis of Di-2,6-(2-pyridylcarbonyl)pyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3167
_journal_page_last               3176
_journal_paper_doi               10.1021/ic900115c
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C116.8 H113.2 Cl2 N54 Ni12 O39.8'
_chemical_formula_weight         3685.63
_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-97
_cell_angle_alpha                87.440(1)
_cell_angle_beta                 84.744(1)
_cell_angle_gamma                85.770(1)
_cell_formula_units_Z            2
_cell_length_a                   14.5652(2)
_cell_length_b                   18.9292(3)
_cell_length_c                   27.2138(4)
_cell_measurement_temperature    180(2)
_cell_volume                     7445.72(19)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            88627
_diffrn_reflns_theta_full        59.00
_diffrn_reflns_theta_max         59.00
_diffrn_reflns_theta_min         6.56
_diffrn_standards_decay_%        -0.2
_exptl_absorpt_coefficient_mu    2.730
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             3761
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2037
_refine_ls_number_reflns         20764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2189
_refine_ls_wR_factor_ref         0.2549
_reflns_number_gt                13192
_reflns_number_total             20764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900115c_si_001_3.cif
_cod_data_source_block           complex3
_cod_original_formula_sum        'C116.80 H113.20 Cl2 N54 Ni12 O39.80'
_cod_database_code               4301886