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_4301884
_publ_contact_author_address
;Patriarchou Grigoriou & Neapoleos
15310 Aghia Paraskevi Attikis
Greece
;
_publ_contact_author_email       tbou@ims.demokritos.gr
_publ_contact_author_fax         '+30 210 6503365'
_publ_contact_author_name        'Athanassios K. Boudalis'
_publ_contact_author_phone       '+30 210 6503346'
_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            'C42 H50 Cl2 Cu4 N12 O20'
_chemical_formula_weight         1368.00
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.2410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3132(2)
_cell_length_b                   10.57660(10)
_cell_length_c                   21.9862(4)
_cell_measurement_temperature    180(2)
_cell_volume                     2630.74(7)
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_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     1.54180
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28638
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         7.00
_exptl_absorpt_coefficient_mu    3.522
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         4294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+2.6761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                3968
_reflns_number_total             4294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900115c_si_001_1.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301884