Defective Dicubane-like Tetranuclear Nickel(II) Cyanate and Azide Nanoscale Magnets
Zurine Serna; Noelia De la Pinta; M. Karmele Urtiaga; Luis Lezama; Gotzon Madariaga; J. Modesto Clemente-Juan; Eugenio Coronado; Roberto Cortés; Inorganic Chemistry 49 (2010) 11541–11549; doi:10.1021/ic101970j

data_4317362
_publ_contact_author
;
   Prof. Roberto Cortes Montero
   Facultad de Ciencia y Tecnolog\'ia
   Dpto. de Qu\'imica Inorg\'anica 
   Universidad del Pa\'is Vasco
   Apartado 644
   48080 Bilbao
   Spain
;
_publ_contact_author_email       roberto.cortes@ehu.es
_publ_contact_author_fax         '34 4 6013500'
_publ_contact_author_phone       '34 4 6015521'
_publ_section_title
;
 Defective Dicubane-like Tetranuclear Nickel(II) Cyanate and Azide
 Nanoscale Magnets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11541
_journal_page_last               11549
_journal_paper_doi               10.1021/ic101970j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C46 H40 N14 Ni4 O10, 2(Cl O4), 2(O)'
_chemical_formula_sum            'C46 H40 Cl2 N14 Ni4 O20'
_chemical_formula_weight         1414.58
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.456(3)
_cell_length_b                   10.906(2)
_cell_length_c                   19.990(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     2932.4(13)
_computing_cell_refinement       'Enraf-Nonius CAD-4'
_computing_data_collection       'Enraf-Nonius CAD-4'
_computing_data_reduction        'Xtal 3.2 (Hall, Flack & Stewart, 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.896
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1297
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7679
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.999
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.2038
_refine_ls_R_factor_obs          0.0743
_refine_ls_shift/esd_max         2.692
_refine_ls_shift/esd_mean        0.345
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2997
_refine_ls_wR_factor_obs         0.1844
_reflns_number_observed          3040
_reflns_number_total             7679
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic101970j_si_001_2.cif
_cod_data_source_block           nin3clo4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4317362