Structural analysis and magnetic properties of the dicubane-like tetramer [Ni(dpk·OH)(N3)]4·2H2O (dpk = di-2-pyridyl ketone) †
Serna, Zurine E.; Barandika, M. Gotzone; Cortés, Roberto; Urtiaga, M. Karmele; Barberis, Gaston E.; Rojo, Teófilo; Journal of the Chemical Society, Dalton Transactions  (2000) 29–; doi:10.1039/a905430h

data_7008883
_publ_section_title
;
 Structural analysis and magnetic properties of the dicubane-like
 tetramer [Ni(dpk&#x00B7;OH)(N3)]4&#x00B7;2H2O
 (dpk&#x2005;=&#x2005;di-2-pyridyl ketone)&#x200A;&#x2020;
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              29
_journal_paper_doi               10.1039/a905430h
_journal_year                    2000
_chemical_formula_sum            'C22 H20 N10 Ni2 O5'
_chemical_formula_weight         621.90
_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
_cell_angle_alpha                91.57(4)
_cell_angle_beta                 105.53(5)
_cell_angle_gamma                96.26(3)
_cell_formula_units_Z            2
_cell_length_a                   10.230(3)
_cell_length_b                   10.358(4)
_cell_length_c                   13.396(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1357.1(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7830
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.58
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.439
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_F_000             636
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          2.676
_refine_ls_shift/su_mean         0.227
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2620
_reflns_number_observed          3953
_reflns_number_total             7830
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a905430h.txt
_cod_data_source_block           nibpco
_cod_original_cell_volume        1357.1(10)
_cod_database_code               7008883