First Structural and Magnetic Studies of Ni Clusters Containing 2,6-Diacetylpyridine-dioxime as a Ligand
Albert Escuer; Jordi Esteban; Núria Aliaga-Alcalde; Mercé Font-Bardia; Teresa Calvet; Olivier Roubeau; Simon J. Teat; Inorganic Chemistry 49 (2010) 2259–2266; doi:10.1021/ic9020965

data_4315000
_publ_section_title
;
 First Structural and Magnetic Studies of Ni Clusters Containing
 2,6-Diacetylpyridine-dioxime as a Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2259
_journal_page_last               2266
_journal_paper_doi               10.1021/ic9020965
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C18 H18 N6 Ni2 O4'
_chemical_formula_weight         499.80
_chemical_name_systematic
; 
 ? 
;
_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                 92.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.319(2)
_cell_length_b                   14.755(3)
_cell_length_c                   7.123(2)
_cell_measurement_reflns_used    29755
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      0.98
_cell_volume                     873.6(4)
_computing_cell_refinement       'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       MxCube
_computing_data_reduction        'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'phi rotation at various kappa'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'ESRF BM16'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75150
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3726
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.34
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    2.552
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL2000, Otwinoski, 2003'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+0.5881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2093
_reflns_number_total             2141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9020965_si_001_1.cif
_cod_data_source_block           je121
_cod_database_code               4315000