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_4315002
_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            'C35 H53 N9 Ni4 O20'
_chemical_formula_weight         1154.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.11
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.968
_cell_length_b                   17.407
_cell_length_c                   35.032
_cell_measurement_temperature    293(2)
_cell_volume                     10913.375
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10758
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.433
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4784
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         10758
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0660P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                7243
_reflns_number_total             10758
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic9020965_si_001_3.cif
_cod_data_source_block           af05fu2n
_cod_depositor_comments
;

2020-11-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C70 H106 N18 Ni8 O40'
_cod_original_formula_weight         2309.41
_cod_original_formula_units_Z            4
_cod_original_cell_volume        10913.3
_cod_database_code               4315002