High Nuclearity in Azido/Oximate Chemistry: Ni14 and Ni13 Clusters with S = 6 and 9 Ground States
Jordi Esteban; Laura Alcázar; Maria Torres-Molina; Montserrat Monfort; Mercè Font-Bardia; Albert Escuer; Inorganic Chemistry 51 (2012) 5503–5505; doi:10.1021/ic3004036

data_4329228
_publ_section_title
;
 High Nuclearity in Azido/Oximate Chemistry: Ni14 and Ni13 Clusters with S
 = 6 and 9 Ground States
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5503
_journal_page_last               5505
_journal_paper_doi               10.1021/ic3004036
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C88 H96 Cl2 N48 Ni14 O24, 7(C H4 O), 5.50(H2 O), 2(Cl)'
_chemical_formula_sum            'C95 H135 Cl4 N48 Ni14 O36.5'
_chemical_formula_weight         3497.25
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                108.409(5)
_cell_angle_beta                 92.219(5)
_cell_angle_gamma                115.014(4)
_cell_formula_units_Z            1
_cell_length_a                   16.2274(14)
_cell_length_b                   16.7091(16)
_cell_length_c                   19.2008(18)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.28
_cell_volume                     4385.7(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17249
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.596
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       prism
_exptl_crystal_F_000             1793
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         17249
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+8.5287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1601
_reflns_number_gt                12562
_reflns_number_total             17249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004036_si_002.cif
_cod_data_source_block           af40mtm1na
_cod_original_formula_sum        'C95 H135 Cl4 N48 Ni14 O36.50'
_cod_database_code               4329228