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_4329227
_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         'C94 H116 N52 Ni13 O22, 7(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C101 H152 N52 Ni13 O31'
_chemical_formula_weight         3353.98
_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                 91.96(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.582(13)
_cell_length_b                   22.488(8)
_cell_length_c                   27.802(10)
_cell_measurement_reflns_used    230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     15360(11)
_computing_cell_refinement       'AUTOMAR (Claudio Klein, 2007)'
_computing_data_collection       'MARXDS (Claudio Klein, 2005)'
_computing_data_reduction        'MARSCALE (Claudio Klein, 2007)'
_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 0.949
_diffrn_measured_fraction_theta_max 0.778
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.1124
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            23067
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       prism
_exptl_crystal_F_000             6936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         14280
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1587
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.2161
_reflns_number_gt                6378
_reflns_number_total             14280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004036_si_001.cif
_cod_data_source_block           je829_2b
_cod_database_code               4329227