New topologies in pentanuclear nickel/oximato clusters: structural and magnetic characterization.
Esteban, Jordi; Font-Bardia, Mercè; Costa, José Sánchez; Teat, Simon J.; Escuer, Albert; Inorganic chemistry 53 (2014) 3194–3203; doi:10.1021/ic500057j

data_4337617
_publ_section_title
;
 New topologies in pentanuclear nickel/oximato clusters: structural and
 magnetic characterization.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3194
_journal_page_last               3203
_journal_paper_doi               10.1021/ic500057j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'4(C45 H40.5 N18 Ni5 O13), 2(N O3), 11(C H4 O), 5(H2 O)'
_chemical_formula_sum            'C191 H216 N74 Ni20 O74'
_chemical_formula_weight         5906.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   34.0083(4)
_cell_length_b                   34.0083(4)
_cell_length_c                   12.0595(2)
_cell_measurement_reflns_used    11278
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      1.3
_cell_measurement_theta_min      61.12
_cell_volume                     13947.6(3)
_computing_cell_refinement       'Nonius Collect - HKL2000'
_computing_data_collection       'Nonius Collect - HKL2000'
_computing_data_reduction        'Nonius Collect - HKL2000'
_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-Nonius FR591 KappaCCD 2000'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'confocal multilayer mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0036
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10705
_diffrn_reflns_theta_full        61.12
_diffrn_reflns_theta_max         61.12
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_T_max  0.9464
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6064
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.442
_refine_diff_density_min         -1.646
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         10705
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1211P)^2^+22.6245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2190
_reflns_number_gt                10161
_reflns_number_total             10705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500057j_si_001.cif
_cod_data_source_block           af24fua1na
_cod_original_sg_symbol_H-M      P42/n
_cod_database_code               4337617