High-Spin Molecules: Synthesis, X-ray Characterization, and Magnetic Behavior of Two New Cyano-Bridged NiII9MoV6 and NiII9WV6 Clusters with a S = 12 Ground State
Federica Bonadio; Mathias Gross; Helen Stoeckli-Evans; Silvio Decurtins; Inorganic Chemistry 41 (2002) 5891–5896; doi:10.1021/ic025562t

data_4318783
_publ_section_title
;
 High-Spin Molecules: Synthesis, X-ray Characterization, and Magnetic
 Behavior of Two New Cyano-Bridged NiII9MoV6 and NiII9WV6 Clusters with a
 S = 12 Ground State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5891
_journal_page_last               5896
_journal_paper_doi               10.1021/ic025562t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C89 H166 Mo6 N48 Ni9 O42'
_chemical_formula_weight         3684.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
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_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                 113.555(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.4957(18)
_cell_length_b                   19.2583(10)
_cell_length_c                   32.4279(17)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.12
_cell_volume                     16312.9(18)
_computing_cell_refinement       'CELL (Stoe & Cie GmbH, Darmstadt, 2000)'
_computing_data_collection       'EXPOSE (Stoe & Cie GmbH, Darmstadt, 2000)'
_computing_data_reduction
'INTEGRATE (Stoe & Cie GmbH, Darmstadt, 2000)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measurement_device_type  'STOE Image Plate Diffraction System'
_diffrn_measurement_method       'phi oscillation'
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            56833
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             7504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         14808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+40.6509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                11147
_reflns_number_total             14808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025562t_s1_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        16312.9(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4318783