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_4318784
_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            'C87.5 H158 N48 Ni9 O39.5 W6'
_chemical_formula_weight         4146.11
_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                 113.727(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.5278(16)
_cell_length_b                   19.2008(18)
_cell_length_c                   32.4072(17)
_cell_measurement_reflns_used    7787
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      1.92
_cell_volume                     16251(2)
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 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_measured_fraction_theta_full 0.763
_diffrn_measured_fraction_theta_max 0.763
_diffrn_measurement_device_type  'STOE IPDS'
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            37913
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.318
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_type   empirical_DIFABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8124
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.622
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.000001(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         12020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0655P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                8267
_reflns_number_total             12020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025562t_s1_2.cif
_cod_data_source_block           2
_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_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C87.50 H158 N48 Ni9 O39.50 W6'
_cod_database_code               4318784