Molecules based on M(v) (M = Mo, W) and Ni(ii) ions: a new class of trigonal bipyramidal cluster and confirmation of SMM behavior for the pentadecanuclear molecule {NiII[NiII(tmphen)(MeOH)]6[Ni(H2O)3]2[μ-CN]30[WV(CN)3]6}
Hilfiger, Matthew G.; Zhao, Hanhua; Prosvirin, Andrey; Wernsdorfer, Wolfgang; Dunbar, Kim R.; Dalton Transactions  (2009) 5155–5163; doi:10.1039/b903691a

data_7001599
_publ_section_title
;
 Molecules based on M(v) (M = Mo, W) and Ni(ii) ions: a new class of
 trigonal bipyramidal cluster and confirmation of SMM behavior for the
 pentadecanuclear molecule
 {NiII[NiII(tmphen)(MeOH)]6[Ni(H2O)3]2[\m-CN]30[WV(CN)3]6}
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              5155
_journal_page_last               5163
_journal_paper_doi               10.1039/b903691a
_journal_year                    2009
_chemical_formula_sum            'C168 H171 Mo6 N66 Ni9 O18'
_chemical_formula_weight         4506.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   32.214(5)
_cell_length_b                   32.214(5)
_cell_length_c                   21.074(4)
_cell_measurement_temperature    140(2)
_cell_volume                     18939(5)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'profile data from \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  0.1367
_diffrn_reflns_av_sigmaI/netI    0.1301
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73793
_diffrn_reflns_theta_full        28.76
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6867
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.724
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         10423
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.2684
_refine_ls_R_factor_gt           0.1192
_refine_ls_shift/su_max          1.216
_refine_ls_shift/su_mean         0.061
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3394
_refine_ls_wR_factor_ref         0.4215
_reflns_number_gt                3548
_reflns_number_total             10423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903691a.txt
_cod_data_source_block           c:\comp4.cif
_cod_depositor_comments
;

2018-07-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H57 Mo2 N22 Ni3 O6'
_cod_original_formula_weight         1502.25
_cod_original_formula_units_Z            9
_cod_database_code               7001599