A Rare and Highly Oxidized Mo25.5+Unit Stabilized by Oxo Anions and Supported by Formamidinate Bridges
Cotton, F. Albert; Murillo, Carlos A.; Yu, Rongmin; Zhao, Qinliang; Inorganic Chemistry 45 (2006) 9046–9052; doi:10.1021/ic061352v

data_4333068
_publ_section_title
;
 A Rare and Highly Oxidized Mo25.5+Unit Stabilized by Oxo Anions and
 Supported by Formamidinate Bridges
;
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9046
_journal_page_last               9052
_journal_paper_doi               10.1021/ic061352v
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C90 H54 F36 Mo4 N12 O2, C H2 Cl2'
_chemical_formula_sum            'C91 H56 Cl2 F36 Mo4 N12 O2'
_chemical_formula_weight         2488.14
_chemical_name_common            '[Mo2(DmCF3F)3]2(OH)2,CH2Cl2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.168(3)
_cell_angle_beta                 79.495(3)
_cell_angle_gamma                62.515(3)
_cell_formula_units_Z            1
_cell_length_a                   13.902(3)
_cell_length_b                   14.435(3)
_cell_length_c                   14.909(3)
_cell_measurement_reflns_used    10559
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.548
_cell_measurement_theta_min      2.217
_cell_volume                     2388.3(9)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'BRUKER SMART 1000'
_diffrn_measurement_method       \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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17754
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.8851
_exptl_absorpt_correction_T_min  0.8083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.479
_refine_diff_density_min         -2.120
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         10559
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0758P)^2^+4.0691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                8101
_reflns_number_total             10559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061352vsup1.cif
_cod_data_source_block           xl1
_cod_original_cell_volume        2388.2(9)
_cod_database_code               4333068