High oxidation state aqueous organometallics. Formation and structure of an oxo-centred Cp*MoV trinuclear cation by chemical reduction of Cp*2Mo2O5
Demirhan, Funda; Gun, Jenny; Lev, Ovadia; Modestov, Alexandre; Poli, Rinaldo; Richard, Philippe; Journal of the Chemical Society, Dalton Transactions  (2002) 2109–; doi:10.1039/b203583a

data_7011753
_publ_section_title
;
 High oxidation state aqueous organometallics. Formation and structure
 of an oxo-centred Cp*MoV trinuclear cation by chemical reduction of
 Cp*2Mo2O5
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2109
_journal_paper_doi               10.1039/b203583a
_journal_year                    2002
_chemical_formula_moiety         'C36 H45 O10 F9 Mo3,0.5(C12 O12 F18 Zn2)'
_chemical_formula_sum            'C42 H45 F18 Mo3 O16 Zn'
_chemical_formula_weight         1500.97
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.767(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8671(1)
_cell_length_b                   11.7975(1)
_cell_length_c                   37.6903(5)
_cell_measurement_reflns_used    10806
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     5250.01(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            20526
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         2.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         11521
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0409P)^2^+2.7984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                8375
_reflns_number_total             11521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203583a.txt
_cod_data_source_block           fa4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        5250.02(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7011753