Electrochemical, Spectroscopic, Structural, and Magnetic Characterization of the Reduced and Protonated α-Dawson Anions in [Fe(η5-C5Me5)2]5[HS2Mo18O62].3HCONMe2.2Et2O and [NBu4]5[HS2Mo18O62].2H2O1
Suzy Juraja; Truc Vu; Peter J. S. Richardt; Alan M. Bond; Terence J. Cardwell; John D. Cashion; Gary D. Fallon; Georgii Lazarev; Boujemaa Moubaraki; Keith S. Murray; Anthony G. Wedd; Inorganic Chemistry 41 (2002) 1072–1078; doi:10.1021/ic010780s

data_4317622
_publ_contact_author_address
;
School of Chemistry
PO Box 23
Monash University
Victoria  3800
Australia
;
_publ_contact_author_email       ' alan.bond@sci.monash.edu.au '
_publ_contact_author_fax         ' 61 3 99054597 '
_publ_contact_author_name        'Alan M. Bond'
_publ_section_title
;
 Electrochemical, Spectroscopic, Structural, and Magnetic Characterization
 of the Reduced and Protonated \a-Dawson Anions in
 [Fe(\h5-C5Me5)2]5[HS2Mo18O62].3HCONMe2.2Et2O and
 [NBu4]5[HS2Mo18O62].2H2O1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1072
_journal_page_last               1078
_journal_paper_doi               10.1021/ic010780s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C80 H181 Mo18 N5 O64 S2'
_chemical_formula_weight         4028.34
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2000-01-18
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 105.9381(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1255(3)
_cell_length_b                   15.4110(2)
_cell_length_c                   35.8646(4)
_cell_measurement_reflns_used    207009
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     13353.3(3)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       'Nonius/KappaCCD Diffractometer Control'
_computing_data_reduction        Denzo-SMN
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution    'teXsan (MSC, 1992-1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type  'Quantum CCD'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04470
_diffrn_reflns_av_sigmaI/netI    0.100
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            91833
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             7984.00
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.53
_refine_diff_density_min         -0.96
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.338
_refine_ls_goodness_of_fit_ref   1.513
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9796
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0564
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                9796
_reflns_number_total             14633
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic010780s.cif
_cod_data_source_block           k2_00
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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        'C80 H181 N5 Mo18 O64 S2 '
_cod_database_code               4317622