Electrochemical Synthesis and Structural and Physical Characterization of One- and Two-Electron-Reduced Forms of [SMo12O40]2-
Truc Vu; Alan M. Bond; David C. R. Hockless; Boujemaa Moubaraki; Keith S. Murray; Georgii Lazarev; Anthony G. Wedd; Inorganic Chemistry 40 (2001) 65–72; doi:10.1021/ic991310p

data_4319137
_publ_contact_author_address
;
School of Chemistry, 
P.O. Box 23, 
Monash  University,
Victoria, 3800, Australia 
;
_publ_contact_author_email       ' alan.bond@sci.monash.edu.au '
_publ_contact_author_fax         ' 61 3 9905 9129 '
_publ_contact_author_name        ' Alan M. Bond '
_publ_contact_author_phone       ' 61 3 9905 1338 '
_publ_section_title
;
 Electrochemical Synthesis and Structural and Physical Characterization of
 One- and Two-Electron-Reduced Forms of [SMo12O40]2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              65
_journal_page_last               72
_journal_paper_doi               10.1021/ic991310p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         ' (C16 H36 N +)3, (O40 S Mo12 3-)   '
_chemical_formula_sum            'C48 H108 Mo12 N3 O40 S'
_chemical_formula_weight         2550.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2000-04-10
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
Refinement by David Hockless
Report by David Hockless July 1998
Cif editted by Tony Willis 
(hence e-mail address) for Keith Murray 
April 2000
;
_cell_angle_alpha                94.86(2)
_cell_angle_beta                 93.10(1)
_cell_angle_gamma                91.05(2)
_cell_formula_units_Z            2
_cell_length_a                   13.840(3)
_cell_length_b                   15.587(4)
_cell_length_c                   19.370(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      43.0
_cell_measurement_theta_min      31.5
_cell_volume                     4156.4(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00722
_diffrn_orient_matrix_UB_12      -0.03636
_diffrn_orient_matrix_UB_13      -0.04441
_diffrn_orient_matrix_UB_21      0.01884
_diffrn_orient_matrix_UB_22      0.05241
_diffrn_orient_matrix_UB_23      -0.02299
_diffrn_orient_matrix_UB_31      0.06951
_diffrn_orient_matrix_UB_32      -0.00888
_diffrn_orient_matrix_UB_33      0.01386
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.03421
_diffrn_reflns_av_sigmaI/netI    0.140
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12975
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        2.20
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.228
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2514.00
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.54
_refine_diff_density_min         -0.77
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.684
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     733
_refine_ls_number_reflns         5796
_refine_ls_number_restraints     24
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.0870
_refine_ls_shift/su_mean         0.02
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.000004|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                5796
_reflns_number_total             12378
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic991310p.cif
_cod_data_source_block           MUR40
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.000004|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.000004|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4156(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C48 H108 Mo12 N3 O40 S '
_cod_database_code               4319137