Synthesis and structures of heterometallic trinuclear clusters [CpFe(CO)2]2(μ3-S2)W(CO)5 and Cp2Fe2(CO)3(μ-CO)(μ3-S)W(CO)5 and kinetic study of migration of the W(CO)5 moiety in the disulfido complex
Kuge, Katsuaki; Tobita, Hiromi; Ogino, Hiroshi; Chemical Communications  (1999) 1061–; doi:10.1039/a901660k

data_7110513
_publ_section_title
;
 Synthesis and structures of heterometallic trinuclear clusters
 [CpFe(CO)2]2(\m3-S2)W(CO)5 and Cp2Fe2(CO)3(\m-CO)(\m3-S)W(CO)5 and
 kinetic study of migration of the W(CO)5 moiety in the disulfido complex
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1061
_journal_paper_doi               10.1039/a901660k
_journal_year                    1999
_chemical_formula_moiety         'C18 H10 Fe2 O8 S W '
_chemical_formula_sum            'C18 H10 Fe2 O8 S W'
_chemical_formula_weight         681.88
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_audit_creation_date             'Wed Jun 17 16:57:39 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.896(9)
_cell_length_b                   9.848(5)
_cell_length_c                   12.815(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.0
_cell_volume                     2132(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02297
_diffrn_orient_matrix_UB_12      -0.09049
_diffrn_orient_matrix_UB_13      -0.01842
_diffrn_orient_matrix_UB_21      -0.05237
_diffrn_orient_matrix_UB_22      0.04378
_diffrn_orient_matrix_UB_23      -0.01372
_diffrn_orient_matrix_UB_31      0.01527
_diffrn_orient_matrix_UB_32      0.01438
_diffrn_orient_matrix_UB_33      -0.07458
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.456
_diffrn_reflns_av_sigmaI/netI    0.120
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2795
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        -0.49
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.868
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1296.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.852
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     271
_refine_ls_number_reflns         1372
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0387
_refine_ls_shift/esd_max         0.8950
_refine_ls_shift/esd_mean        0.2230
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00216|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0513
_reflns_number_observed          1372
_reflns_number_total             2790
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            901660ksup1.cif
_cod_data_source_block           2
_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) +
0.00216|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) + 0.00216|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2132(3)
_cod_original_sg_symbol_H-M      'P c a 21     '
_cod_original_formula_sum        'C18 H10 Fe2 O8 S W '
_cod_database_code               7110513