Coupling of co-ordinated acetylide ligands with and without CO on chalcogen-stabilised mixed-metal clusters. Synthesis and characterisation of [M2Fe3(L)2(CO)6(μ3-E)2{μ-CC(Ph)C(Ph)C}] and [M2Fe2(L)2(CO)4(μ3-E)2{μ-CC(Ph)(CO)C(Ph)C}] (L = η5-C5Me5 or η5-C5H5, M = Mo or W, E = S, Se or Te)
Mathur, Pradeep; Ahmed, Moawia O.; Dash, Aswini K.; Walawalkar, Mrinalini G.; Puranik, Vedavati G.; Journal of the Chemical Society, Dalton Transactions  (2000) 2916–; doi:10.1039/b003517n

data_7009767
_publ_section_title
;
 Coupling of co-ordinated acetylide ligands with and without CO on
 chalcogen-stabilised mixed-metal clusters. Synthesis and
 characterisation of [M2Fe3(L)2(CO)6(\m3-E)2{\m-CC(Ph)C(Ph)C}] and
 [M2Fe2(L)2(CO)4(\m3-E)2{\m-CC(Ph)(CO)C(Ph)C}]
 (L&#x2005;=&#x2005;\h5-C5Me5 or \h5-C5H5, M&#x2005;=&#x2005;Mo or W,
 E&#x2005;=&#x2005;S, Se or Te)
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2916
_journal_paper_doi               10.1039/b003517n
_journal_year                    2000
_chemical_formula_sum            'C32.5 H20 Cl Fe3 O6 S2 W2'
_chemical_formula_weight         1141.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.668(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.561(2)
_cell_length_b                   8.1880(8)
_cell_length_c                   21.932(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      31.267
_cell_measurement_theta_min      2.696
_cell_volume                     3460.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47103
_diffrn_reflns_theta_full        34.06
_diffrn_reflns_theta_max         34.06
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    8.092
_exptl_absorpt_correction_T_max  0.8251
_exptl_absorpt_correction_T_min  0.1917
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.791
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         13421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                8679
_reflns_number_total             13421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003517n.txt
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C32.50 H20 Cl Fe3 O6 S2 W2'
_cod_database_code               7009767