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_7009768
_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_moiety         C31H20Fe2O5S2W2
_chemical_formula_sum            'C15.5 H10 Fe O2.5 S W'
_chemical_formula_weight         507.99
_chemical_name_common            'Mixed metal cluster'
_chemical_name_systematic        'Metal acetylidine complex'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.1950(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0470(3)
_cell_length_b                   9.50700(10)
_cell_length_c                   20.4070(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2907.27(9)
_computing_cell_refinement       'DENZO-SMN (Nonius-Denzo Software)'
_computing_data_collection       'DENZO-SMN (Nonius-Denzo Software)'
_computing_data_reduction        'DENZO-SMN (Nonius-Denzo Software)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1993)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-93 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.468
_diffrn_measured_fraction_theta_max 0.468
_diffrn_measurement_device_type  'Nonius Kappa CCD Diffractometer'
_diffrn_measurement_method       'combination of four set of frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3555
_diffrn_reflns_theta_full        24.74
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        '< 4%'
_exptl_absorpt_coefficient_mu    9.050
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plates'
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          '0.217 mm'
_exptl_crystal_size_mid          '0.217 mm'
_exptl_crystal_size_min          '0.023 mm'
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.00042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+16.5829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                2449
_reflns_number_total             2484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003517n.txt
_cod_data_source_block           12
_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^)+(0.0169P)^2^+16.5829P] 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^)+(0.0169P)^2^+16.5829P] 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      'C 2/c'
_cod_original_formula_sum        'C15.50 H10 Fe O2.50 S W'
_cod_database_code               7009768