Synthesis, structure and mechanism of formation of chalcogen-stabilised mixed-metal clusters featuring acetylide bridging and acetylide coupling
Pradeep Mathur; Moawia O. Ahmed; John H. Kaldis; Michael J. McGlinchey; J. Chem. Soc., Dalton Trans.  (2002) 619–629; doi:10.1039/b107090h

data_7011054
_publ_section_title
;
 Synthesis, structure and mechanism of formation of
 chalcogen-stabilised mixed-metal clusters featuring acetylide bridging
 and acetylide coupling
;
_journal_issue                   4
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              619
_journal_page_last               629
_journal_paper_doi               10.1039/b107090h
_journal_year                    2002
_chemical_formula_sum            'C34 H20 Fe3 Mo2 O8 S2'
_chemical_formula_weight         980.05
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.538(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2463(9)
_cell_length_b                   18.9432(9)
_cell_length_c                   17.4513(4)
_cell_measurement_reflns_used    5776
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.59
_cell_volume                     3383.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-V.5.03 Sheldrick, 1994'
_computing_structure_solution    'SHELXTL-V.5.03 Sheldrick, 1994'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Bruker Smart CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25378
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  0.719342
_exptl_absorpt_correction_T_min  0.472290
_exptl_absorpt_correction_type   'empirical (SADABS Sheldrick, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00052(6)
_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_all   0.966
_refine_ls_goodness_of_fit_obs   1.032
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_restrained_S_obs      1.032
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_obs          0.0286
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0627
_refine_ls_wR_factor_obs         0.0563
_reflns_number_observed          4253
_reflns_number_total             5776
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b107090h.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0318P)^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^)+(0.0318P)^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_database_code               7011054