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_7011056
_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            'C33 H20 Fe3 Mo2 O7 S2'
_chemical_formula_weight         952.04
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.301(2)
_cell_angle_beta                 85.743(2)
_cell_angle_gamma                80.224(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7776(11)
_cell_length_b                   10.9285(13)
_cell_length_c                   16.850(2)
_cell_measurement_reflns_used    15220
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.21
_cell_volume                     1588.5(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      299(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15220
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.576991
_exptl_absorpt_correction_type   'empirical (SADABS Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .12
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0014(3)
_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   0.978
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         15180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_obs          0.0473
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1300
_refine_ls_wR_factor_obs         0.1195
_reflns_number_observed          11288
_reflns_number_total             15220
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b107090h.txt
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0785P)^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^)+(0.0785P)^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      P-1
_cod_database_code               7011056