Deconstruction of cyclic and acyclic trithiocarbonates by C‒S and CS bond cleavage during oxidative decarbonylation of dimolybdenum alkyne complexes †
Adams, Harry; Allott, Christopher; Bancroft, Matthew N.; Morris, Michael J.; Journal of the Chemical Society, Dalton Transactions  (2000) 4145–; doi:10.1039/b004293p

data_7009907
_publ_section_title
;
 Deconstruction of cyclic and acyclic trithiocarbonates by C--S and
 C&#xE006;S bond cleavage during oxidative decarbonylation of
 dimolybdenum alkyne complexes&#x200A;&#x2020;
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4145
_journal_paper_doi               10.1039/b004293p
_journal_year                    2000
_chemical_formula_sum            'C28 H26 Mo2 O6 S3'
_chemical_formula_weight         746.55
_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                78.15(2)
_cell_angle_beta                 77.210(10)
_cell_angle_gamma                87.97(2)
_cell_formula_units_Z            2
_cell_length_a                   10.051(2)
_cell_length_b                   12.137(4)
_cell_length_c                   12.260(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1427.3(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1478
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9417
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       blocks
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.780
_refine_diff_density_min         -5.743
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   0.909
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_restrained_S_obs      0.909
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_obs          0.0773
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1813P)^2^+2.3681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2891
_refine_ls_wR_factor_obs         0.1964
_reflns_number_observed          6617
_reflns_number_total             7983
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004293p.txt
_cod_data_source_block           mbigs-5r
_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^)+(0.1813P)^2^+2.3681P] 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^)+(0.1813P)^2^+2.3681P] 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               7009907