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_7009905
_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            'C19 H22 Mo2 O4 S3'
_chemical_formula_weight         602.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 95.00(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.086(3)
_cell_length_b                   13.077(3)
_cell_length_c                   33.601(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4414.9(19)
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            10070
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  0.8982
_exptl_absorpt_correction_T_min  0.50836
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_obs          0.0406
_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^)+(0.0246P)^2^+7.2010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0913
_refine_ls_wR_factor_obs         0.0797
_reflns_number_observed          5743
_reflns_number_total             7770
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004293p.txt
_cod_data_source_block           mb1874r
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+7.2010P] 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^)+(0.0246P)^2^+7.2010P] 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)/n
_cod_database_code               7009905