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_7009908
_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            'C23 H22 Mo2 O8 S3'
_chemical_formula_weight         714.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.97(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.994(4)
_cell_length_b                   8.4820(10)
_cell_length_c                   16.713(4)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      12.561
_cell_volume                     2519.6(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5513
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        11.25
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       'oblong blocks'
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.139
_refine_ls_goodness_of_fit_obs   1.006
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.451
_refine_ls_restrained_S_obs      1.006
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_obs          0.0393
_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^)+(0.0748P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1625
_refine_ls_wR_factor_obs         0.1014
_reflns_number_observed          3605
_reflns_number_total             4384
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004293p.txt
_cod_data_source_block           mb5872
_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^)+(0.0748P)^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^)+(0.0748P)^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      P2(1)/c
_cod_database_code               7009908