Activation of dichloromethane by a V(III) thiolate complex: an example of S-based nucleophilic reactivity in an early transition metal thiolate.
Chen, Tzu-Tso; Chen, Yu-Sen; Chang, Ya-Ho; Wang, Jung-Ching; Tsai, Yi-Fang; Lee, Gene-Hsiang; Kuo, Tin-Shen; Hsu, Hua-Fen; Chemical communications (Cambridge, England) 49 (2013) 1109–1111; doi:10.1039/c2cc37801a

data_7112419
_publ_section_title
;
 Activation of dichloromethane by a V(III) thiolate complex: an example of
 S-based nucleophilic reactivity in an early transition metal thiolate.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1109
_journal_page_last               1111
_journal_paper_doi               10.1039/c2cc37801a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C79.93 H98.07 O0.56 P3 S6 Si6 V'
_chemical_formula_weight         1572.52
_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-97
_cell_angle_alpha                80.6212(11)
_cell_angle_beta                 86.5684(12)
_cell_angle_gamma                70.7773(7)
_cell_formula_units_Z            2
_cell_length_a                   13.2824(2)
_cell_length_b                   16.9608(3)
_cell_length_c                   20.7372(3)
_cell_measurement_reflns_used    67094
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.29
_cell_volume                     4352.15(12)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67094
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         19900
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+1.5046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1644
_reflns_number_gt                13331
_reflns_number_total             19900
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7108811
_cod_data_source_file            c2cc37801a.txt
_cod_data_source_block           ic15446
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7112419