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_7112418
_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            'C55 H74 P2 S6 Si6 V'
_chemical_formula_weight         1208.92
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.204(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.551(8)
_cell_length_b                   11.965(4)
_cell_length_c                   21.288(6)
_cell_measurement_reflns_used    5847
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.21
_cell_volume                     6556(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1425
_diffrn_reflns_av_sigmaI/netI    0.1862
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48085
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         0.79
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5264
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          1.971
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         16135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1902
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                7071
_reflns_number_total             16135
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7108810
_cod_data_source_file            c2cc37801a.txt
_cod_data_source_block           p2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/c
_cod_database_code               7112418