Lithiation of η6-fluorobenzenetricarbonylchromium(0) and reaction with dialkyl disulfides: synthesis of η6-1,2-bis- and 1,2,3-tris-alkylsulfanylbenzenetricarbonylchromium(0) complexes
Woolford, Helen; Elsegood, Mark R. J.; Weaver, George W.; RSC Advances 2 (2012) 6049–; doi:10.1039/c2ra20592k

data_7238649
_publ_section_title
;
 Lithiation of \h6-fluorobenzenetricarbonylchromium(0) and reaction with
 dialkyl disulfides: synthesis of \h6-1,2-bis- and
 1,2,3-tris-alkylsulfanylbenzenetricarbonylchromium(0) complexes
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              6049
_journal_paper_doi               10.1039/c2ra20592k
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C11 H10 Cr O3 S2'
_chemical_formula_sum            'C11 H10 Cr O3 S2'
_chemical_formula_weight         306.31
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.629(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.349(3)
_cell_length_b                   25.347(11)
_cell_length_c                   7.531(3)
_cell_measurement_reflns_used    1017
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.82
_cell_volume                     1211.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.1360
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8036
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2007/2, Sheldrick, G.M., (2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.855
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.041(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+16.9098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2398
_refine_ls_wR_factor_ref         0.2693
_reflns_number_gt                1205
_reflns_number_total             1899
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2ra20592k.txt
_cod_data_source_block           10a\b
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7238649