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_7238650
_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         'C13 H14 Cr O3 S2'
_chemical_formula_sum            'C13 H14 Cr O3 S2'
_chemical_formula_weight         334.36
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4396(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6871(12)
_cell_length_b                   7.2672(8)
_cell_length_c                   18.787(2)
_cell_measurement_reflns_used    5388
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.04
_cell_measurement_theta_min      2.84
_cell_volume                     1446.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_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 0.941
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6719
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16190
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         31.18
_diffrn_reflns_theta_min         2.84
_diffrn_standards_decay_%        4
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10, Sheldrick, G.M., (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.092(14)
_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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+0.2541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                4581
_reflns_number_total             4899
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2ra20592k.txt
_cod_data_source_block           10b
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7238650