Reactivity of Bis(3,5-dimethylpyrazol-1-yl)methyllithium with S or CS2, Followed by Reaction with Fe3(CO)12and Ar3SnCl or RX: Unexpected Formation of (3,5-Dimethylpyrazol-1-yl)dithioformate Derivatives
Liu, Xia-Li; Zhang, Xiao-Yan; Song, Hai-Bin; Tang, Liang-Fu; Organometallics 31 (2012) 5108–; doi:10.1021/om300448a

data_4078842
_publ_section_title
;
 Reactivity of Bis(3,5-dimethylpyrazol-1-yl)methyllithium with S or CS2,
 Followed by Reaction with Fe3(CO)12and Ar3SnCl or RX: Unexpected
 Formation of (3,5-Dimethylpyrazol-1-yl)dithioformate Derivatives
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              5108
_journal_paper_doi               10.1021/om300448a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C35 H30 Fe2 N4 O6 S Sn'
_chemical_formula_sum            'C35 H30 Fe2 N4 O6 S Sn'
_chemical_formula_weight         865.08
_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                71.639(11)
_cell_angle_beta                 75.339(12)
_cell_angle_gamma                88.962(14)
_cell_formula_units_Z            2
_cell_length_a                   9.7770(11)
_cell_length_b                   12.0010(14)
_cell_length_c                   15.9930(14)
_cell_measurement_reflns_used    6063
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      1.80
_cell_volume                     1719.1(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17626
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.7108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.940
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         8092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                6494
_reflns_number_total             8092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300448a_si_001.cif
_cod_data_source_block           1a
_cod_original_cell_volume        1719.1(3)
_cod_database_code               4078842