Synthesis of Ferrocenyl and Ruthenocenyl Thioamide Derivatives Using a Single-Step Three-Component Reaction
Patra, Malay; Hess, Jeannine; Konatschnig, Sandro; Spingler, Bernhard; Gasser, Gilles; Organometallics 32 (2013) 6098–; doi:10.1021/om400715m

data_4081616
_publ_section_title
;
 Synthesis of Ferrocenyl and Ruthenocenyl Thioamide Derivatives Using a
 Single-Step Three-Component Reaction
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6098
_journal_paper_doi               10.1021/om400715m
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C19 H19 Fe N S'
_chemical_formula_weight         349.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.4053(8)
_cell_length_b                   23.4053(8)
_cell_length_c                   5.8962(4)
_cell_measurement_reflns_used    2981
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      31.0587
_cell_measurement_theta_min      3.4748
_cell_volume                     3230.0(3)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       '\o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5909
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         31.13
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.9589
_exptl_absorpt_correction_T_min  0.6860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.9031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                3262
_reflns_number_total             3572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400715m_si_002.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               4081616