Dehydrogenative desulfurization of thiourea derivatives to give carbodiimides, using hydrosilane and an iron complex.
Hayasaka, Kazumasa; Fukumoto, Kozo; Nakazawa, Hiroshi; Dalton transactions (Cambridge, England : 2003) 42 (2013) 10271–10276; doi:10.1039/c3dt50996f

data_7023205
_publ_section_title
;
 Dehydrogenative desulfurization of thiourea derivatives to give
 carbodiimides, using hydrosilane and an iron complex.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10271
_journal_page_last               10276
_journal_paper_doi               10.1039/c3dt50996f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C31 H34 Fe N2 O Si'
_chemical_formula_sum            'C31 H34 Fe N2 O Si'
_chemical_formula_weight         534.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                75.248(10)
_cell_angle_beta                 85.249(12)
_cell_angle_gamma                87.497(12)
_cell_formula_units_Z            2
_cell_length_a                   9.637(2)
_cell_length_b                   11.752(3)
_cell_length_c                   12.788(3)
_cell_measurement_reflns_used    5063
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0270
_cell_volume                     1395.4(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
scan:
Number of images: 360
Slice: -80.0000 - 100.0000
Image width: 0.5000
Exp time: 10.0000
Rotation axis: Phi
Omega: 0.0000
Chi: 0.0000
Phi: 0.0000
XTD: 35.2024
2theta: 9.8178
scan:
Number of images: 100
Slice: -30.0000 - 20.0000
Image width: 0.5000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 0.0000
XTD: 35.2024
2theta: 9.8178
scan:
Number of images: 100
Slice: -30.0000 - 20.0000
Image width: 0.5000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 90.0000
XTD: 35.2024
2theta: 9.8178
scan:
Number of images: 100
Slice: -30.0000 - 20.0000
Image width: 0.5000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 180.0000
XTD: 35.2024
2theta: 9.8178

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13883
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.03
_diffrn_source_current           280.0000
_diffrn_source_power             16.8000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.9529
_exptl_absorpt_correction_T_min  0.8776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             564
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0856
_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^)+(0.0288P)^2^+3.1276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                5266
_reflns_number_total             6266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50996f.txt
_cod_data_source_block           HYK-315
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1395.3(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7023205