Stepwise hydrogenation of an arylthiophosphinidene isocyanide complex to give tethered aldimine and aminocarbene functions.
Alvarez, M. Angeles; Alvarez, Belén; García, M Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11039–11042; doi:10.1039/c3dt51562a

data_7021809
_publ_section_title
;
 Stepwise hydrogenation of an arylthiophosphinidene isocyanide complex to
 give tethered aldimine and aminocarbene functions.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11039
_journal_page_last               11042
_journal_paper_doi               10.1039/c3dt51562a
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H50 Mo2 N O2 P S, C H2 Cl2'
_chemical_formula_sum            'C36 H52 Cl2 Mo2 N O2 P S'
_chemical_formula_weight         856.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-03-08T17:52:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.314(5)
_cell_angle_beta                 80.496(4)
_cell_angle_gamma                84.132(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3398(5)
_cell_length_b                   11.3848(7)
_cell_length_c                   17.6131(10)
_cell_measurement_reflns_used    6166
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.2948
_cell_measurement_theta_min      3.9046
_cell_measurement_wavelength     1.54184
_cell_volume                     2031.8(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'ONYX CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15087
_diffrn_reflns_theta_full        74.46
_diffrn_reflns_theta_max         74.46
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    7.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.4
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.051
_refine_diff_density_min         -0.9
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7913
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1051P)^2^+12.3846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.182
_refine_ls_wR_factor_ref         0.1979
_reflns_number_gt                6294
_reflns_number_total             7913
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt51562a.txt
_cod_data_source_block           compound4
_cod_database_code               7021809