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_7021807
_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         'C32 H12 B F24, C35 H49 Mo2 N O2 P S'
_chemical_formula_sum            'C67 H61 B F24 Mo2 N O2 P S'
_chemical_formula_weight         1633.89
_chemical_name_systematic
;
?
;
_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
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_audit_creation_date             2013-03-13T17:40:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                66.598(4)
_cell_angle_beta                 89.260(3)
_cell_angle_gamma                85.463(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1501(4)
_cell_length_b                   16.3707(7)
_cell_length_c                   17.9886(8)
_cell_measurement_reflns_used    12124
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.3413
_cell_measurement_theta_min      2.9484
_cell_measurement_wavelength     1.54184
_cell_volume                     3542.1(3)
_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 0.946
_diffrn_measured_fraction_theta_max 0.946
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
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_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25677
_diffrn_reflns_theta_full        74.51
_diffrn_reflns_theta_max         74.51
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_exptl_absorpt_coefficient_mu    4.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72658
_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            brown
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         1.788
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         13717
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.11
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+6.8416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2171
_reflns_number_gt                10934
_reflns_number_total             13717
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt51562a.txt
_cod_data_source_block           compound2
_cod_original_cell_volume        3542.1(2)
_cod_database_code               7021807