(Iminophosphoranyl)(thiophosphoranyl)methanide {CH(PPh2NSiMe3)(Ph2PS)}−as a Ligand in Rare-Earth-Element Chemistry
Murugesapandian, Balasubramanian; Kuzdrowska, Magdalena; Gamer, Michael T.; Hartenstein, Larissa; Roesky, Peter W.; Organometallics 32 (2013) 1500–1506; doi:10.1021/om400001e

data_4080127
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT)
      Institut fuer Anorganische Chemie
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_publ_contact_author_email       roesky@kit.edu
_publ_contact_author_fax         '+49 721 60844854'
_publ_contact_author_phone       '+49 721 60846117'
_publ_section_title
;
 (Iminophosphoranyl)(thiophosphoranyl)methanide
 {CH(PPh2NSiMe3)(Ph2PS)}&#x2212;as a Ligand in Rare-Earth-Element
 Chemistry
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1500
_journal_page_last               1506
_journal_paper_doi               10.1021/om400001e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C36 H58 Lu N3 P2 S Si5'
_chemical_formula_sum            'C36 H58 Lu N3 P2 S Si5'
_chemical_formula_weight         942.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 92.596(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.0044(4)
_cell_length_b                   18.1553(4)
_cell_length_c                   28.2986(6)
_cell_measurement_reflns_used    100134
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      1.59
_cell_volume                     9240.6(3)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            189329
_diffrn_reflns_theta_full        25.58
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    2.408
_exptl_absorpt_correction_T_max  0.5658
_exptl_absorpt_correction_T_min  0.3941
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.397
_exptl_crystal_size_min          0.286
_refine_diff_density_max         1.240
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.284
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         17285
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+38.6413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                13693
_reflns_number_total             17285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400001e_si_001.cif
_cod_data_source_block           3d
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080127