CH‒NH Tautomerism in the Products of the Reactions of the Methanide [HC(PPh2NSiMe3)2]−with Pnictogen and Tellurium Iodides
Thirumoorthi, Ramalingam; Chivers, Tristram; Gendy, Chris; Vargas-Baca, Ignacio; Organometallics 32 (2013) 5360–; doi:10.1021/om400649c

data_4081603
_publ_section_title
;
 CH--NH Tautomerism in the Products of the Reactions of the Methanide
 [HC(PPh2NSiMe3)2]&#x2212;with Pnictogen and Tellurium Iodides
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5360
_journal_paper_doi               10.1021/om400649c
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C31 H41 N2 P2 Si2, 0.5(I6 Te2)'
_chemical_formula_sum            'C31 H41 I3 N2 P2 Si2 Te'
_chemical_formula_weight         1068.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                91.900(5)
_cell_angle_beta                 101.227(5)
_cell_angle_gamma                104.260(5)
_cell_formula_units_Z            2
_cell_length_a                   10.380(5)
_cell_length_b                   12.247(5)
_cell_length_c                   16.205(5)
_cell_measurement_reflns_used    16369
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.1
_cell_volume                     1951.2(14)
_computing_cell_refinement       'DENZO (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 1999)'
_computing_data_reduction        'Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phi\omega scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15593
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    3.302
_exptl_absorpt_correction_T_max  0.6550
_exptl_absorpt_correction_T_min  0.4924
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelets
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0083P)^2^+11.3531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                7291
_reflns_number_total             8462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400649c_si_001.cif
_cod_data_source_block           compound4B
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4081603