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_4081602
_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, Sb F6'
_chemical_formula_sum            'C31 H41 F6 N2 P2 Sb Si2'
_chemical_formula_weight         795.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000(15)
_cell_angle_beta                 97.3450(13)
_cell_angle_gamma                90.0000(14)
_cell_formula_units_Z            4
_cell_length_a                   11.0280(4)
_cell_length_b                   13.9200(5)
_cell_length_c                   24.6140(10)
_cell_measurement_reflns_used    21257
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      1.7
_cell_volume                     3747.5(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20399
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.8062
_exptl_absorpt_correction_T_min  0.7169
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.643
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8082
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+30.1081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                6402
_reflns_number_total             8082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400649c_si_001.cif
_cod_data_source_block           compound4A
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4081602