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_4081599
_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
'2(C31 H39 I N2 P2 Sb1 Si2), 2(Sb F6), (C H2 Cl2)'
_chemical_formula_sum            'C63 H80 Cl2 F12 I2 N4 P4 Sb4 Si4'
_chemical_formula_weight         2169.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7360(4)
_cell_length_b                   19.1750(5)
_cell_length_c                   23.7080(4)
_cell_measurement_reflns_used    27895
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      1.7
_cell_volume                     8062.8(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26710
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    2.364
_exptl_absorpt_correction_T_max  0.7332
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0000P)^2^+84.3232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                6649
_reflns_number_total             8713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400649c_si_001.cif
_cod_data_source_block           compound[(SbI)2][SbF6]
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               4081599