#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:52:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178705 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/16/4081603.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4081603
loop_
_publ_author_name
'Thirumoorthi, Ramalingam'
'Chivers, Tristram'
'Gendy, Chris'
'Vargas-Baca, Ignacio'
_publ_section_title
;
 CH--NH Tautomerism in the Products of the Reactions of the Methanide
 [HC(PPh2NSiMe3)2]−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       'phiω 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/[σ²(Fo²)+(0.0083P)²+11.3531P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Te1 Te 0.49548(3) 0.55412(3) 0.13642(2) 0.02673(8) Uani 1 1 d .
I1 I 0.48220(4) 0.76079(3) 0.21805(3) 0.03764(10) Uani 1 1 d .
I2 I 0.50748(4) 0.43175(3) 0.28096(2) 0.03463(9) Uani 1 1 d .
I3 I 0.51718(4) 0.34160(3) 0.03845(2) 0.03492(9) Uani 1 1 d .
Si1 Si 0.81252(15) -0.08837(12) 0.75196(9) 0.0279(3) Uani 1 1 d .
Si2 Si 0.79386(16) 0.15033(13) 0.50681(10) 0.0319(3) Uani 1 1 d .
P1 P 1.05353(13) 0.12618(10) 0.79334(8) 0.0200(2) Uani 1 1 d .
P2 P 1.03781(12) 0.27520(11) 0.64442(8) 0.0210(3) Uani 1 1 d .
N1 N 0.9179(4) 0.0428(4) 0.7364(3) 0.0237(9) Uani 1 1 d D
H1 H 0.895(6) 0.073(5) 0.696(3) 0.04(2) Uiso 1 1 d D
N2 N 0.9107(4) 0.1829(4) 0.5989(3) 0.0269(9) Uani 1 1 d .
C1 C 1.1650(5) 0.0467(4) 0.8431(3) 0.0233(10) Uani 1 1 d .
C2 C 1.2006(6) -0.0309(5) 0.7928(4) 0.0334(12) Uani 1 1 d .
H2 H 1.1668 -0.0398 0.7348 0.040 Uiso 1 1 calc R
C3 C 1.2854(6) -0.0939(5) 0.8287(4) 0.0422(15) Uani 1 1 d .
H3 H 1.3083 -0.1462 0.7951 0.051 Uiso 1 1 calc R
C4 C 1.3371(6) -0.0797(5) 0.9149(4) 0.0436(15) Uani 1 1 d .
H4 H 1.3946 -0.1227 0.9390 0.052 Uiso 1 1 calc R
C5 C 1.3044(7) -0.0031(6) 0.9648(4) 0.0446(15) Uani 1 1 d .
H5 H 1.3399 0.0060 1.0227 0.054 Uiso 1 1 calc R
C6 C 1.2187(6) 0.0610(5) 0.9295(3) 0.0304(12) Uani 1 1 d .
H6 H 1.1969 0.1135 0.9635 0.036 Uiso 1 1 calc R
C7 C 1.0199(5) 0.2155(4) 0.8714(3) 0.0214(10) Uani 1 1 d .
C8 C 0.8881(5) 0.2023(4) 0.8824(3) 0.0279(11) Uani 1 1 d .
H8 H 0.8174 0.1469 0.8493 0.033 Uiso 1 1 calc R
C9 C 0.8616(6) 0.2714(5) 0.9425(3) 0.0314(12) Uani 1 1 d .
H9 H 0.7729 0.2630 0.9495 0.038 Uiso 1 1 calc R
C10 C 0.9664(6) 0.3527(5) 0.9922(3) 0.0345(13) Uani 1 1 d .
H10 H 0.9483 0.3982 1.0333 0.041 Uiso 1 1 calc R
C11 C 1.0969(6) 0.3671(5) 0.9817(4) 0.0377(14) Uani 1 1 d .
H11 H 1.1671 0.4221 1.0157 0.045 Uiso 1 1 calc R
C12 C 1.1247(5) 0.3000(4) 0.9204(3) 0.0300(11) Uani 1 1 d .
H12 H 1.2130 0.3114 0.9120 0.036 Uiso 1 1 calc R
C13 C 1.0029(5) 0.3886(4) 0.7018(3) 0.0232(10) Uani 1 1 d .
C14 C 1.1064(6) 0.4833(5) 0.7397(4) 0.0333(12) Uani 1 1 d .
H14 H 1.1958 0.4878 0.7358 0.040 Uiso 1 1 calc R
C15 C 1.0771(7) 0.5696(5) 0.7827(4) 0.0423(15) Uani 1 1 d .
H15 H 1.1464 0.6323 0.8079 0.051 Uiso 1 1 calc R
C16 C 0.9446(7) 0.5631(5) 0.7883(4) 0.0387(14) Uani 1 1 d .
H16 H 0.9244 0.6224 0.8162 0.046 Uiso 1 1 calc R
C17 C 0.8422(6) 0.4695(5) 0.7530(4) 0.0381(14) Uani 1 1 d .
H17 H 0.7534 0.4647 0.7584 0.046 Uiso 1 1 calc R
C18 C 0.8713(5) 0.3829(5) 0.7096(3) 0.0288(11) Uani 1 1 d .
H18 H 0.8017 0.3200 0.6853 0.035 Uiso 1 1 calc R
C19 C 1.1547(5) 0.3432(4) 0.5812(3) 0.0244(10) Uani 1 1 d .
C20 C 1.1338(6) 0.4390(5) 0.5435(4) 0.0402(14) Uani 1 1 d .
H20 H 1.0668 0.4714 0.5558 0.048 Uiso 1 1 calc R
C21 C 1.2120(6) 0.4865(5) 0.4878(4) 0.0415(15) Uani 1 1 d .
H21 H 1.1942 0.5483 0.4604 0.050 Uiso 1 1 calc R
C22 C 1.3154(5) 0.4436(5) 0.4725(3) 0.0322(12) Uani 1 1 d .
H22 H 1.3682 0.4763 0.4351 0.039 Uiso 1 1 calc R
C23 C 1.3407(5) 0.3524(5) 0.5124(3) 0.0321(12) Uani 1 1 d .
H23 H 1.4125 0.3242 0.5030 0.038 Uiso 1 1 calc R
C24 C 1.2611(5) 0.3012(4) 0.5667(3) 0.0273(11) Uani 1 1 d .
H24 H 1.2791 0.2389 0.5934 0.033 Uiso 1 1 calc R
C25 C 1.1415(5) 0.2122(4) 0.7237(3) 0.0224(10) Uani 1 1 d .
H25A H 1.1856 0.1663 0.6947 0.027 Uiso 1 1 calc R
H25B H 1.2123 0.2727 0.7577 0.027 Uiso 1 1 calc R
C26 C 0.8553(7) -0.1174(5) 0.8639(4) 0.0421(15) Uani 1 1 d .
H26A H 0.9433 -0.1325 0.8757 0.063 Uiso 1 1 calc R
H26B H 0.7885 -0.1820 0.8746 0.063 Uiso 1 1 calc R
H26C H 0.8564 -0.0529 0.8996 0.063 Uiso 1 1 calc R
C27 C 0.6369(6) -0.0748(5) 0.7216(5) 0.0531(18) Uani 1 1 d .
H27A H 0.6233 -0.0193 0.7600 0.080 Uiso 1 1 calc R
H27B H 0.5743 -0.1463 0.7238 0.080 Uiso 1 1 calc R
H27C H 0.6215 -0.0516 0.6653 0.080 Uiso 1 1 calc R
C28 C 0.8421(7) -0.1971(5) 0.6829(4) 0.0397(14) Uani 1 1 d .
H28A H 0.8287 -0.1766 0.6258 0.060 Uiso 1 1 calc R
H28B H 0.7796 -0.2684 0.6859 0.060 Uiso 1 1 calc R
H28C H 0.9336 -0.2034 0.7007 0.060 Uiso 1 1 calc R
C29 C 0.6285(6) 0.1679(7) 0.5240(5) 0.0547(18) Uani 1 1 d .
H29A H 0.6057 0.1284 0.5715 0.082 Uiso 1 1 calc R
H29B H 0.5592 0.1377 0.4746 0.082 Uiso 1 1 calc R
H29C H 0.6349 0.2468 0.5350 0.082 Uiso 1 1 calc R
C30 C 0.7715(8) -0.0011(5) 0.4719(5) 0.0551(19) Uani 1 1 d .
H30A H 0.8570 -0.0123 0.4646 0.083 Uiso 1 1 calc R
H30B H 0.7066 -0.0209 0.4193 0.083 Uiso 1 1 calc R
H30C H 0.7394 -0.0479 0.5139 0.083 Uiso 1 1 calc R
C31 C 0.8438(8) 0.2357(6) 0.4198(4) 0.0520(18) Uani 1 1 d .
H31A H 0.8452 0.3130 0.4328 0.078 Uiso 1 1 calc R
H31B H 0.7793 0.2067 0.3681 0.078 Uiso 1 1 calc R
H31C H 0.9325 0.2313 0.4136 0.078 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
I2 Te1 I1 96.69(3) .
I2 Te1 I3 87.15(3) .
I1 Te1 I3 175.880(18) .
I2 Te1 I3 171.818(16) 2_665
I1 Te1 I3 91.49(3) 2_665
I3 Te1 I3 84.68(3) 2_665
Te1 I3 Te1 95.32(3) 2_665
N1 Si1 C28 107.7(3) .
N1 Si1 C27 105.8(3) .
C28 Si1 C27 111.3(3) .
N1 Si1 C26 109.5(2) .
C28 Si1 C26 110.6(3) .
C27 Si1 C26 111.8(3) .
N2 Si2 C29 109.6(3) .
N2 Si2 C31 113.8(3) .
C29 Si2 C31 109.3(4) .
N2 Si2 C30 108.2(3) .
C29 Si2 C30 108.3(3) .
C31 Si2 C30 107.4(3) .
N1 P1 C1 110.3(2) .
N1 P1 C7 113.4(2) .
C1 P1 C7 109.5(2) .
N1 P1 C25 107.6(2) .
C1 P1 C25 106.6(2) .
C7 P1 C25 109.2(2) .
N2 P2 C13 115.0(2) .
N2 P2 C19 117.4(2) .
C13 P2 C19 105.1(2) .
N2 P2 C25 109.3(2) .
C13 P2 C25 104.9(2) .
C19 P2 C25 103.9(2) .
P1 N1 Si1 133.2(3) .
P1 N1 H1 108(5) .
Si1 N1 H1 119(5) .
P2 N2 Si2 141.9(3) .
C6 C1 C2 119.4(5) .
C6 C1 P1 122.3(4) .
C2 C1 P1 118.3(4) .
C3 C2 C1 120.1(5) .
C3 C2 H2 120.0 .
C1 C2 H2 120.0 .
C2 C3 C4 120.0(6) .
C2 C3 H3 120.0 .
C4 C3 H3 120.0 .
C5 C4 C3 120.6(6) .
C5 C4 H4 119.7 .
C3 C4 H4 119.7 .
C4 C5 C6 120.0(6) .
C4 C5 H5 120.0 .
C6 C5 H5 120.0 .
C5 C6 C1 119.9(5) .
C5 C6 H6 120.1 .
C1 C6 H6 120.1 .
C8 C7 C12 119.5(5) .
C8 C7 P1 119.8(4) .
C12 C7 P1 120.6(4) .
C9 C8 C7 120.0(5) .
C9 C8 H8 120.0 .
C7 C8 H8 120.0 .
C10 C9 C8 120.0(5) .
C10 C9 H9 120.0 .
C8 C9 H9 120.0 .
C11 C10 C9 120.6(5) .
C11 C10 H10 119.7 .
C9 C10 H10 119.7 .
C10 C11 C12 120.1(5) .
C10 C11 H11 120.0 .
C12 C11 H11 120.0 .
C11 C12 C7 119.8(5) .
C11 C12 H12 120.1 .
C7 C12 H12 120.1 .
C18 C13 C14 118.8(5) .
C18 C13 P2 119.7(4) .
C14 C13 P2 121.5(4) .
C15 C14 C13 120.5(5) .
C15 C14 H14 119.7 .
C13 C14 H14 119.7 .
C14 C15 C16 119.8(6) .
C14 C15 H15 120.1 .
C16 C15 H15 120.1 .
C17 C16 C15 120.4(5) .
C17 C16 H16 119.8 .
C15 C16 H16 119.8 .
C16 C17 C18 119.9(5) .
C16 C17 H17 120.0 .
C18 C17 H17 120.0 .
C17 C18 C13 120.6(5) .
C17 C18 H18 119.7 .
C13 C18 H18 119.7 .
C24 C19 C20 118.9(5) .
C24 C19 P2 122.6(4) .
C20 C19 P2 118.5(4) .
C21 C20 C19 120.1(5) .
C21 C20 H20 119.9 .
C19 C20 H20 119.9 .
C22 C21 C20 120.6(6) .
C22 C21 H21 119.7 .
C20 C21 H21 119.7 .
C21 C22 C23 119.5(5) .
C21 C22 H22 120.2 .
C23 C22 H22 120.2 .
C22 C23 C24 120.9(5) .
C22 C23 H23 119.5 .
C24 C23 H23 119.5 .
C19 C24 C23 119.7(5) .
C19 C24 H24 120.2 .
C23 C24 H24 120.2 .
P1 C25 P2 116.3(3) .
P1 C25 H25A 108.2 .
P2 C25 H25A 108.2 .
P1 C25 H25B 108.2 .
P2 C25 H25B 108.2 .
H25A C25 H25B 107.4 .
Si1 C26 H26A 109.5 .
Si1 C26 H26B 109.5 .
H26A C26 H26B 109.5 .
Si1 C26 H26C 109.5 .
H26A C26 H26C 109.5 .
H26B C26 H26C 109.5 .
Si1 C27 H27A 109.5 .
Si1 C27 H27B 109.5 .
H27A C27 H27B 109.5 .
Si1 C27 H27C 109.5 .
H27A C27 H27C 109.5 .
H27B C27 H27C 109.5 .
Si1 C28 H28A 109.5 .
Si1 C28 H28B 109.5 .
H28A C28 H28B 109.5 .
Si1 C28 H28C 109.5 .
H28A C28 H28C 109.5 .
H28B C28 H28C 109.5 .
Si2 C29 H29A 109.5 .
Si2 C29 H29B 109.5 .
H29A C29 H29B 109.5 .
Si2 C29 H29C 109.5 .
H29A C29 H29C 109.5 .
H29B C29 H29C 109.5 .
Si2 C30 H30A 109.5 .
Si2 C30 H30B 109.5 .
H30A C30 H30B 109.5 .
Si2 C30 H30C 109.5 .
H30A C30 H30C 109.5 .
H30B C30 H30C 109.5 .
Si2 C31 H31A 109.5 .
Si2 C31 H31B 109.5 .
H31A C31 H31B 109.5 .
Si2 C31 H31C 109.5 .
H31A C31 H31C 109.5 .
H31B C31 H31C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te1 I2 2.8211(9) .
Te1 I1 2.8628(11) .
Te1 I3 3.0821(11) .
Te1 I3 3.1395(10) 2_665
I3 Te1 3.1395(10) 2_665
Si1 N1 1.763(5) .
Si1 C28 1.833(6) .
Si1 C27 1.844(7) .
Si1 C26 1.850(6) .
Si2 N2 1.695(4) .
Si2 C29 1.854(7) .
Si2 C31 1.861(7) .
Si2 C30 1.865(6) .
P1 N1 1.613(4) .
P1 C1 1.783(5) .
P1 C7 1.785(5) .
P1 C25 1.795(5) .
P2 N2 1.547(4) .
P2 C13 1.794(5) .
P2 C19 1.806(5) .
P2 C25 1.828(5) .
N1 H1 0.79(2) .
C1 C6 1.391(7) .
C1 C2 1.394(7) .
C2 C3 1.368(8) .
C2 H2 0.9300 .
C3 C4 1.384(9) .
C3 H3 0.9300 .
C4 C5 1.365(9) .
C4 H4 0.9300 .
C5 C6 1.382(8) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.385(7) .
C7 C12 1.393(7) .
C8 C9 1.380(7) .
C8 H8 0.9300 .
C9 C10 1.377(8) .
C9 H9 0.9300 .
C10 C11 1.367(8) .
C10 H10 0.9300 .
C11 C12 1.385(8) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C18 1.381(7) .
C13 C14 1.399(7) .
C14 C15 1.375(8) .
C14 H14 0.9300 .
C15 C16 1.379(9) .
C15 H15 0.9300 .
C16 C17 1.375(9) .
C16 H16 0.9300 .
C17 C18 1.380(8) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C24 1.383(7) .
C19 C20 1.385(8) .
C20 C21 1.378(8) .
C20 H20 0.9300 .
C21 C22 1.364(8) .
C21 H21 0.9300 .
C22 C23 1.365(8) .
C22 H22 0.9300 .
C23 C24 1.384(7) .
C23 H23 0.9300 .
C24 H24 0.9300 .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
