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#$Date: 2016-03-22 11:05:44 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178884 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/13/4111381.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_4111381
loop_
_publ_author_name
'Michael P. Shaver'
'Michael D. Fryzuk'
_publ_section_title
;
 Cleavage of Hydrazine and 1,1-Dimethylhydrazine by Dinuclear Tantalum
 Hydrides: Formation of Imides, Nitrides, and N,N-Dimethylamine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              500
_journal_page_last               501
_journal_paper_doi               10.1021/ja043732q
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C24 H37 N3 P1 Si2 Ta1'
_chemical_formula_sum            'C24 H37 N3 P Si2 Ta'
_chemical_formula_weight         630.18
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.22(3)
_cell_angle_beta                 111.66(3)
_cell_angle_gamma                108.490(12)
_cell_formula_units_Z            2
_cell_length_a                   11.340(12)
_cell_length_b                   11.984(12)
_cell_length_c                   12.27(3)
_cell_measurement_reflns_used    12494
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.68
_cell_volume                     1375(4)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.864
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12494
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    4.158
_exptl_absorpt_correction_T_max  0.5350
_exptl_absorpt_correction_T_min  0.3519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Tompa-analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       irregular
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0265
_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)+(0.0271P)²+2.9813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                5480
_reflns_number_total             5657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043732qsi20041014_012607.cif
_cod_data_source_block           mf553
_cod_original_cell_volume        1375(3)
_cod_database_code               4111381
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
C1 C 0.0806(4) 0.2548(3) 0.1190(3) 0.0196(7) Uani 1 1 d .
H1A H 0.0551 0.1657 0.0750 0.024 Uiso 1 1 calc R
H1B H 0.0191 0.2826 0.0609 0.024 Uiso 1 1 calc R
C2 C 0.3161(4) 0.2485(4) 0.0799(3) 0.0226(7) Uani 1 1 d .
H2A H 0.3884 0.2988 0.0604 0.027 Uiso 1 1 calc R
H2B H 0.2343 0.1865 0.0002 0.027 Uiso 1 1 calc R
C3 C -0.0857(5) 0.1138(4) 0.2326(4) 0.0391(11) Uani 1 1 d .
H3A H -0.0531 0.0482 0.2188 0.059 Uiso 1 1 calc R
H3B H -0.1725 0.0935 0.1582 0.059 Uiso 1 1 calc R
H3C H -0.1034 0.1183 0.3053 0.059 Uiso 1 1 calc R
C4 C -0.0143(5) 0.3901(5) 0.2892(4) 0.0353(10) Uani 1 1 d .
H4A H -0.0290 0.3947 0.3635 0.053 Uiso 1 1 calc R
H4B H -0.1033 0.3674 0.2161 0.053 Uiso 1 1 calc R
H4C H 0.0547 0.4721 0.3024 0.053 Uiso 1 1 calc R
C5 C 0.2428(5) 0.0238(4) 0.1680(4) 0.0339(10) Uani 1 1 d .
H5A H 0.2824 -0.0220 0.2178 0.051 Uiso 1 1 calc R
H5B H 0.1856 -0.0314 0.0798 0.051 Uiso 1 1 calc R
H5C H 0.1843 0.0509 0.1985 0.051 Uiso 1 1 calc R
C6 C 0.4999(5) 0.1095(4) 0.1282(4) 0.0368(10) Uani 1 1 d .
H6A H 0.5771 0.1820 0.1353 0.055 Uiso 1 1 calc R
H6B H 0.4429 0.0529 0.0405 0.055 Uiso 1 1 calc R
H6C H 0.5382 0.0645 0.1800 0.055 Uiso 1 1 calc R
C7 C 0.2025(4) 0.2850(4) 0.4946(4) 0.0255(8) Uani 1 1 d .
C8 C 0.1922(6) 0.1708(5) 0.5105(5) 0.0532(15) Uani 1 1 d .
H8 H 0.1905 0.1069 0.4495 0.064 Uiso 1 1 calc R
C9 C 0.1845(7) 0.1506(9) 0.6167(8) 0.096(3) Uani 1 1 d .
H9 H 0.1765 0.0721 0.6263 0.115 Uiso 1 1 calc R
C10 C 0.1881(7) 0.2402(12) 0.7066(7) 0.105(4) Uani 1 1 d .
H10 H 0.1842 0.2256 0.7788 0.127 Uiso 1 1 calc R
C11 C 0.1974(6) 0.3515(10) 0.6903(5) 0.082(3) Uani 1 1 d .
H11 H 0.1981 0.4142 0.7516 0.099 Uiso 1 1 calc R
C12 C 0.2060(5) 0.3760(6) 0.5860(4) 0.0456(12) Uani 1 1 d .
H12 H 0.2142 0.4550 0.5779 0.055 Uiso 1 1 calc R
C13 C 0.5868(4) 0.2461(3) 0.4183(3) 0.0179(7) Uani 1 1 d .
C14 C 0.5563(4) 0.1776(4) 0.4914(4) 0.0241(7) Uani 1 1 d .
H14 H 0.4658 0.1502 0.4869 0.029 Uiso 1 1 calc R
C15 C 0.6564(5) 0.1486(4) 0.5707(4) 0.0351(10) Uani 1 1 d .
H15 H 0.6341 0.1029 0.6209 0.042 Uiso 1 1 calc R
C16 C 0.7879(5) 0.1853(5) 0.5776(4) 0.0395(11) Uani 1 1 d .
H16 H 0.8561 0.1645 0.6313 0.047 Uiso 1 1 calc R
C17 C 0.8183(5) 0.2528(5) 0.5050(5) 0.0429(11) Uani 1 1 d .
H17 H 0.9089 0.2794 0.5097 0.052 Uiso 1 1 calc R
C18 C 0.7192(4) 0.2828(4) 0.4249(4) 0.0313(9) Uani 1 1 d .
H18 H 0.7421 0.3283 0.3747 0.038 Uiso 1 1 calc R
C19 C 0.2624(4) 0.4731(3) 0.0924(3) 0.0203(7) Uani 1 1 d .
H19 H 0.1972 0.4307 0.0005 0.024 Uiso 1 1 calc R
C20 C 0.4083(4) 0.5503(4) 0.1094(4) 0.0280(8) Uani 1 1 d .
H20A H 0.4764 0.5850 0.1995 0.034 Uiso 1 1 calc R
H20B H 0.4370 0.4945 0.0647 0.034 Uiso 1 1 calc R
C21 C 0.4126(5) 0.6581(4) 0.0599(5) 0.0377(10) Uani 1 1 d .
H21A H 0.5103 0.7092 0.0789 0.045 Uiso 1 1 calc R
H21B H 0.3545 0.6231 -0.0323 0.045 Uiso 1 1 calc R
C22 C 0.3591(5) 0.7416(4) 0.1176(5) 0.0374(10) Uani 1 1 d .
H22A H 0.3579 0.8071 0.0796 0.045 Uiso 1 1 calc R
H22B H 0.4232 0.7841 0.2086 0.045 Uiso 1 1 calc R
C23 C 0.2118(5) 0.6649(4) 0.0968(4) 0.0317(9) Uani 1 1 d .
H23A H 0.1461 0.6289 0.0060 0.038 Uiso 1 1 calc R
H23B H 0.1808 0.7206 0.1385 0.038 Uiso 1 1 calc R
C24 C 0.2073(4) 0.5583(3) 0.1490(4) 0.0217(7) Uani 1 1 d .
H24A H 0.1096 0.5074 0.1299 0.026 Uiso 1 1 calc R
H24B H 0.2651 0.5946 0.2412 0.026 Uiso 1 1 calc R
N1 N 0.4821(3) 0.2741(3) 0.3351(3) 0.0172(6) Uani 1 1 d .
N2 N 0.2128(3) 0.3059(3) 0.3867(3) 0.0169(6) Uani 1 1 d .
N3 N 0.5112(8) 0.4164(6) 0.5794(6) 0.0193(13) Uani 0.50 1 d P
Si1 Si 0.05155(10) 0.26860(9) 0.26201(9) 0.0207(2) Uani 1 1 d .
Si2 Si 0.38861(10) 0.16482(9) 0.18305(9) 0.01950(19) Uiso 1 1 d .
P1 P 0.26372(9) 0.35060(8) 0.16247(8) 0.01533(17) Uani 1 1 d .
Ta1 Ta 0.409897(12) 0.396878(11) 0.402096(11) 0.01217(5) Uani 1 1 d .
H1 H 0.570(10) 0.453(9) 0.559(9) 0.12(3) Uiso 1 1 d .
H4 H 0.472(9) 0.441(8) 0.566(8) 0.01(2) Uiso 0.50 1 d P
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'
Ta Ta -0.7052 6.5227 '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_1
_geom_angle_site_symmetry_3
P1 C1 Si1 110.99(19) . .
P1 C2 Si2 108.3(2) . .
C12 C7 C8 118.4(5) . .
C12 C7 N2 122.1(4) . .
C8 C7 N2 119.5(4) . .
C7 C8 C9 119.7(7) . .
C10 C9 C8 121.8(8) . .
C9 C10 C11 118.3(6) . .
C10 C11 C12 121.8(7) . .
C7 C12 C11 119.9(6) . .
C18 C13 C14 118.4(3) . .
C18 C13 N1 121.0(3) . .
C14 C13 N1 120.5(3) . .
C15 C14 C13 120.8(4) . .
C16 C15 C14 120.8(4) . .
C17 C16 C15 118.5(4) . .
C16 C17 C18 121.5(4) . .
C13 C18 C17 119.9(4) . .
C20 C19 C24 110.9(3) . .
C20 C19 P1 111.0(3) . .
C24 C19 P1 110.3(3) . .
C21 C20 C19 112.2(3) . .
C22 C21 C20 111.7(4) . .
C21 C22 C23 110.9(4) . .
C22 C23 C24 111.3(3) . .
C23 C24 C19 111.4(3) . .
C13 N1 Si2 113.3(2) . .
C13 N1 Ta1 121.6(2) . .
Si2 N1 Ta1 122.49(17) . .
C7 N2 Si1 113.5(3) . .
C7 N2 Ta1 118.6(2) . .
Si1 N2 Ta1 127.28(18) . .
Ta1 N3 Ta1 81.4(3) . 2_666
N2 Si1 C4 111.86(19) . .
N2 Si1 C3 112.10(19) . .
C4 Si1 C3 107.8(2) . .
N2 Si1 C1 106.0(2) . .
C4 Si1 C1 111.34(19) . .
C3 Si1 C1 107.7(2) . .
N1 Si2 C6 113.3(2) . .
N1 Si2 C5 111.30(19) . .
C6 Si2 C5 108.1(2) . .
N1 Si2 C2 105.88(19) . .
C6 Si2 C2 107.8(2) . .
C5 Si2 C2 110.4(2) . .
C2 P1 C1 105.57(19) . .
C2 P1 C19 106.5(2) . .
C1 P1 C19 106.15(17) . .
C2 P1 Ta1 106.44(16) . .
C1 P1 Ta1 106.74(13) . .
C19 P1 Ta1 124.16(14) . .
N3 Ta1 N3 98.6(3) . 2_666
N3 Ta1 N2 94.6(2) . .
N3 Ta1 N2 121.2(2) 2_666 .
N3 Ta1 N1 95.1(3) . .
N3 Ta1 N1 122.3(2) 2_666 .
N2 Ta1 N1 113.04(13) . .
N3 Ta1 P1 175.15(19) . .
N3 Ta1 P1 86.2(2) 2_666 .
N2 Ta1 P1 82.45(11) . .
N1 Ta1 P1 82.58(12) . .
N3 Ta1 Ta1 50.7(2) . 2_666
N3 Ta1 Ta1 47.9(2) 2_666 2_666
N2 Ta1 Ta1 117.72(11) . 2_666
N1 Ta1 Ta1 119.07(12) . 2_666
P1 Ta1 Ta1 134.10(7) . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 P1 1.830(4) .
C1 Si1 1.888(5) .
C2 P1 1.817(4) .
C2 Si2 1.879(4) .
C3 Si1 1.868(4) .
C4 Si1 1.864(5) .
C5 Si2 1.872(5) .
C6 Si2 1.862(4) .
C7 C12 1.383(7) .
C7 C8 1.394(7) .
C7 N2 1.434(5) .
C8 C9 1.400(9) .
C9 C10 1.360(15) .
C10 C11 1.364(14) .
C11 C12 1.399(8) .
C13 C18 1.390(6) .
C13 C14 1.390(5) .
C13 N1 1.435(4) .
C14 C15 1.386(5) .
C15 C16 1.379(7) .
C16 C17 1.377(7) .
C17 C18 1.391(6) .
C19 C20 1.528(5) .
C19 C24 1.537(5) .
C19 P1 1.842(4) .
C20 C21 1.526(6) .
C21 C22 1.517(7) .
C22 C23 1.523(6) .
C23 C24 1.531(5) .
N1 Si2 1.740(4) .
N1 Ta1 2.073(3) .
N2 Si1 1.742(4) .
N2 Ta1 2.070(4) .
N3 Ta1 1.973(8) .
N3 Ta1 2.059(7) 2_666
P1 Ta1 2.624(5) .
Ta1 N3 2.059(7) 2_666
Ta1 Ta1 2.630(3) 2_666
