#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/18/4311877.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_4311877
loop_
_publ_author_name
'Xianghua Yu'
'Siwei Bi'
'Ilia A. Guzei'
'Zhenyang Lin'
'Zi-Ling Xue'
_publ_section_title
;
 Zirconium, Hafnium, and Tantalum Amide Silyl Complexes: Their Preparation
 and Conversion to Metallaheterocyclic Complexes via γ-Hydrogen
 Abstraction by Silyl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7111
_journal_page_last               7119
_journal_paper_doi               10.1021/ic049023v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C28 H55 N4 Si3 Ta'
_chemical_formula_weight         712.98
_chemical_name_systematic
; 
tantalum amide silyl
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 124.894(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.771(3)
_cell_length_b                   33.042(8)
_cell_length_c                   12.751(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3376.6(17)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       multi-scan
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35528
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    3.384
_exptl_absorpt_correction_T_max  0.4301
_exptl_absorpt_correction_T_min  0.2576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.522
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0261
_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/[σ²(Fo²)+(0.0172P)²+3.8589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                7438
_reflns_number_total             8104
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049023vrom20040721_122003.cif
_cod_data_source_block           tguzei
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3376.6(15)
_cod_database_code               4311877
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.760284(12) 0.129125(3) 0.069629(10) 0.02064(4) Uani 1 1 d . . .
Si1 Si 0.78527(9) 0.13829(2) 0.30752(7) 0.02227(15) Uani 1 1 d . . .
Si2 Si 0.64984(10) 0.04964(3) -0.10628(8) 0.03141(17) Uani 1 1 d . . .
Si3 Si 0.72696(11) 0.11794(3) -0.21503(9) 0.03395(18) Uani 1 1 d . . .
N1 N 0.5214(3) 0.12457(7) 0.0048(2) 0.0281(5) Uani 1 1 d . . .
N2 N 0.8121(3) 0.18575(7) 0.0645(2) 0.0288(5) Uani 1 1 d . . .
N3 N 0.9794(3) 0.10229(7) 0.1844(2) 0.0283(5) Uani 1 1 d . . .
N4 N 0.7146(3) 0.10009(7) -0.0916(2) 0.0254(5) Uani 1 1 d . . .
C1 C 0.4290(4) 0.10406(11) 0.0471(3) 0.0381(7) Uani 1 1 d . . .
H1A H 0.3685 0.1242 0.0623 0.046(10) Uiso 1 1 d R . .
H1B H 0.5069 0.0893 0.1265 0.052(11) Uiso 1 1 d R . .
H1C H 0.3493 0.0850 -0.0188 0.042(10) Uiso 1 1 d R . .
C2 C 0.4036(4) 0.14236(10) -0.1222(3) 0.0369(7) Uani 1 1 d . . .
H2A H 0.3283 0.1213 -0.1818 0.068(13) Uiso 1 1 d R . .
H2B H 0.4657 0.1542 -0.1536 0.034(9) Uiso 1 1 d R . .
H2C H 0.3382 0.1635 -0.1159 0.042(10) Uiso 1 1 d R . .
C3 C 0.6930(4) 0.21956(9) 0.0028(3) 0.0362(7) Uani 1 1 d . . .
H3A H 0.7168 0.2396 0.0679 0.054(11) Uiso 1 1 d R . .
H3B H 0.5790 0.2094 -0.0385 0.040(9) Uiso 1 1 d R . .
H3C H 0.7042 0.2323 -0.0614 0.059(12) Uiso 1 1 d R . .
C4 C 0.9815(4) 0.20119(9) 0.1194(3) 0.0363(7) Uani 1 1 d . . .
H4A H 0.9967 0.2065 0.0511 0.048(10) Uiso 1 1 d R . .
H4B H 1.0634 0.1810 0.1784 0.044(10) Uiso 1 1 d R . .
H4C H 0.9975 0.2263 0.1660 0.051(11) Uiso 1 1 d R . .
C5 C 1.0837(4) 0.10470(11) 0.1354(3) 0.0409(8) Uani 1 1 d . . .
H5A H 1.1958 0.1139 0.2040 0.021(7) Uiso 1 1 d R . .
H5B H 1.0341 0.1240 0.0643 0.024(8) Uiso 1 1 d R . .
H5C H 1.0908 0.0780 0.1055 0.040(9) Uiso 1 1 d R . .
C6 C 1.0537(4) 0.07361(9) 0.2899(3) 0.0365(7) Uani 1 1 d . . .
H6A H 1.0702 0.0475 0.2621 0.039(9) Uiso 1 1 d R . .
H6B H 0.9797 0.0700 0.3178 0.043(10) Uiso 1 1 d R . .
H6C H 1.1616 0.0841 0.3610 0.051(11) Uiso 1 1 d R . .
C7 C 0.7093(5) 0.02780(11) 0.0500(3) 0.0468(9) Uani 1 1 d . . .
H7A H 0.8303 0.0236 0.1053 0.052(11) Uiso 1 1 d R . .
H7B H 0.6523 0.0019 0.0351 0.059(12) Uiso 1 1 d R . .
H7C H 0.6767 0.0466 0.0915 0.051(11) Uiso 1 1 d R . .
C8 C 0.7540(5) 0.01510(11) -0.1575(4) 0.0493(9) Uani 1 1 d . . .
H8A H 0.7210 0.0228 -0.2433 0.074(14) Uiso 1 1 d R . .
H8B H 0.7199 -0.0129 -0.1588 0.063(13) Uiso 1 1 d R . .
H8C H 0.8754 0.0174 -0.0973 0.059(12) Uiso 1 1 d R . .
C9 C 0.4190(4) 0.04241(11) -0.2190(3) 0.0407(7) Uani 1 1 d . . .
H9A H 0.3639 0.0535 -0.1809 0.056(11) Uiso 1 1 d R . .
H9B H 0.3939 0.0135 -0.2357 0.073(14) Uiso 1 1 d R . .
H9C H 0.3783 0.0565 -0.2995 0.063(13) Uiso 1 1 d R . .
C10 C 0.9243(5) 0.10347(15) -0.1973(4) 0.0558(10) Uani 1 1 d . . .
H10A H 1.0151 0.1212 -0.1341 0.069(14) Uiso 1 1 d R . .
H10B H 0.9091 0.1064 -0.2798 0.102(18) Uiso 1 1 d R . .
H10C H 0.9520 0.0753 -0.1688 0.074(15) Uiso 1 1 d R . .
C11 C 0.5476(4) 0.09981(12) -0.3748(3) 0.0450(8) Uani 1 1 d . . .
H11A H 0.5419 0.0702 -0.3745 0.059(12) Uiso 1 1 d R . .
H11B H 0.5633 0.1085 -0.4408 0.067(13) Uiso 1 1 d R . .
H11C H 0.4436 0.1113 -0.3931 0.069(13) Uiso 1 1 d R . .
C12 C 0.7161(6) 0.17477(11) -0.2296(4) 0.0566(11) Uani 1 1 d . . .
H12A H 0.6125 0.1843 -0.2426 0.070(14) Uiso 1 1 d R . .
H12B H 0.7182 0.1828 -0.3026 0.072(14) Uiso 1 1 d R . .
H12C H 0.8117 0.1867 -0.1513 0.074(15) Uiso 1 1 d R . .
C13 C 0.9730(3) 0.17253(9) 0.4350(3) 0.0291(6) Uani 1 1 d . . .
C14 C 0.9420(4) 0.21561(9) 0.3809(3) 0.0354(7) Uani 1 1 d . . .
H14A H 1.0407 0.2323 0.4378 0.050(11) Uiso 1 1 d R . .
H14B H 0.8453 0.2272 0.3747 0.045(10) Uiso 1 1 d R . .
H14C H 0.9204 0.2148 0.2958 0.044(10) Uiso 1 1 d R . .
C15 C 0.9905(4) 0.17472(11) 0.5629(3) 0.0392(7) Uani 1 1 d . . .
H15A H 1.0847 0.1923 0.6224 0.035(9) Uiso 1 1 d R . .
H15B H 1.0102 0.1475 0.5995 0.046(10) Uiso 1 1 d R . .
H15C H 0.8877 0.1858 0.5481 0.040(9) Uiso 1 1 d R . .
C16 C 1.1416(4) 0.15845(10) 0.4641(3) 0.0378(7) Uani 1 1 d . . .
H16A H 1.1339 0.1566 0.3842 0.047(10) Uiso 1 1 d R . .
H16B H 1.1698 0.1318 0.5053 0.052(11) Uiso 1 1 d R . .
H16C H 1.2285 0.1780 0.5213 0.048(10) Uiso 1 1 d R . .
C17 C 0.6046(3) 0.17058(8) 0.2828(3) 0.0273(6) Uani 1 1 d . . .
C18 C 0.5207(4) 0.19846(9) 0.1823(3) 0.0345(7) Uani 1 1 d . . .
H18 H 0.5426 0.1987 0.1187 0.051(11) Uiso 1 1 d R . .
C19 C 0.4061(4) 0.22575(10) 0.1727(4) 0.0442(8) Uani 1 1 d . . .
H19 H 0.3520 0.2444 0.1036 0.062(12) Uiso 1 1 d R . .
C20 C 0.3702(4) 0.22607(10) 0.2620(4) 0.0468(9) Uani 1 1 d . . .
H20 H 0.2932 0.2451 0.2561 0.061(12) Uiso 1 1 d R . .
C21 C 0.4473(4) 0.19842(10) 0.3608(4) 0.0431(8) Uani 1 1 d . . .
H21 H 0.4210 0.1979 0.4219 0.045(10) Uiso 1 1 d R . .
C22 C 0.5633(4) 0.17128(9) 0.3715(3) 0.0326(6) Uani 1 1 d . . .
H22 H 0.6158 0.1527 0.4408 0.034(9) Uiso 1 1 d R . .
C23 C 0.7826(4) 0.09213(9) 0.3976(3) 0.0279(6) Uani 1 1 d . . .
C24 C 0.9272(4) 0.07126(9) 0.4933(3) 0.0343(7) Uani 1 1 d . . .
H24 H 1.0329 0.0810 0.5173 0.040(10) Uiso 1 1 d R . .
C25 C 0.9216(5) 0.03692(10) 0.5541(3) 0.0439(8) Uani 1 1 d . . .
H25 H 1.0222 0.0238 0.6183 0.044(10) Uiso 1 1 d R . .
C26 C 0.7707(5) 0.02197(10) 0.5211(3) 0.0455(9) Uani 1 1 d . . .
H26 H 0.7663 -0.0018 0.5612 0.054(11) Uiso 1 1 d R . .
C27 C 0.6265(5) 0.04148(10) 0.4300(3) 0.0395(7) Uani 1 1 d . . .
H27 H 0.5219 0.0315 0.4080 0.045(10) Uiso 1 1 d R . .
C28 C 0.6322(4) 0.07588(9) 0.3694(3) 0.0314(6) Uani 1 1 d . . .
H28 H 0.5305 0.0889 0.3067 0.025(8) Uiso 1 1 d 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'
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
_geom_angle_publ_flag
N2 Ta1 N3 105.21(10) . . ?
N2 Ta1 N1 108.96(10) . . ?
N3 Ta1 N1 142.11(10) . . ?
N2 Ta1 N4 108.87(10) . . ?
N3 Ta1 N4 93.11(9) . . ?
N1 Ta1 N4 91.00(9) . . ?
N2 Ta1 Si1 93.83(8) . . ?
N3 Ta1 Si1 82.30(7) . . ?
N1 Ta1 Si1 79.61(7) . . ?
N4 Ta1 Si1 157.24(7) . . ?
C23 Si1 C17 102.30(13) . . ?
C23 Si1 C13 106.72(13) . . ?
C17 Si1 C13 98.65(12) . . ?
C23 Si1 Ta1 121.23(9) . . ?
C17 Si1 Ta1 111.32(9) . . ?
C13 Si1 Ta1 113.75(9) . . ?
N4 Si2 C9 113.94(14) . . ?
N4 Si2 C7 112.29(14) . . ?
C9 Si2 C7 105.82(17) . . ?
N4 Si2 C8 112.34(15) . . ?
C9 Si2 C8 108.06(16) . . ?
C7 Si2 C8 103.66(18) . . ?
N4 Si3 C11 111.63(14) . . ?
N4 Si3 C10 113.72(16) . . ?
C11 Si3 C10 107.96(18) . . ?
N4 Si3 C12 113.34(15) . . ?
C11 Si3 C12 104.30(19) . . ?
C10 Si3 C12 105.2(2) . . ?
C1 N1 C2 109.5(2) . . ?
C1 N1 Ta1 135.3(2) . . ?
C2 N1 Ta1 114.88(19) . . ?
C4 N2 C3 108.7(2) . . ?
C4 N2 Ta1 124.06(19) . . ?
C3 N2 Ta1 127.17(19) . . ?
C6 N3 C5 109.1(2) . . ?
C6 N3 Ta1 137.0(2) . . ?
C5 N3 Ta1 112.34(19) . . ?
Si3 N4 Si2 115.54(13) . . ?
Si3 N4 Ta1 130.55(13) . . ?
Si2 N4 Ta1 113.90(12) . . ?
C14 C13 C16 107.3(3) . . ?
C14 C13 C15 107.8(2) . . ?
C16 C13 C15 107.7(3) . . ?
C14 C13 Si1 108.1(2) . . ?
C16 C13 Si1 112.9(2) . . ?
C15 C13 Si1 112.8(2) . . ?
C18 C17 C22 116.1(3) . . ?
C18 C17 Si1 121.0(2) . . ?
C22 C17 Si1 122.5(2) . . ?
C19 C18 C17 121.9(3) . . ?
C20 C19 C18 120.6(3) . . ?
C19 C20 C21 119.2(3) . . ?
C20 C21 C22 120.4(3) . . ?
C21 C22 C17 121.8(3) . . ?
C28 C23 C24 114.7(3) . . ?
C28 C23 Si1 121.4(2) . . ?
C24 C23 Si1 123.8(2) . . ?
C25 C24 C23 122.8(3) . . ?
C26 C25 C24 120.0(3) . . ?
C27 C26 C25 119.6(3) . . ?
C26 C27 C28 120.4(3) . . ?
C27 C28 C23 122.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 N2 1.949(2) . ?
Ta1 N3 1.982(2) . ?
Ta1 N1 1.987(2) . ?
Ta1 N4 2.073(2) . ?
Ta1 Si1 2.9164(10) . ?
Si1 C23 1.918(3) . ?
Si1 C17 1.928(3) . ?
Si1 C13 1.969(3) . ?
Si2 N4 1.755(3) . ?
Si2 C9 1.871(3) . ?
Si2 C7 1.872(4) . ?
Si2 C8 1.878(4) . ?
Si3 N4 1.748(2) . ?
Si3 C11 1.870(4) . ?
Si3 C10 1.871(4) . ?
Si3 C12 1.884(4) . ?
N1 C1 1.457(4) . ?
N1 C2 1.470(4) . ?
N2 C4 1.471(4) . ?
N2 C3 1.474(4) . ?
N3 C6 1.455(4) . ?
N3 C5 1.470(4) . ?
C13 C14 1.535(4) . ?
C13 C16 1.539(4) . ?
C13 C15 1.541(4) . ?
C17 C18 1.401(4) . ?
C17 C22 1.402(4) . ?
C18 C19 1.387(4) . ?
C19 C20 1.370(5) . ?
C20 C21 1.379(5) . ?
C21 C22 1.389(4) . ?
C23 C28 1.405(4) . ?
C23 C24 1.410(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.374(5) . ?
C26 C27 1.371(5) . ?
C27 C28 1.393(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660897
