#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/70/4077052.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_4077052
loop_
_publ_author_name
'Gavenonis, John'
'Tilley, T. Don'
_publ_section_title
;
 Tantalum Alkyl and Silyl Complexes of the Bulky (Terphenyl)imido Ligand
 [2,6-(2,4,6-Me3C6H2)2C6H3N]2-([Ar*N]2-). Generation and Reactivity of
 [(Ar*N)(Ar*NH)Ta(H)(OSO2CF3)], Which Reversibly Transfers Hydride to an
 Aromatic Ring of the Arylamide Ligand
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5549
_journal_paper_doi               10.1021/om020509y
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C50 H57 N2 Ta '
_chemical_formula_sum            'C50 H57 N2 Ta'
_chemical_formula_weight         866.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2430(7)
_cell_length_b                   11.1702(5)
_cell_length_c                   21.552(1)
_cell_measurement_reflns_used    2701
_cell_measurement_temperature    161.2
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      4.0
_cell_volume                     4246.8(3)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.052d'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      161.2
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       ω-scan
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19234
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.619
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.51
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.650
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         3140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0380
_refine_ls_wR_factor_gt          0.0243
_refine_ls_wR_factor_ref         0.0243
_reflns_number_gt                3140
_reflns_number_total             8557
_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            om020509y.cif
_cod_data_source_block           Complex_4
_cod_original_cell_volume        4246.7(3)
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_original_formula_sum        'C50 H57 N2 Ta '
_cod_database_code               4077052
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,1/2+y,1/2-z'
'   -x,   -y,   -z'
'   +x,1/2-y,1/2+z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Ta(1) 0.31592(2) -0.05365(3) 0.67258(2) 0.02669(8) Uij
N(1) 0.2290(3) -0.1026(4) 0.6826(2) 0.029(2) Uij
N(2) 0.2884(4) 0.1000(5) 0.6253(3) 0.034(2) Uij
C(1) 0.3853(4) -0.0355(7) 0.7682(3) 0.031(3) Uij
C(2) 0.3490(5) -0.2089(6) 0.6290(3) 0.032(3) Uij
C(3) 0.1624(5) -0.1627(6) 0.6861(4) 0.030(3) Uij
C(4) 0.1528(5) -0.2023(6) 0.7456(4) 0.029(3) Uij
C(5) 0.0870(6) -0.2645(7) 0.7467(4) 0.042(3) Uij
C(6) 0.0322(5) -0.2862(7) 0.6911(5) 0.059(4) Uij
C(7) 0.0407(5) -0.2457(7) 0.6330(4) 0.050(3) Uij
C(8) 0.1050(5) -0.1821(6) 0.6291(4) 0.030(3) Uij
C(9) 0.2133(5) -0.1788(7) 0.8051(4) 0.029(3) Uij
C(10) 0.2682(5) -0.2647(6) 0.8306(4) 0.031(3) Uij
C(11) 0.3242(5) -0.2408(7) 0.8856(4) 0.044(3) Uij
C(12) 0.3286(5) -0.1302(8) 0.9165(4) 0.044(3) Uij
C(13) 0.2744(5) -0.0469(9) 0.8896(4) 0.042(3) Uij
C(14) 0.2177(5) -0.0661(8) 0.8348(4) 0.045(3) Uij
C(15) 0.1136(4) -0.1313(7) 0.5683(4) 0.029(3) Uij
C(16) 0.0958(4) -0.0108(6) 0.5536(4) 0.030(3) Uij
C(17) 0.1079(4) 0.0415(7) 0.4985(4) 0.036(2) Uij
C(18) 0.1395(5) -0.0239(7) 0.4575(4) 0.037(3) Uij
C(19) 0.1574(5) -0.1439(7) 0.4713(4) 0.041(3) Uij
C(20) 0.1452(5) -0.1960(7) 0.5258(4) 0.041(3) Uij
C(21) 0.2676(5) -0.3830(7) 0.7967(4) 0.041(3) Uij
C(22) 0.3910(6) -0.1033(7) 0.9748(4) 0.053(4) Uij
C(23) 0.1636(5) 0.0325(7) 0.8060(4) 0.050(3) Uij
C(24) 0.0632(4) 0.0650(7) 0.5985(3) 0.035(3) Uij
C(25) 0.1518(5) 0.0315(7) 0.3974(4) 0.056(3) Uij
C(26) 0.1667(5) -0.3260(7) 0.5397(4) 0.048(3) Uij
C(27) 0.3303(4) 0.2048(6) 0.6202(3) 0.028(3) Uij
C(28) 0.4064(4) 0.1947(6) 0.6192(3) 0.028(2) Uij
C(29) 0.4481(4) 0.2988(7) 0.6174(4) 0.034(3) Uij
C(30) 0.4156(5) 0.4107(6) 0.6152(3) 0.037(3) Uij
C(31) 0.3392(5) 0.4190(6) 0.6145(3) 0.033(3) Uij
C(32) 0.2956(5) 0.3193(7) 0.6179(3) 0.029(3) Uij
C(33) 0.4440(4) 0.0771(7) 0.6184(4) 0.031(3) Uij
C(34) 0.5045(4) 0.0431(8) 0.6703(4) 0.039(3) Uij
C(35) 0.5442(4) -0.0628(8) 0.6667(4) 0.036(3) Uij
C(36) 0.5296(5) -0.1313(7) 0.6115(4) 0.039(3) Uij
C(37) 0.4731(5) -0.0923(7) 0.5593(4) 0.036(3) Uij
C(38) 0.4288(4) 0.0071(7) 0.5623(4) 0.032(3) Uij
C(39) 0.2142(4) 0.3325(6) 0.6168(4) 0.028(3) Uij
C(40) 0.1595(5) 0.3539(6) 0.5597(4) 0.031(3) Uij
C(41) 0.0854(5) 0.3767(6) 0.5604(4) 0.029(3) Uij
C(42) 0.0634(5) 0.3799(6) 0.6172(4) 0.035(3) Uij
C(43) 0.1175(5) 0.3586(6) 0.6733(4) 0.034(3) Uij
C(44) 0.1918(5) 0.3351(6) 0.6742(4) 0.032(3) Uij
C(45) 0.5289(5) 0.1196(7) 0.7299(4) 0.039(3) Uij
C(46) 0.5734(5) -0.2442(7) 0.6077(4) 0.050(3) Uij
C(47) 0.3650(4) 0.0397(7) 0.5049(3) 0.038(3) Uij
C(48) 0.1817(4) 0.3507(7) 0.4966(4) 0.036(3) Uij
C(49) -0.0185(5) 0.4039(7) 0.6165(4) 0.049(3) Uij
C(50) 0.2490(5) 0.3120(7) 0.7373(4) 0.039(3) Uij
H(1) 0.240(4) 0.117(6) 0.620(3) 0.0446 Uij
H(2) 0.4372 -0.0374 0.7677 0.0372 Uij
H(3) 0.3751 -0.0995 0.7938 0.0372 Uij
H(4) 0.3745 0.0385 0.7857 0.0372 Uij
H(5) 0.4016 -0.2044 0.6309 0.0379 Uij
H(6) 0.3208 -0.2133 0.5854 0.0379 Uij
H(7) 0.3395 -0.2783 0.6512 0.0379 Uij
H(8) -0.0121 -0.3296 0.6928 0.0703 Uij
H(9) 0.0021 -0.2615 0.5950 0.0597 Uij
H(10) 0.0799 -0.2923 0.7864 0.0510 Uij
H(11) 0.0943 0.1228 0.4890 0.0432 Uij
H(12) 0.1783 -0.1901 0.4430 0.0497 Uij
H(13) 0.3606 -0.3008 0.9028 0.0530 Uij
H(14) 0.2763 0.0287 0.9101 0.0504 Uij
H(15) 0.1021 0.0839 0.6358 0.0419 Uij
H(16) 0.0242 0.0218 0.6105 0.0419 Uij
H(17) 0.0430 0.1369 0.5774 0.0419 Uij
H(18) 0.1990 0.0725 0.4072 0.0669 Uij
H(19) 0.1121 0.0864 0.3803 0.0669 Uij
H(20) 0.1522 -0.0295 0.3667 0.0669 Uij
H(21) 0.1919 -0.3547 0.5091 0.0577 Uij
H(22) 0.1222 -0.3720 0.5370 0.0577 Uij
H(23) 0.1994 -0.3328 0.5816 0.0577 Uij
H(24) 0.3020 -0.4365 0.8236 0.0491 Uij
H(25) 0.2825 -0.3709 0.7580 0.0491 Uij
H(26) 0.2180 -0.4160 0.7870 0.0491 Uij
H(27) 0.3966 -0.0191 0.9800 0.0642 Uij
H(28) 0.3791 -0.1369 1.0116 0.0642 Uij
H(29) 0.4370 -0.1369 0.9700 0.0642 Uij
H(30) 0.1638 0.0430 0.7623 0.0604 Uij
H(31) 0.1140 0.0121 0.8087 0.0604 Uij
H(32) 0.1790 0.1048 0.8288 0.0604 Uij
H(33) 0.4448 0.4808 0.6142 0.0438 Uij
H(34) 0.5001 0.2924 0.6176 0.0405 Uij
H(35) 0.3162 0.4958 0.6115 0.0399 Uij
H(36) 0.5822 -0.0883 0.7032 0.0429 Uij
H(37) 0.4646 -0.1353 0.5200 0.0430 Uij
H(38) 0.0487 0.3904 0.5211 0.0346 Uij
H(39) 0.1031 0.3601 0.7127 0.0407 Uij
H(40) 0.4858 0.1573 0.7383 0.0467 Uij
H(41) 0.5636 0.1789 0.7234 0.0467 Uij
H(42) 0.5528 0.0707 0.7653 0.0467 Uij
H(43) 0.5477 -0.3107 0.6197 0.0602 Uij
H(44) 0.6226 -0.2381 0.6359 0.0602 Uij
H(45) 0.5776 -0.2549 0.5650 0.0602 Uij
H(46) 0.3213 -0.0062 0.5054 0.0453 Uij
H(47) 0.3799 0.0233 0.4666 0.0453 Uij
H(48) 0.3537 0.1225 0.5065 0.0453 Uij
H(49) 0.2247 0.4005 0.4995 0.0436 Uij
H(50) 0.1936 0.2709 0.4876 0.0436 Uij
H(51) 0.1406 0.3788 0.4632 0.0436 Uij
H(52) -0.0508 0.3689 0.5793 0.0588 Uij
H(53) -0.0270 0.4878 0.6161 0.0588 Uij
H(54) -0.0291 0.3699 0.6537 0.0588 Uij
H(55) 0.2767 0.2412 0.7340 0.0465 Uij
H(56) 0.2829 0.3778 0.7474 0.0465 Uij
H(57) 0.2234 0.3023 0.7702 0.0465 Uij
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 200 0.003 0.002 'International Tables'
H 0 228 0.000 0.000 'International Tables'
N 0 8 0.006 0.003 'International Tables'
Ta 0 4 -0.705 6.523 'International Tables'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(1) Ta(1) N(2) 102.4(3) yes
N(1) Ta(1) C(1) 104.2(3) yes
N(1) Ta(1) C(2) 99.7(3) yes
N(2) Ta(1) C(1) 115.0(3) yes
N(2) Ta(1) C(2) 122.5(3) yes
C(1) Ta(1) C(2) 109.7(3) yes
Ta(1) N(1) C(3) 169.2(5) yes
Ta(1) N(2) C(27) 132.8(5) yes
N(1) C(3) C(4) 120.6(7) yes
N(1) C(3) C(8) 119.1(7) yes
C(4) C(3) C(8) 120.3(7) yes
C(3) C(4) C(5) 118.7(8) yes
C(3) C(4) C(9) 119.5(7) yes
C(5) C(4) C(9) 121.8(8) yes
C(4) C(5) C(6) 120.9(8) yes
C(5) C(6) C(7) 120.7(8) yes
C(6) C(7) C(8) 120.9(8) yes
C(3) C(8) C(7) 118.4(8) yes
C(3) C(8) C(15) 119.3(7) yes
C(7) C(8) C(15) 122.2(8) yes
C(4) C(9) C(10) 121.2(7) yes
C(4) C(9) C(14) 119.7(7) yes
C(10) C(9) C(14) 119.0(8) yes
C(9) C(10) C(11) 120.3(7) yes
C(9) C(10) C(21) 119.8(7) yes
C(11) C(10) C(21) 119.9(7) yes
C(10) C(11) C(12) 121.4(8) yes
C(11) C(12) C(13) 116.7(8) yes
C(11) C(12) C(22) 121.2(8) yes
C(13) C(12) C(22) 122.1(8) yes
C(12) C(13) C(14) 124.1(9) yes
C(9) C(14) C(13) 118.3(9) yes
C(9) C(14) C(23) 120.9(8) yes
C(13) C(14) C(23) 120.7(9) yes
C(8) C(15) C(16) 120.0(8) yes
C(8) C(15) C(20) 122.5(7) yes
C(16) C(15) C(20) 117.2(8) yes
C(15) C(16) C(17) 121.2(8) yes
C(15) C(16) C(24) 119.8(8) yes
C(17) C(16) C(24) 119.0(7) yes
C(16) C(17) C(18) 120.5(7) yes
C(17) C(18) C(19) 119.0(8) yes
C(17) C(18) C(25) 120.8(7) yes
C(19) C(18) C(25) 120.1(8) yes
C(18) C(19) C(20) 120.5(8) yes
C(15) C(20) C(19) 121.5(8) yes
C(15) C(20) C(26) 119.6(8) yes
C(19) C(20) C(26) 118.9(8) yes
N(2) C(27) C(28) 119.5(7) yes
N(2) C(27) C(32) 120.0(7) yes
C(28) C(27) C(32) 120.5(7) yes
C(27) C(28) C(29) 118.9(7) yes
C(27) C(28) C(33) 122.3(7) yes
C(29) C(28) C(33) 118.7(7) yes
C(28) C(29) C(30) 121.6(7) yes
C(29) C(30) C(31) 118.7(7) yes
C(30) C(31) C(32) 122.3(7) yes
C(27) C(32) C(31) 118.0(7) yes
C(27) C(32) C(39) 121.6(7) yes
C(31) C(32) C(39) 120.4(7) yes
C(28) C(33) C(34) 119.9(7) yes
C(28) C(33) C(38) 120.8(7) yes
C(34) C(33) C(38) 118.4(7) yes
C(33) C(34) C(35) 119.7(7) yes
C(33) C(34) C(45) 121.6(8) yes
C(35) C(34) C(45) 118.7(7) yes
C(34) C(35) C(36) 121.8(7) yes
C(35) C(36) C(37) 117.7(7) yes
C(35) C(36) C(46) 121.5(8) yes
C(37) C(36) C(46) 120.8(8) yes
C(36) C(37) C(38) 122.3(7) yes
C(33) C(38) C(37) 119.8(7) yes
C(33) C(38) C(47) 120.8(7) yes
C(37) C(38) C(47) 119.5(8) yes
C(32) C(39) C(40) 121.2(7) yes
C(32) C(39) C(44) 120.2(7) yes
C(40) C(39) C(44) 118.3(8) yes
C(39) C(40) C(41) 120.2(8) yes
C(39) C(40) C(48) 119.7(8) yes
C(41) C(40) C(48) 120.1(8) yes
C(40) C(41) C(42) 121.5(8) yes
C(41) C(42) C(43) 118.1(8) yes
C(41) C(42) C(49) 120.3(8) yes
C(43) C(42) C(49) 121.6(8) yes
C(42) C(43) C(44) 121.9(8) yes
C(39) C(44) C(43) 120.0(7) yes
C(39) C(44) C(50) 120.2(8) yes
C(43) C(44) C(50) 119.8(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ta(1) N(1) 1.743(6) yes
Ta(1) N(2) 1.994(6) yes
Ta(1) C(1) 2.136(7) yes
Ta(1) C(2) 2.132(7) yes
N(1) C(3) 1.405(9) yes
N(2) C(27) 1.418(9) yes
C(3) C(4) 1.409(9) yes
C(3) C(8) 1.414(10) yes
C(4) C(5) 1.39(1) yes
C(4) C(9) 1.487(10) yes
C(5) C(6) 1.37(1) yes
C(6) C(7) 1.38(1) yes
C(7) C(8) 1.392(10) yes
C(8) C(15) 1.473(10) yes
C(9) C(10) 1.395(9) yes
C(9) C(14) 1.405(10) yes
C(10) C(11) 1.380(10) yes
C(10) C(21) 1.508(9) yes
C(11) C(12) 1.396(10) yes
C(12) C(13) 1.37(1) yes
C(12) C(22) 1.50(1) yes
C(13) C(14) 1.374(10) yes
C(14) C(23) 1.50(1) yes
C(15) C(16) 1.402(9) yes
C(15) C(20) 1.402(10) yes
C(16) C(17) 1.390(9) yes
C(16) C(24) 1.516(9) yes
C(17) C(18) 1.381(9) yes
C(18) C(19) 1.39(1) yes
C(18) C(25) 1.503(10) yes
C(19) C(20) 1.379(10) yes
C(20) C(26) 1.51(1) yes
C(27) C(28) 1.399(9) yes
C(27) C(32) 1.422(9) yes
C(28) C(29) 1.395(9) yes
C(28) C(33) 1.484(9) yes
C(29) C(30) 1.379(9) yes
C(30) C(31) 1.395(10) yes
C(31) C(32) 1.381(9) yes
C(32) C(39) 1.487(10) yes
C(33) C(34) 1.409(9) yes
C(33) C(38) 1.406(9) yes
C(34) C(35) 1.40(1) yes
C(34) C(45) 1.511(10) yes
C(35) C(36) 1.381(10) yes
C(36) C(37) 1.388(10) yes
C(36) C(46) 1.51(1) yes
C(37) C(38) 1.385(9) yes
C(38) C(47) 1.511(9) yes
C(39) C(40) 1.393(9) yes
C(39) C(44) 1.398(9) yes
C(40) C(41) 1.380(10) yes
C(40) C(48) 1.513(9) yes
C(41) C(42) 1.381(10) yes
C(42) C(43) 1.373(10) yes
C(42) C(49) 1.52(1) yes
C(43) C(44) 1.377(10) yes
C(44) C(50) 1.511(10) yes
