#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/51/4075166.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_4075166
loop_
_publ_author_name
'Anderson, Laura L.'
'Schmidt, Joseph A. R.'
'Arnold, John'
'Bergman, Robert G.'
_publ_section_title
;
 Neutral and Cationic Alkyl Tantalum Imido Complexes: Synthesis and
 Migratory Insertion Reactions.
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3394
_journal_page_last               3406
_journal_paper_doi               10.1021/om060081t
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C25 H30 N Ta '
_chemical_formula_sum            'C25 H30 N Ta'
_chemical_formula_weight         525.47
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      159
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_primary     direct
_audit_creation_date             'Sat Feb  2 17:57:44 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   11.1584(4)
_cell_length_b                   11.1584(4)
_cell_length_c                   10.1563(5)
_cell_measurement_reflns_used    4201
_cell_measurement_temperature    133.2
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      3.0
_cell_volume                     1095.14(8)
_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      133.2
_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  0.0413
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4878
_diffrn_reflns_theta_max         24.70
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.020
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            color
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520.00
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.50
_refine_diff_density_min         -1.48
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0315
_refine_ls_wR_factor_gt          0.0307
_reflns_number_gt                2062
_reflns_number_total             2340
_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            om060081tsi20060125_023927.cif
_cod_data_source_block           Bn3Ta_NtBu_for_L2A_by_JS
_cod_original_cell_volume        1095.14(7)
_cod_original_sg_symbol_H-M      'P 3 1 c    '
_cod_original_formula_sum        'C25 H30 N Ta '
_cod_database_code               4075166
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -y,   +x-y,   +z'
'   -x+y,   -x,   +z'
'   +y,   +x,1/2+z'
'   -x,   -x+y,1/2+z'
'   +x-y,   -y,1/2+z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ta(1) 0.0217(1) 0.022 0.0258(1) 0.011 0.000 0.000
N(1) 0.029(2) 0.029 0.006(3) 0.015 0.000 0.000
C(1) 0.027(2) 0.020(2) 0.037(3) 0.010(2) 0.002(2) 0.001(2)
C(2) 0.016(2) 0.022(2) 0.043(3) 0.005(2) 0.011(2) 0.002(2)
C(3) 0.035(2) 0.025(2) 0.036(3) 0.013(2) 0.004(2) -0.007(2)
C(4) 0.043(3) 0.041(3) 0.030(3) 0.018(2) 0.007(2) 0.003(2)
C(5) 0.035(2) 0.027(2) 0.041(3) 0.014(2) 0.012(2) 0.010(2)
C(6) 0.022(2) 0.023(2) 0.045(3) 0.006(2) 0.007(2) -0.009(2)
C(7) 0.021(2) 0.025(2) 0.038(3) 0.005(2) 0.000(2) -0.004(2)
C(8) 0.037(3) 0.037 0.020(4) 0.018 0.000 0.000
C(9) 0.039(3) 0.053(3) 0.048(3) 0.019(3) 0.013(2) 0.011(3)
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) -0.333 0.333 0.270 0.023 Uij
N(1) -0.333 0.333 0.4411(6) 0.021 Uij
C(1) -0.1076(4) 0.4513(5) 0.2322(4) 0.030 Uij
C(2) -0.1203(4) 0.5652(5) 0.1709(5) 0.027 Uij
C(3) -0.1559(5) 0.5609(5) 0.0374(5) 0.033 Uij
C(4) -0.1830(6) 0.6596(5) -0.0159(5) 0.039 Uij
C(5) -0.1735(5) 0.7662(5) 0.0616(5) 0.035 Uij
C(6) -0.1366(4) 0.7732(5) 0.1936(5) 0.032 Uij
C(7) -0.1110(5) 0.6756(4) 0.2482(5) 0.031 Uij
C(8) -0.333 0.333 0.5860(8) 0.025 Uij
C(9) -0.4835(6) 0.2604(6) 0.6315(6) 0.050 Uij
H(1) -0.077 0.406 0.174 0.036 Uij
H(2) -0.053 0.478 0.310 0.036 Uij
H(3) -0.162 0.489 -0.017 0.040 Uij
H(4) -0.207 0.655 -0.106 0.047 Uij
H(5) -0.193 0.833 0.025 0.042 Uij
H(6) -0.128 0.847 0.247 0.039 Uij
H(7) -0.087 0.682 0.339 0.037 Uij
H(8) -0.530 0.167 0.600 0.060 Uij
H(9) -0.528 0.307 0.598 0.060 Uij
H(10) -0.487 0.260 0.725 0.060 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 50 0.003 0.002 'International Tables'
H 0 60 0.000 0.000 'International Tables'
N 0 2 0.006 0.003 'International Tables'
Ta 0 2 -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) C(1) 100.0(1) yes
N(1) Ta(1) C(1) 100.0(1) yes
N(1) Ta(1) C(1) 100.0(1) yes
C(1) Ta(1) C(1) 117.06(7) yes
C(1) Ta(1) C(1) 117.06(7) yes
C(1) Ta(1) C(1) 117.06(7) yes
Ta(1) N(1) C(8) 180.0 yes
Ta(1) C(1) C(2) 90.8(3) yes
C(1) C(2) C(3) 121.4(4) yes
C(1) C(2) C(7) 120.9(5) yes
C(3) C(2) C(7) 117.4(4) yes
C(2) C(3) C(4) 121.2(4) yes
C(3) C(4) C(5) 120.4(5) yes
C(4) C(5) C(6) 119.2(5) yes
C(5) C(6) C(7) 121.2(4) yes
C(2) C(7) C(6) 120.7(5) yes
N(1) C(8) C(9) 107.7(4) yes
N(1) C(8) C(9) 107.7(4) yes
N(1) C(8) C(9) 107.7(4) yes
C(9) C(8) C(9) 111.2(4) yes
C(9) C(8) C(9) 111.2(4) yes
C(9) C(8) C(9) 111.2(4) 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) 1.737(6) yes
Ta(1) C(1) 2.216(4) yes
Ta(1) C(1) 2.216(4) yes
Ta(1) C(1) 2.216(4) yes
N(1) C(8) 1.47(1) yes
C(1) C(2) 1.485(6) yes
C(2) C(3) 1.407(7) yes
C(2) C(7) 1.420(7) yes
C(3) C(4) 1.389(8) yes
C(4) C(5) 1.385(7) yes
C(5) C(6) 1.393(7) yes
C(6) C(7) 1.373(8) yes
C(8) C(9) 1.524(6) yes
C(8) C(9) 1.524(6) yes
C(8) C(9) 1.524(6) yes
