#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/24/8102488.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_8102488
loop_
_publ_author_name
'Stephan Peter Blöß'
'Jürgen Nuss'
'Martin Jansen'
_publ_section_title
;
 Crystal structure of bis(trichloro-bis(diethylamido)tantalum(V)),
 [TaCl3(C4H10N)2]2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              499
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'C16 H40 Cl6 N4 Ta2 '
_chemical_formula_sum            'C8 H20 Cl3 N2 Ta'
_chemical_formula_weight         431.56
_chemical_name_systematic        bis(trichloro-bis(diethylamido)-tantalum(V))
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                83.7050(10)
_cell_angle_beta                 87.7900(10)
_cell_angle_gamma                87.3350(10)
_cell_formula_units_Z            4
_cell_length_a                   9.1629(6)
_cell_length_b                   10.9357(7)
_cell_length_c                   14.1722(9)
_cell_measurement_reflns_used    8063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.07
_cell_measurement_theta_min      2.68
_cell_volume                     1409.20(16)
_computing_cell_refinement       'SAINT32 (Bruker AXS)'
_computing_data_collection       'SMART32 (Bruker AXS)'
_computing_data_reduction        'SAINT32 (Bruker AXS)'
_computing_molecular_graphics    'ATOMS (Dowty, 2008) [9]'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 [8]'
_computing_structure_solution    'SHELXS-97 [7]'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       '3-circle goniometer'
_diffrn_measurement_device_type  'SMART APEX I, Bruker AXS'
_diffrn_measurement_method       \wscans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22085
_diffrn_reflns_theta_full        34.06
_diffrn_reflns_theta_max         34.06
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.339
_exptl_absorpt_correction_T_max  0.287
_exptl_absorpt_correction_T_min  0.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
semi empirical absorption correction with SADABS,
G.M. Sheldrick, SADABS, Version 2008/1, University of Göttingen. Germany. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.616
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         11238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0329P)²+1.2848P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                10717
_reflns_number_total             11238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2678.cff
_cod_data_source_block           blo25_m
_cod_database_code               8102488
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.913249(9) 0.860070(8) 0.087749(6) 0.01454(3) Uani 1 1 d . . .
Ta2 Ta 0.469157(9) 0.355050(8) 0.422799(6) 0.01495(3) Uani 1 1 d . . .
Cl11 Cl 1.16277(6) 0.95552(5) 0.03907(4) 0.01715(9) Uani 1 1 d . . .
Cl12 Cl 0.88302(6) 1.01033(5) 0.19498(4) 0.01864(9) Uani 1 1 d . . .
Cl13 Cl 0.96636(7) 0.75052(6) -0.04487(4) 0.02306(11) Uani 1 1 d . . .
Cl21 Cl 0.32372(6) 0.51543(5) 0.51814(4) 0.01889(10) Uani 1 1 d . . .
Cl22 Cl 0.48977(7) 0.23422(6) 0.57051(4) 0.02051(10) Uani 1 1 d . . .
Cl23 Cl 0.45069(7) 0.51461(5) 0.29573(4) 0.02106(10) Uani 1 1 d . . .
N1 N 0.9947(2) 0.7376(2) 0.18331(15) 0.0193(4) Uani 1 1 d . . .
N2 N 0.7143(2) 0.8060(2) 0.09280(15) 0.0192(4) Uani 1 1 d . . .
N3 N 0.6106(2) 0.26370(19) 0.35011(15) 0.0171(3) Uani 1 1 d . . .
N4 N 0.2979(2) 0.27366(19) 0.38935(15) 0.0175(3) Uani 1 1 d . . .
C11 C 1.1217(3) 0.7605(3) 0.23953(19) 0.0243(5) Uani 1 1 d . . .
H11A H 1.161(4) 0.838(4) 0.211(3) 0.029 Uiso 1 1 d . . .
H11B H 1.202(4) 0.694(4) 0.225(3) 0.029 Uiso 1 1 d . . .
C12 C 1.0833(4) 0.7624(3) 0.3441(2) 0.0330(6) Uani 1 1 d . . .
H12A H 1.009(5) 0.822(4) 0.356(3) 0.040 Uiso 1 1 d . . .
H12B H 1.172(5) 0.770(4) 0.372(3) 0.040 Uiso 1 1 d . . .
H12C H 1.041(5) 0.684(4) 0.373(3) 0.040 Uiso 1 1 d . . .
C13 C 0.9427(3) 0.6105(2) 0.2037(2) 0.0248(5) Uani 1 1 d . . .
H13A H 0.849(4) 0.609(4) 0.172(3) 0.030 Uiso 1 1 d . . .
H13B H 0.929(4) 0.590(4) 0.274(3) 0.030 Uiso 1 1 d . . .
C14 C 1.0454(5) 0.5176(3) 0.1616(3) 0.0400(8) Uani 1 1 d . . .
H14A H 1.082(5) 0.544(5) 0.099(4) 0.048 Uiso 1 1 d . . .
H14B H 1.005(5) 0.431(5) 0.167(3) 0.048 Uiso 1 1 d . . .
H14C H 1.139(6) 0.511(5) 0.185(4) 0.048 Uiso 1 1 d . . .
C21 C 0.6276(3) 0.8067(3) 0.1834(2) 0.0235(5) Uani 1 1 d . . .
H21A H 0.694(4) 0.804(4) 0.233(3) 0.028 Uiso 1 1 d . . .
H21B H 0.579(4) 0.726(4) 0.196(3) 0.028 Uiso 1 1 d . . .
C22 C 0.5151(3) 0.9135(3) 0.1817(2) 0.0319(6) Uani 1 1 d . . .
H22A H 0.565(5) 0.995(4) 0.167(3) 0.038 Uiso 1 1 d . . .
H22B H 0.463(5) 0.910(4) 0.240(3) 0.038 Uiso 1 1 d . . .
H22C H 0.448(5) 0.906(4) 0.135(3) 0.038 Uiso 1 1 d . . .
C23 C 0.6276(4) 0.7683(3) 0.0156(2) 0.0300(6) Uani 1 1 d . . .
H23A H 0.679(5) 0.806(4) -0.050(3) 0.036 Uiso 1 1 d . . .
H23B H 0.530(5) 0.808(4) 0.020(3) 0.036 Uiso 1 1 d . . .
C24 C 0.6228(5) 0.6279(4) 0.0219(3) 0.0450(10) Uani 1 1 d . . .
H24A H 0.720(6) 0.586(5) 0.019(4) 0.054 Uiso 1 1 d . . .
H24B H 0.565(6) 0.601(5) -0.026(4) 0.054 Uiso 1 1 d . . .
H24C H 0.576(6) 0.592(5) 0.084(4) 0.054 Uiso 1 1 d . . .
C31 C 0.6212(3) 0.1269(2) 0.36971(18) 0.0199(4) Uani 1 1 d . . .
H31A H 0.625(4) 0.093(3) 0.307(3) 0.024 Uiso 1 1 d . . .
H31B H 0.533(4) 0.103(3) 0.398(3) 0.024 Uiso 1 1 d . . .
C32 C 0.7519(3) 0.0795(3) 0.4286(2) 0.0269(5) Uani 1 1 d . . .
H32A H 0.839(5) 0.107(4) 0.399(3) 0.032 Uiso 1 1 d . . .
H32B H 0.756(4) -0.013(4) 0.442(3) 0.032 Uiso 1 1 d . . .
H32C H 0.748(4) 0.106(4) 0.491(3) 0.032 Uiso 1 1 d . . .
C33 C 0.7169(3) 0.3110(2) 0.27474(19) 0.0213(4) Uani 1 1 d . . .
H33A H 0.805(4) 0.267(4) 0.281(3) 0.026 Uiso 1 1 d . . .
H33B H 0.732(4) 0.394(4) 0.284(3) 0.026 Uiso 1 1 d . . .
C34 C 0.6624(3) 0.3035(3) 0.1755(2) 0.0270(5) Uani 1 1 d . . .
H34A H 0.649(4) 0.225(4) 0.161(3) 0.032 Uiso 1 1 d . . .
H34B H 0.729(5) 0.332(4) 0.131(3) 0.032 Uiso 1 1 d . . .
H34C H 0.572(5) 0.353(4) 0.165(3) 0.032 Uiso 1 1 d . . .
C41 C 0.2797(3) 0.2286(2) 0.29572(18) 0.0210(4) Uani 1 1 d . . .
H41A H 0.372(4) 0.227(4) 0.263(3) 0.025 Uiso 1 1 d . . .
H41B H 0.225(4) 0.293(4) 0.256(3) 0.025 Uiso 1 1 d . . .
C42 C 0.2153(3) 0.1028(3) 0.3003(2) 0.0298(6) Uani 1 1 d . . .
H42A H 0.267(5) 0.047(4) 0.342(3) 0.036 Uiso 1 1 d . . .
H42B H 0.221(5) 0.080(4) 0.232(3) 0.036 Uiso 1 1 d . . .
H42C H 0.121(5) 0.102(4) 0.322(3) 0.036 Uiso 1 1 d . . .
C43 C 0.1633(3) 0.2714(2) 0.45097(18) 0.0204(4) Uani 1 1 d . . .
H43A H 0.185(4) 0.292(4) 0.516(3) 0.024 Uiso 1 1 d . . .
H43B H 0.135(4) 0.187(4) 0.459(3) 0.024 Uiso 1 1 d . . .
C44 C 0.0439(3) 0.3611(3) 0.4110(2) 0.0272(5) Uani 1 1 d . . .
H44A H 0.072(5) 0.435(4) 0.400(3) 0.033 Uiso 1 1 d . . .
H44B H -0.046(5) 0.354(4) 0.446(3) 0.033 Uiso 1 1 d . . .
H44C H 0.018(5) 0.343(4) 0.349(3) 0.033 Uiso 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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 N1 98.71(9) . . ?
N2 Ta1 Cl12 98.59(7) . . ?
N1 Ta1 Cl12 92.81(6) . . ?
N2 Ta1 Cl13 89.74(7) . . ?
N1 Ta1 Cl13 97.28(7) . . ?
Cl12 Ta1 Cl13 165.82(2) . . ?
N2 Ta1 Cl11 165.81(6) . . ?
N1 Ta1 Cl11 94.28(7) . . ?
Cl12 Ta1 Cl11 86.386(19) . . ?
Cl13 Ta1 Cl11 82.95(2) . . ?
N2 Ta1 Cl11 89.39(6) . 2_775 ?
N1 Ta1 Cl11 171.58(6) . 2_775 ?
Cl12 Ta1 Cl11 83.66(2) . 2_775 ?
Cl13 Ta1 Cl11 84.98(2) . 2_775 ?
Cl11 Ta1 Cl11 77.900(18) . 2_775 ?
N3 Ta2 N4 96.84(8) . . ?
N3 Ta2 Cl22 98.35(6) . . ?
N4 Ta2 Cl22 93.63(6) . . ?
N3 Ta2 Cl23 90.97(6) . . ?
N4 Ta2 Cl23 94.45(6) . . ?
Cl22 Ta2 Cl23 166.84(2) . . ?
N3 Ta2 Cl21 166.98(6) . . ?
N4 Ta2 Cl21 95.24(6) . . ?
Cl22 Ta2 Cl21 85.67(2) . . ?
Cl23 Ta2 Cl21 83.27(2) . . ?
N3 Ta2 Cl21 91.18(6) . 2_666 ?
N4 Ta2 Cl21 171.97(6) . 2_666 ?
Cl22 Ta2 Cl21 85.40(2) . 2_666 ?
Cl23 Ta2 Cl21 85.14(2) . 2_666 ?
Cl21 Ta2 Cl21 76.748(19) . 2_666 ?
Ta1 Cl11 Ta1 102.101(19) . 2_775 ?
Ta2 Cl21 Ta2 103.252(19) . 2_666 ?
C11 N1 C13 113.2(2) . . ?
C11 N1 Ta1 122.69(17) . . ?
C13 N1 Ta1 124.04(17) . . ?
C23 N2 C21 112.1(2) . . ?
C23 N2 Ta1 129.15(18) . . ?
C21 N2 Ta1 118.71(16) . . ?
C33 N3 C31 112.42(19) . . ?
C33 N3 Ta2 128.80(16) . . ?
C31 N3 Ta2 118.78(16) . . ?
C43 N4 C41 114.14(19) . . ?
C43 N4 Ta2 121.02(16) . . ?
C41 N4 Ta2 124.05(16) . . ?
N1 C11 C12 112.9(2) . . ?
N1 C13 C14 111.8(3) . . ?
N2 C21 C22 112.6(2) . . ?
N2 C23 C24 110.9(2) . . ?
N3 C31 C32 113.4(2) . . ?
N3 C33 C34 112.3(2) . . ?
N4 C41 C42 114.7(2) . . ?
N4 C43 C44 112.5(2) . . ?
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 1.938(2) . ?
Ta1 N1 1.942(2) . ?
Ta1 Cl12 2.3577(6) . ?
Ta1 Cl13 2.3609(6) . ?
Ta1 Cl11 2.5952(6) . ?
Ta1 Cl11 2.6370(6) 2_775 ?
Ta2 N3 1.934(2) . ?
Ta2 N4 1.939(2) . ?
Ta2 Cl22 2.3589(6) . ?
Ta2 Cl23 2.3713(6) . ?
Ta2 Cl21 2.6156(6) . ?
Ta2 Cl21 2.6346(6) 2_666 ?
Cl11 Ta1 2.6370(6) 2_775 ?
Cl21 Ta2 2.6346(6) 2_666 ?
N1 C11 1.481(3) . ?
N1 C13 1.485(3) . ?
N2 C23 1.481(3) . ?
N2 C21 1.485(3) . ?
N3 C33 1.484(3) . ?
N3 C31 1.490(3) . ?
N4 C43 1.483(3) . ?
N4 C41 1.483(3) . ?
C11 C12 1.512(4) . ?
C13 C14 1.508(5) . ?
C21 C22 1.520(4) . ?
C23 C24 1.531(5) . ?
C31 C32 1.524(4) . ?
C33 C34 1.522(4) . ?
C41 C42 1.516(4) . ?
C43 C44 1.519(4) . ?
