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#$Date: 2016-03-21 19:07:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178836 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/90/4109048.cif $
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#
# 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_4109048
loop_
_publ_author_name
'Mikhail V. Barybin'
'William W. Brennessel'
'Benjamin E. Kucera'
'Mikhail E. Minyaev'
'Victor J. Sussman'
'Victor G. Young'
'John E. Ellis'
_publ_contact_author_address
;Department of Chemistry
University of Minnesota
207 Pleasant St. SE
Minneapolis, MN 55455
USA
;
_publ_contact_author_email       ellis@chem.umn.edu
_publ_contact_author_name        'John E. Ellis'
_publ_contact_author_phone       001+612-625-6391
_publ_section_title
;
 Homoleptic Isocyanidemetalates of 4d- and 5d-Transition Metals:
 [Nb(CNXyl)6]-, [Ta(CNXyl)6]-, and Derivatives Thereof1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1141
_journal_page_last               1150
_journal_paper_doi               10.1021/ja065964q
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C54 H54 Cs N6 Ta'
_chemical_formula_sum            'C54 H54 Cs N6 Ta'
_chemical_formula_weight         1100.89
_chemical_name_common
;
Cesium hexakis(2,6-dimethylphenylisocyanido)-tantalum
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(12)
_cell_angle_beta                 90.000(12)
_cell_angle_gamma                120.000(10)
_cell_formula_units_Z            3
_cell_length_a                   23.490(16)
_cell_length_b                   23.490(16)
_cell_length_c                   7.772(5)
_cell_measurement_reflns_used    5358
_cell_measurement_temperature    173(2)
_cell_volume                     3714(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11360
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.985
_exptl_absorpt_correction_T_max  0.8899
_exptl_absorpt_correction_T_min  0.6308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       needle
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.498
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0323P)²+1.6992P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                1666
_reflns_number_total             1884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065964qsi20060823_114245_3.cif
_cod_data_source_block           00235
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4109048
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ta1 Ta 0.6667 0.3333 0.8333 0.02188(10) Uani 1 6 d S
Cs1 Cs 0.6667 0.3333 0.3333 0.03269(12) Uani 1 6 d S
N1 N 0.77809(12) 0.46117(12) 0.6085(3) 0.0358(6) Uani 1 1 d .
C1 C 0.73723(14) 0.41539(14) 0.6891(4) 0.0267(6) Uani 1 1 d .
C2 C 0.82730(14) 0.52613(14) 0.5826(4) 0.0329(7) Uani 1 1 d .
C3 C 0.86391(16) 0.54229(16) 0.4283(5) 0.0437(9) Uani 1 1 d .
C4 C 0.8504(2) 0.4900(2) 0.2977(6) 0.0656(12) Uani 1 1 d .
H4A H 0.8832 0.5085 0.2055 0.098 Uiso 1 1 calc R
H4B H 0.8064 0.4735 0.2491 0.098 Uiso 1 1 calc R
H4C H 0.8528 0.4538 0.3531 0.098 Uiso 1 1 calc R
C5 C 0.91187(17) 0.60746(18) 0.4014(6) 0.0555(11) Uani 1 1 d .
H5 H 0.9372 0.6194 0.2988 0.067 Uiso 1 1 calc R
C6 C 0.92308(17) 0.65514(18) 0.5222(6) 0.0602(12) Uani 1 1 d .
H6 H 0.9554 0.6996 0.5008 0.072 Uiso 1 1 calc R
C7 C 0.88748(18) 0.63848(17) 0.6748(6) 0.0535(11) Uani 1 1 d .
H7 H 0.8964 0.6717 0.7576 0.064 Uiso 1 1 calc R
C8 C 0.83873(16) 0.57372(16) 0.7085(5) 0.0395(8) Uani 1 1 d .
C9 C 0.7993(2) 0.55543(19) 0.8714(5) 0.0561(10) Uani 1 1 d .
H9A H 0.8171 0.5935 0.9485 0.084 Uiso 1 1 calc R
H9B H 0.8015 0.5193 0.9279 0.084 Uiso 1 1 calc R
H9C H 0.7534 0.5415 0.8443 0.084 Uiso 1 1 calc 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'
Cs Cs -0.3680 2.1192 '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
C1 Ta1 C1 85.22(11) 18_546 2_655
C1 Ta1 C1 85.22(11) 18_546 .
C1 Ta1 C1 94.79(11) 2_655 .
C1 Ta1 C1 94.79(11) 18_546 16_656
C1 Ta1 C1 85.22(11) 2_655 16_656
C1 Ta1 C1 179.993(1) . 16_656
C1 Ta1 C1 180.0 18_546 3_665
C1 Ta1 C1 94.79(11) 2_655 3_665
C1 Ta1 C1 94.79(11) . 3_665
C1 Ta1 C1 85.21(11) 16_656 3_665
C1 Ta1 C1 94.78(11) 18_546 17_556
C1 Ta1 C1 180.0 2_655 17_556
C1 Ta1 C1 85.22(11) . 17_556
C1 Ta1 C1 94.78(11) 16_656 17_556
C1 Ta1 C1 85.21(11) 3_665 17_556
C1 Ta1 Cs1 121.81(8) 18_546 .
C1 Ta1 Cs1 58.20(8) 2_655 .
C1 Ta1 Cs1 58.20(8) . .
C1 Ta1 Cs1 121.80(8) 16_656 .
C1 Ta1 Cs1 58.20(8) 3_665 .
C1 Ta1 Cs1 121.80(8) 17_556 .
C1 Ta1 Cs1 58.19(8) 18_546 1_556
C1 Ta1 Cs1 121.80(8) 2_655 1_556
C1 Ta1 Cs1 121.80(8) . 1_556
C1 Ta1 Cs1 58.20(8) 16_656 1_556
C1 Ta1 Cs1 121.80(8) 3_665 1_556
C1 Ta1 Cs1 58.20(8) 17_556 1_556
Cs1 Ta1 Cs1 180.0 . 1_556
C1 Cs1 C1 56.58(9) 18_545 16_655
C1 Cs1 C1 123.43(9) 18_545 2_655
C1 Cs1 C1 123.43(9) 16_655 2_655
C1 Cs1 C1 123.43(9) 18_545 .
C1 Cs1 C1 180.00(4) 16_655 .
C1 Cs1 C1 56.57(9) 2_655 .
C1 Cs1 C1 56.57(9) 18_545 17
C1 Cs1 C1 56.57(9) 16_655 17
C1 Cs1 C1 180.0 2_655 17
C1 Cs1 C1 123.42(9) . 17
C1 Cs1 C1 180.0 18_545 3_665
C1 Cs1 C1 123.42(9) 16_655 3_665
C1 Cs1 C1 56.57(9) 2_655 3_665
C1 Cs1 C1 56.57(9) . 3_665
C1 Cs1 C1 123.42(9) 17 3_665
C1 Cs1 N1 19.75(6) 18_545 18_545
C1 Cs1 N1 73.62(8) 16_655 18_545
C1 Cs1 N1 106.90(8) 2_655 18_545
C1 Cs1 N1 106.38(8) . 18_545
C1 Cs1 N1 73.10(8) 17 18_545
C1 Cs1 N1 160.25(6) 3_665 18_545
C1 Cs1 N1 106.39(8) 18_545 2_655
C1 Cs1 N1 106.90(8) 16_655 2_655
C1 Cs1 N1 19.75(6) 2_655 2_655
C1 Cs1 N1 73.10(8) . 2_655
C1 Cs1 N1 160.25(6) 17 2_655
C1 Cs1 N1 73.62(8) 3_665 2_655
N1 Cs1 N1 92.60(7) 18_545 2_655
C1 Cs1 N1 73.10(8) 18_545 16_655
C1 Cs1 N1 19.75(6) 16_655 16_655
C1 Cs1 N1 106.38(8) 2_655 16_655
C1 Cs1 N1 160.25(6) . 16_655
C1 Cs1 N1 73.62(8) 17 16_655
C1 Cs1 N1 106.90(8) 3_665 16_655
N1 Cs1 N1 87.41(7) 18_545 16_655
N1 Cs1 N1 92.59(7) 2_655 16_655
C1 Cs1 N1 106.90(8) 18_545 .
C1 Cs1 N1 160.25(6) 16_655 .
C1 Cs1 N1 73.62(8) 2_655 .
C1 Cs1 N1 19.75(6) . .
C1 Cs1 N1 106.38(8) 17 .
C1 Cs1 N1 73.10(8) 3_665 .
N1 Cs1 N1 92.59(7) 18_545 .
N1 Cs1 N1 87.41(7) 2_655 .
N1 Cs1 N1 180.00(6) 16_655 .
C1 Cs1 N1 160.24(6) 18_545 3_665
C1 Cs1 N1 106.38(8) 16_655 3_665
C1 Cs1 N1 73.10(8) 2_655 3_665
C1 Cs1 N1 73.62(8) . 3_665
C1 Cs1 N1 106.90(8) 17 3_665
C1 Cs1 N1 19.75(6) 3_665 3_665
N1 Cs1 N1 180.0 18_545 3_665
N1 Cs1 N1 87.41(7) 2_655 3_665
N1 Cs1 N1 92.59(7) 16_655 3_665
N1 Cs1 N1 87.41(7) . 3_665
C1 Cs1 N1 73.62(8) 18_545 17
C1 Cs1 N1 73.10(8) 16_655 17
C1 Cs1 N1 160.24(6) 2_655 17
C1 Cs1 N1 106.90(8) . 17
C1 Cs1 N1 19.75(6) 17 17
C1 Cs1 N1 106.38(8) 3_665 17
N1 Cs1 N1 87.41(7) 18_545 17
N1 Cs1 N1 180.0 2_655 17
N1 Cs1 N1 87.40(7) 16_655 17
N1 Cs1 N1 92.59(7) . 17
N1 Cs1 N1 92.59(7) 3_665 17
C1 N1 C2 155.7(3) . .
C1 N1 Cs1 68.59(19) . .
C2 N1 Cs1 134.2(2) . .
N1 C1 Ta1 178.4(3) . .
N1 C1 Cs1 91.7(2) . .
Ta1 C1 Cs1 88.63(10) . .
N1 C2 C8 119.6(3) . .
N1 C2 C3 118.5(3) . .
C8 C2 C3 121.9(3) . .
C5 C3 C2 118.2(3) . .
C5 C3 C4 121.5(3) . .
C2 C3 C4 120.2(3) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 C3 120.7(4) . .
C6 C5 H5 119.6 . .
C3 C5 H5 119.6 . .
C5 C6 C7 120.5(3) . .
C5 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C6 C7 C8 121.1(4) . .
C6 C7 H7 119.4 . .
C8 C7 H7 119.4 . .
C7 C8 C2 117.5(3) . .
C7 C8 C9 121.5(3) . .
C2 C8 C9 121.0(3) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 C1 2.127(3) 18_546
Ta1 C1 2.127(3) 2_655
Ta1 C1 2.127(3) .
Ta1 C1 2.127(3) 16_656
Ta1 C1 2.127(3) 3_665
Ta1 C1 2.127(3) 17_556
Ta1 Cs1 3.886(3) .
Ta1 Cs1 3.886(3) 1_556
Cs1 C1 3.303(3) 18_545
Cs1 C1 3.304(3) 16_655
Cs1 C1 3.304(3) 2_655
Cs1 C1 3.304(3) .
Cs1 C1 3.304(3) 17
Cs1 C1 3.304(3) 3_665
Cs1 N1 3.547(3) 18_545
Cs1 N1 3.547(3) 2_655
Cs1 N1 3.547(3) 16_655
Cs1 N1 3.547(3) .
Cs1 N1 3.547(3) 3_665
Cs1 N1 3.547(3) 17
N1 C1 1.199(4) .
N1 C2 1.393(4) .
C2 C8 1.407(5) .
C2 C3 1.413(5) .
C3 C5 1.390(5) .
C3 C4 1.500(5) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.382(6) .
C5 H5 0.9500 .
C6 C7 1.390(6) .
C6 H6 0.9500 .
C7 C8 1.397(5) .
C7 H7 0.9500 .
C8 C9 1.499(5) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C1 Cs1 N1 C1 149.0(2) 18_545
C1 Cs1 N1 C1 -180.0 16_655
C1 Cs1 N1 C1 28.3(2) 2_655
C1 Cs1 N1 C1 -151.7(2) 17
C1 Cs1 N1 C1 -31.0(2) 3_665
N1 Cs1 N1 C1 135.18(18) 18_545
N1 Cs1 N1 C1 42.69(18) 2_655
N1 Cs1 N1 C1 -90.5(14) 16_655
N1 Cs1 N1 C1 -44.83(18) 3_665
N1 Cs1 N1 C1 -137.30(18) 17
C1 Cs1 N1 C2 -20.7(3) 18_545
C1 Cs1 N1 C2 10.3(4) 16_655
C1 Cs1 N1 C2 -141.4(3) 2_655
C1 Cs1 N1 C2 -169.7(4) .
C1 Cs1 N1 C2 38.6(3) 17
C1 Cs1 N1 C2 159.3(3) 3_665
N1 Cs1 N1 C2 -34.5(3) 18_545
N1 Cs1 N1 C2 -127.0(3) 2_655
N1 Cs1 N1 C2 100(100) 16_655
N1 Cs1 N1 C2 145.5(3) 3_665
N1 Cs1 N1 C2 53.0(3) 17
C2 N1 C1 Ta1 -98(10) .
Cs1 N1 C1 Ta1 100(10) .
C2 N1 C1 Cs1 161.9(7) .
C1 Ta1 C1 N1 127(10) 18_546
C1 Ta1 C1 N1 -148(10) 2_655
C1 Ta1 C1 N1 -5(9) 16_656
C1 Ta1 C1 N1 -53(10) 3_665
C1 Ta1 C1 N1 32(10) 17_556
Cs1 Ta1 C1 N1 -100(10) .
Cs1 Ta1 C1 N1 80(10) 1_556
C1 Ta1 C1 Cs1 -132.39(6) 18_546
C1 Ta1 C1 Cs1 -47.61(6) 2_655
C1 Ta1 C1 Cs1 95.4(9) 16_656
C1 Ta1 C1 Cs1 47.61(6) 3_665
C1 Ta1 C1 Cs1 132.39(6) 17_556
Cs1 Ta1 C1 Cs1 180.0 1_556
C1 Cs1 C1 N1 -36.1(3) 18_545
C1 Cs1 C1 N1 90(3) 16_655
C1 Cs1 C1 N1 -147.0(3) 2_655
C1 Cs1 C1 N1 33.0(3) 17
C1 Cs1 C1 N1 143.8(3) 3_665
N1 Cs1 C1 N1 -47.22(18) 18_545
N1 Cs1 C1 N1 -134.93(18) 2_655
N1 Cs1 C1 N1 180.0 16_655
N1 Cs1 C1 N1 132.77(18) 3_665
N1 Cs1 C1 N1 45.07(18) 17
C1 Cs1 C1 Ta1 145.406(17) 18_545
C1 Cs1 C1 Ta1 -88(3) 16_655
C1 Cs1 C1 Ta1 34.594(17) 2_655
C1 Cs1 C1 Ta1 -145.399(17) 17
C1 Cs1 C1 Ta1 -34.599(17) 3_665
N1 Cs1 C1 Ta1 134.33(8) 18_545
N1 Cs1 C1 Ta1 46.62(8) 2_655
N1 Cs1 C1 Ta1 1.5(3) 16_655
N1 Cs1 C1 Ta1 -178.4(3) .
N1 Cs1 C1 Ta1 -45.67(8) 3_665
N1 Cs1 C1 Ta1 -133.37(8) 17
C1 N1 C2 C8 -10.5(9) .
Cs1 N1 C2 C8 145.6(2) .
C1 N1 C2 C3 170.2(6) .
Cs1 N1 C2 C3 -33.7(4) .
N1 C2 C3 C5 178.5(3) .
C8 C2 C3 C5 -0.8(5) .
N1 C2 C3 C4 -1.1(5) .
C8 C2 C3 C4 179.6(3) .
C2 C3 C5 C6 -0.4(6) .
C4 C3 C5 C6 179.2(4) .
C3 C5 C6 C7 1.4(6) .
C5 C6 C7 C8 -1.3(6) .
C6 C7 C8 C2 0.2(5) .
C6 C7 C8 C9 -179.0(3) .
N1 C2 C8 C7 -178.4(3) .
C3 C2 C8 C7 0.8(5) .
N1 C2 C8 C9 0.8(5) .
C3 C2 C8 C9 -180.0(3) .
