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#$Date: 2016-03-22 12:28:27 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178951 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/80/4118022.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_4118022
loop_
_publ_author_name
'Elisabeth Oehlke'
'Shushu Kong'
'Pawel Arciszewski'
'Swantje Wiebalck'
'Ulrich Abram'
_publ_contact_author_address
;Freie Universität Berlin, Institute of 
Chemistry and Biochemistry, Fabeckstr. 34-36,
 D-14195 Berlin, Germany
;
_publ_contact_author_email       ulrich.abram@fu-berlin.de
_publ_contact_author_fax         '(#49) 30 83852676'
_publ_contact_author_name        'Ulrich Abram'
_publ_contact_author_phone       '(#49) 30 83854002'
_publ_section_title
;
 Aryl and NHC Compounds of Technetium and Rhenium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9118
_journal_page_last               9121
_journal_paper_doi               10.1021/ja3033718
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C28 H48 Cl N9 Tc, Cl'
_chemical_formula_sum            'C28 H48 Cl2 N9 Tc'
_chemical_formula_weight         679.65
_chemical_name_common            '[TcNCl(LMe)4]Cl'
_chemical_name_systematic
;
Tetrakis(1,3,4,5-tetramethylimidazol-2-ylidene)nitridotechnetium(V)
chloride
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.484(1)
_cell_length_b                   13.484(1)
_cell_length_c                   9.799(1)
_cell_measurement_reflns_used    10.956
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.56
_cell_volume                     1781.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30686
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.690
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2326
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.690
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2092
_reflns_number_gt                1296
_reflns_number_total             2326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3033718_si_002_1.cif
_cod_data_source_block           eotctrime
_cod_database_code               4118022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+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
Tc2 Tc 0.0000 0.0000 0.3786(2) 0.0506(7) Uani 0.50 4 d SP
Tc1 Tc 0.0000 0.0000 0.31405(14) 0.0425(5) Uani 0.50 4 d SP
C1 C 0.1146(4) 0.1144(5) 0.3470(6) 0.0563(10) Uani 1 1 d .
N2 N 0.1216(4) 0.2027(4) 0.4247(5) 0.0559(14) Uani 1 1 d .
C3 C 0.2067(5) 0.2525(5) 0.3973(8) 0.0557(14) Uani 1 1 d .
C4 C 0.2560(3) 0.2012(4) 0.3016(7) 0.0486(12) Uani 1 1 d .
N5 N 0.1954(3) 0.1166(3) 0.2730(5) 0.0477(10) Uani 1 1 d .
C6 C 0.0442(5) 0.2329(5) 0.5217(7) 0.0664(17) Uani 1 1 d .
H6A H 0.0602 0.2968 0.5587 0.100 Uiso 1 1 calc R
H6B H 0.0402 0.1852 0.5943 0.100 Uiso 1 1 calc R
H6C H -0.0185 0.2363 0.4755 0.100 Uiso 1 1 calc R
C7 C 0.2247(5) 0.3522(5) 0.4625(8) 0.0671(16) Uani 1 1 d .
H7A H 0.1718 0.3669 0.5249 0.101 Uiso 1 1 calc R
H7B H 0.2273 0.4023 0.3930 0.101 Uiso 1 1 calc R
H7C H 0.2865 0.3509 0.5110 0.101 Uiso 1 1 calc R
C8 C 0.3515(5) 0.2233(6) 0.2336(8) 0.0673(16) Uani 1 1 d .
H8A H 0.3668 0.1715 0.1699 0.101 Uiso 1 1 calc R
H8B H 0.4031 0.2274 0.3009 0.101 Uiso 1 1 calc R
H8C H 0.3466 0.2853 0.1861 0.101 Uiso 1 1 calc R
C9 C 0.2320(5) 0.0462(5) 0.1734(7) 0.0735(19) Uani 1 1 d .
H9A H 0.1867 -0.0085 0.1666 0.110 Uiso 1 1 calc R
H9B H 0.2960 0.0224 0.2013 0.110 Uiso 1 1 calc R
H9C H 0.2376 0.0782 0.0862 0.110 Uiso 1 1 calc R
N10 N 0.0000 0.0000 0.1569(6) 0.0768(13) Uani 0.50 4 d SP
Cl10 Cl 0.0000 0.0000 0.1569(6) 0.0768(13) Uani 0.50 4 d SP
Cl20 Cl 0.0000 0.0000 0.6034(4) 0.0734(12) Uani 0.50 4 d SP
N20 N 0.0000 0.0000 0.6034(4) 0.0734(12) Uani 0.50 4 d SP
Cl1A Cl 0.5000 0.0000 0.3752(8) 0.0324(19) Uani 0.13 2 d SP
Cl1B Cl 0.5000 0.0000 0.4930(18) 0.122(11) Uani 0.13 2 d SP
Cl2A Cl 0.5000 0.0000 0.145(2) 0.080(6) Uani 0.13 2 d SP
Cl2B Cl 0.5000 0.0000 0.2658(14) 0.056(4) Uani 0.13 2 d SP
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'
Cl Cl 0.1484 0.1585 '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'
Tc Tc -1.4390 0.7593 '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'
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
Tc1 Tc2 N10 0.000(1) . .
Tc1 Tc2 Cl20 180.000(1) . .
N10 Tc2 Cl20 180.0 . .
Tc1 Tc2 C1 81.93(18) . .
N10 Tc2 C1 81.93(18) . .
Cl20 Tc2 C1 98.07(18) . .
Tc1 Tc2 C1 81.93(18) . 3
N10 Tc2 C1 81.93(18) . 3
Cl20 Tc2 C1 98.07(18) . 3
C1 Tc2 C1 163.9(4) . 3
Tc1 Tc2 C1 81.93(18) . 2
N10 Tc2 C1 81.93(18) . 2
Cl20 Tc2 C1 98.07(18) . 2
C1 Tc2 C1 88.87(5) . 2
C1 Tc2 C1 88.87(5) 3 2
Tc1 Tc2 C1 81.93(18) . 4
N10 Tc2 C1 81.93(18) . 4
Cl20 Tc2 C1 98.07(18) . 4
C1 Tc2 C1 88.87(5) . 4
C1 Tc2 C1 88.87(5) 3 4
C1 Tc2 C1 163.9(4) 2 4
Tc2 Tc1 N10 180.000(1) . .
Tc2 Tc1 C1 81.60(17) . .
N10 Tc1 C1 98.40(17) . .
Tc2 Tc1 C1 81.60(17) . 2
N10 Tc1 C1 98.40(17) . 2
C1 Tc1 C1 88.78(5) . 2
Tc2 Tc1 C1 81.60(17) . 3
N10 Tc1 C1 98.40(17) . 3
C1 Tc1 C1 163.2(3) . 3
C1 Tc1 C1 88.78(5) 2 3
Tc2 Tc1 C1 81.60(17) . 4
N10 Tc1 C1 98.40(17) . 4
C1 Tc1 C1 88.78(5) . 4
C1 Tc1 C1 163.2(3) 2 4
C1 Tc1 C1 88.78(5) 3 4
Tc2 Tc1 Cl20 0.000(1) . .
N10 Tc1 Cl20 180.0 . .
C1 Tc1 Cl20 81.60(17) . .
C1 Tc1 Cl20 81.60(17) 2 .
C1 Tc1 Cl20 81.60(17) 3 .
C1 Tc1 Cl20 81.60(17) 4 .
N5 C1 N2 102.9(3) . .
N5 C1 Tc2 132.6(5) . .
N2 C1 Tc2 124.0(4) . .
N5 C1 Tc1 121.2(4) . .
N2 C1 Tc1 135.5(4) . .
Tc2 C1 Tc1 16.47(6) . .
C3 N2 C1 111.5(5) . .
C3 N2 C6 126.3(5) . .
C1 N2 C6 122.2(4) . .
C4 C3 N2 107.6(5) . .
C4 C3 C7 132.5(6) . .
N2 C3 C7 119.6(6) . .
C3 C4 N5 105.3(5) . .
C3 C4 C8 129.9(6) . .
N5 C4 C8 124.7(5) . .
C1 N5 C4 112.7(4) . .
C1 N5 C9 130.0(5) . .
C4 N5 C9 117.3(5) . .
N2 C6 H6A 109.5 . .
N2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C3 C7 H7A 109.5 . .
C3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C3 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N5 C9 H9A 109.5 . .
N5 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N5 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
Tc1 N10 Tc2 0.0 . .
Tc2 Cl20 Tc1 0.0 . .
Cl2B Cl1A Cl1B 180.000(3) . .
Cl2B Cl1A Cl2A 0.000(2) . .
Cl1B Cl1A Cl2A 180.000(4) . .
Cl1A Cl1B Cl2A 180.000(5) . 6
Cl1A Cl1B Cl2B 0.000(1) . .
Cl2A Cl1B Cl2B 180.000(3) 6 .
Cl2B Cl2A Cl1B 180.000(1) . 6_554
Cl2B Cl2A Cl1A 0.000(1) . .
Cl1B Cl2A Cl1A 180.0 6_554 .
Cl1A Cl2B Cl2A 180.000(3) . .
Cl1A Cl2B Cl1B 0.000(1) . .
Cl2A Cl2B Cl1B 180.000(1) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc2 Tc1 0.632(2) .
Tc2 N10 2.172(7) .
Tc2 Cl20 2.203(5) .
Tc2 C1 2.205(4) .
Tc2 C1 2.205(4) 3
Tc2 C1 2.205(4) 2
Tc2 C1 2.205(4) 4
Tc1 N10 1.540(6) .
Tc1 C1 2.207(4) .
Tc1 C1 2.207(4) 2
Tc1 C1 2.207(4) 3
Tc1 C1 2.207(4) 4
Tc1 Cl20 2.835(5) .
C1 N5 1.309(7) .
C1 N2 1.417(8) .
N2 C3 1.356(8) .
N2 C6 1.470(8) .
C3 C4 1.342(6) .
C3 C7 1.509(9) .
C4 N5 1.431(6) .
C4 C8 1.480(8) .
N5 C9 1.448(7) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
Cl1A Cl2B 1.071(19) .
Cl1A Cl1B 1.15(2) .
Cl1A Cl2A 2.26(2) .
Cl1B Cl2A 1.49(3) 6
Cl1B Cl2B 2.226(19) .
Cl2A Cl2B 1.19(3) .
Cl2A Cl1B 1.49(3) 6_554
