#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/82/4308258.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_4308258
loop_
_publ_author_name
'Nguyen Hung Huy'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
Rhenium and Technetium Complexes with N,N-Dialkyl-N'-benzoylthioureas
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5310
_journal_page_last               5319
_journal_paper_doi               10.1021/ic070323x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C40 H30 Cl N4 O3 S2 Tc'
_chemical_formula_sum            'C40 H30 Cl N4 O3 S2 Tc'
_chemical_formula_weight         812.25
_chemical_name_common            TcOCl(PhCONCSPh2)2
_chemical_name_systematic
;
 chlorooxobis(N-benzoyl-N',N'-diphenylthioureato-O,S)technetium(V)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.48(1)
_cell_angle_beta                 99.99(1)
_cell_angle_gamma                114.80(1)
_cell_formula_units_Z            2
_cell_length_a                   10.763(1)
_cell_length_b                   11.207(1)
_cell_length_c                   16.926(1)
_cell_measurement_reflns_used    14375
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.21
_cell_volume                     1809.8(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.1540
_diffrn_reflns_av_sigmaI/netI    0.1663
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33030
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.661
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0556P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                5439
_reflns_number_total             9807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070323x-file001_2.cif
_cod_data_source_block           TcOCl(PhCONCSPh2)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1809.9(3)
_cod_database_code               4308258
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
Tc1 Tc 0.59466(5) 0.64849(5) 0.66772(3) 0.02489(12) Uani 1 1 d . . .
O10 O 0.5992(4) 0.5183(4) 0.6223(2) 0.0374(9) Uani 1 1 d . . .
Cl1 Cl 0.51460(15) 0.53056(15) 0.78013(8) 0.0384(3) Uani 1 1 d . . .
S1 S 0.82781(13) 0.76460(15) 0.74066(8) 0.0315(3) Uani 1 1 d . . .
C2 C 0.8033(5) 0.7850(6) 0.8397(3) 0.0316(12) Uani 1 1 d . . .
N3 N 0.7272(5) 0.8425(5) 0.8612(3) 0.0330(10) Uani 1 1 d . . .
C4 C 0.6299(5) 0.8607(5) 0.8083(3) 0.0304(11) Uani 1 1 d . . .
O5 O 0.5717(4) 0.7998(4) 0.7375(2) 0.0291(8) Uani 1 1 d . . .
C31 C 0.5839(6) 0.9581(6) 0.8385(3) 0.0362(13) Uani 1 1 d . . .
C32 C 0.4848(6) 0.9843(6) 0.7876(4) 0.0403(14) Uani 1 1 d . . .
H32 H 0.4479 0.9404 0.7351 0.048 Uiso 1 1 calc R . .
C33 C 0.4407(8) 1.0758(7) 0.8146(4) 0.0540(18) Uani 1 1 d . . .
H33 H 0.3745 1.0931 0.7803 0.065 Uiso 1 1 calc R . .
C34 C 0.4941(10) 1.1394(10) 0.8908(5) 0.083(3) Uani 1 1 d . . .
H34 H 0.4629 1.1993 0.9091 0.100 Uiso 1 1 calc R . .
C35 C 0.5950(11) 1.1165(11) 0.9424(5) 0.105(4) Uani 1 1 d . . .
H35 H 0.6336 1.1628 0.9942 0.126 Uiso 1 1 calc R . .
C36 C 0.6373(8) 1.0241(9) 0.9156(4) 0.073(3) Uani 1 1 d . . .
H36 H 0.7028 1.0065 0.9503 0.087 Uiso 1 1 calc R . .
N6 N 0.8778(4) 0.7512(5) 0.9004(3) 0.0322(10) Uani 1 1 d . . .
C41 C 0.8489(6) 0.7530(6) 0.9815(3) 0.0347(13) Uani 1 1 d . . .
C42 C 0.9462(7) 0.8444(6) 1.0429(4) 0.0416(14) Uani 1 1 d . . .
H42 H 1.0308 0.9065 1.0337 0.050 Uiso 1 1 calc R . .
C43 C 0.9161(8) 0.8425(8) 1.1200(4) 0.0544(19) Uani 1 1 d . . .
H43 H 0.9796 0.9062 1.1623 0.065 Uiso 1 1 calc R . .
C44 C 0.7951(8) 0.7487(8) 1.1335(4) 0.057(2) Uani 1 1 d . . .
H44 H 0.7767 0.7473 1.1852 0.069 Uiso 1 1 calc R . .
C45 C 0.6997(8) 0.6559(8) 1.0718(4) 0.0552(18) Uani 1 1 d . . .
H45 H 0.6175 0.5908 1.0818 0.066 Uiso 1 1 calc R . .
C46 C 0.7252(7) 0.6589(7) 0.9943(4) 0.0467(16) Uani 1 1 d . . .
H46 H 0.6593 0.5979 0.9516 0.056 Uiso 1 1 calc R . .
C51 C 0.9810(5) 0.7042(6) 0.8883(3) 0.0327(12) Uani 1 1 d . . .
C52 C 0.9613(6) 0.5799(7) 0.9077(3) 0.0414(14) Uani 1 1 d . . .
H52 H 0.8829 0.5273 0.9272 0.050 Uiso 1 1 calc R . .
C53 C 1.0610(7) 0.5343(7) 0.8977(4) 0.0496(17) Uani 1 1 d . . .
H53 H 1.0481 0.4502 0.9095 0.060 Uiso 1 1 calc R . .
C54 C 1.1767(7) 0.6128(8) 0.8708(4) 0.0518(18) Uani 1 1 d . . .
H54 H 1.2427 0.5820 0.8643 0.062 Uiso 1 1 calc R . .
C55 C 1.1971(7) 0.7376(8) 0.8529(4) 0.0555(19) Uani 1 1 d . . .
H55 H 1.2765 0.7907 0.8344 0.067 Uiso 1 1 calc R . .
C56 C 1.0985(6) 0.7841(7) 0.8626(4) 0.0425(14) Uani 1 1 d . . .
H56 H 1.1126 0.8689 0.8517 0.051 Uiso 1 1 calc R . .
S11 S 0.66735(13) 0.79895(15) 0.57617(8) 0.0311(3) Uani 1 1 d . . .
C12 C 0.5148(5) 0.7729(5) 0.5067(3) 0.0285(11) Uani 1 1 d . . .
N13 N 0.3862(4) 0.7330(5) 0.5205(3) 0.0315(10) Uani 1 1 d . . .
C14 C 0.3349(5) 0.6636(5) 0.5771(3) 0.0267(11) Uani 1 1 d . . .
O15 O 0.3887(4) 0.6043(4) 0.6254(2) 0.0321(8) Uani 1 1 d . . .
C61 C 0.1929(5) 0.6434(6) 0.5845(3) 0.0327(12) Uani 1 1 d . . .
C62 C 0.1382(6) 0.5866(6) 0.6498(4) 0.0424(14) Uani 1 1 d . . .
H62 H 0.1934 0.5652 0.6899 0.051 Uiso 1 1 calc R . .
C63 C 0.0047(7) 0.5619(8) 0.6559(4) 0.0551(18) Uani 1 1 d . . .
H63 H -0.0304 0.5250 0.7000 0.066 Uiso 1 1 calc R . .
C64 C -0.0763(6) 0.5924(7) 0.5963(5) 0.0553(19) Uani 1 1 d . . .
H64 H -0.1674 0.5747 0.6000 0.066 Uiso 1 1 calc R . .
C65 C -0.0272(6) 0.6473(7) 0.5321(4) 0.0492(17) Uani 1 1 d . . .
H65 H -0.0844 0.6674 0.4925 0.059 Uiso 1 1 calc R . .
C66 C 0.1084(5) 0.6742(6) 0.5250(4) 0.0364(13) Uani 1 1 d . . .
H66 H 0.1424 0.7123 0.4809 0.044 Uiso 1 1 calc R . .
N16 N 0.5325(4) 0.8095(4) 0.4328(2) 0.0279(9) Uani 1 1 d . . .
C71 C 0.4126(5) 0.7990(6) 0.3718(3) 0.0315(12) Uani 1 1 d . . .
C72 C 0.3469(6) 0.8781(6) 0.3830(4) 0.0423(14) Uani 1 1 d . . .
H72 H 0.3766 0.9377 0.4299 0.051 Uiso 1 1 calc R . .
C73 C 0.2360(6) 0.8683(7) 0.3236(4) 0.0521(18) Uani 1 1 d . . .
H73 H 0.1911 0.9217 0.3310 0.063 Uiso 1 1 calc R . .
C74 C 0.1919(7) 0.7826(7) 0.2551(5) 0.062(2) Uani 1 1 d . . .
H74 H 0.1157 0.7753 0.2162 0.074 Uiso 1 1 calc R . .
C75 C 0.2613(7) 0.7054(7) 0.2435(4) 0.0569(19) Uani 1 1 d . . .
H75 H 0.2330 0.6476 0.1959 0.068 Uiso 1 1 calc R . .
C76 C 0.3731(6) 0.7140(6) 0.3025(4) 0.0391(14) Uani 1 1 d . . .
H76 H 0.4200 0.6625 0.2949 0.047 Uiso 1 1 calc R . .
C81 C 0.6652(5) 0.8527(5) 0.4087(3) 0.0281(11) Uani 1 1 d . . .
C82 C 0.7137(6) 0.7626(6) 0.3881(3) 0.0329(12) Uani 1 1 d . . .
H82 H 0.6640 0.6734 0.3927 0.039 Uiso 1 1 calc R . .
C83 C 0.8376(6) 0.8061(7) 0.3605(4) 0.0430(15) Uani 1 1 d . . .
H83 H 0.8723 0.7465 0.3468 0.052 Uiso 1 1 calc R . .
C84 C 0.9079(7) 0.9375(7) 0.3535(4) 0.0513(17) Uani 1 1 d . . .
H84 H 0.9920 0.9670 0.3361 0.062 Uiso 1 1 calc R . .
C85 C 0.8575(7) 1.0268(7) 0.3714(4) 0.0521(17) Uani 1 1 d . . .
H85 H 0.9050 1.1154 0.3645 0.063 Uiso 1 1 calc R . .
C86 C 0.7341(6) 0.9828(6) 0.4001(4) 0.0428(14) Uani 1 1 d . . .
H86 H 0.6989 1.0422 0.4133 0.051 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Tc Tc -1.4390 0.7593 '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
O10 Tc1 O15 99.12(17) . . ?
O10 Tc1 O5 171.95(18) . . ?
O15 Tc1 O5 78.32(14) . . ?
O10 Tc1 S11 100.73(15) . . ?
O15 Tc1 S11 92.52(11) . . ?
O5 Tc1 S11 87.05(10) . . ?
O10 Tc1 S1 101.49(14) . . ?
O15 Tc1 S1 159.38(11) . . ?
O5 Tc1 S1 81.18(10) . . ?
S11 Tc1 S1 84.27(5) . . ?
O10 Tc1 Cl1 91.89(15) . . ?
O15 Tc1 Cl1 85.18(11) . . ?
O5 Tc1 Cl1 80.33(10) . . ?
S11 Tc1 Cl1 167.38(5) . . ?
S1 Tc1 Cl1 93.51(5) . . ?
C2 S1 Tc1 101.52(18) . . ?
N3 C2 N6 116.6(5) . . ?
N3 C2 S1 124.7(4) . . ?
N6 C2 S1 118.4(4) . . ?
C2 N3 C4 123.4(5) . . ?
O5 C4 N3 126.4(5) . . ?
O5 C4 C31 118.0(4) . . ?
N3 C4 C31 115.6(5) . . ?
C4 O5 Tc1 132.7(3) . . ?
C36 C31 C32 119.0(6) . . ?
C36 C31 C4 121.6(5) . . ?
C32 C31 C4 119.4(5) . . ?
C31 C32 C33 120.3(6) . . ?
C34 C33 C32 119.9(6) . . ?
C33 C34 C35 120.8(7) . . ?
C36 C35 C34 119.1(7) . . ?
C31 C36 C35 120.9(7) . . ?
C2 N6 C51 123.3(4) . . ?
C2 N6 C41 119.7(4) . . ?
C51 N6 C41 116.9(4) . . ?
C42 C41 C46 121.6(6) . . ?
C42 C41 N6 119.8(6) . . ?
C46 C41 N6 118.6(5) . . ?
C41 C42 C43 118.5(7) . . ?
C44 C43 C42 120.3(7) . . ?
C43 C44 C45 120.6(7) . . ?
C44 C45 C46 120.0(7) . . ?
C41 C46 C45 119.0(7) . . ?
C56 C51 C52 120.8(5) . . ?
C56 C51 N6 120.6(5) . . ?
C52 C51 N6 118.4(5) . . ?
C51 C52 C53 119.1(6) . . ?
C54 C53 C52 120.1(6) . . ?
C53 C54 C55 120.6(6) . . ?
C54 C55 C56 119.8(7) . . ?
C51 C56 C55 119.5(6) . . ?
C12 S11 Tc1 105.51(19) . . ?
N13 C12 N16 116.5(4) . . ?
N13 C12 S11 127.4(4) . . ?
N16 C12 S11 115.8(4) . . ?
C14 N13 C12 127.5(4) . . ?
O15 C14 N13 128.7(5) . . ?
O15 C14 C61 114.5(5) . . ?
N13 C14 C61 116.7(4) . . ?
C14 O15 Tc1 129.1(3) . . ?
C66 C61 C62 118.5(5) . . ?
C66 C61 C14 121.1(5) . . ?
C62 C61 C14 120.3(5) . . ?
C63 C62 C61 121.2(6) . . ?
C64 C63 C62 119.0(7) . . ?
C65 C64 C63 121.6(6) . . ?
C64 C65 C66 120.3(6) . . ?
C65 C66 C61 119.4(6) . . ?
C12 N16 C81 122.7(4) . . ?
C12 N16 C71 120.1(4) . . ?
C81 N16 C71 117.1(4) . . ?
C76 C71 C72 121.2(5) . . ?
C76 C71 N16 118.4(5) . . ?
C72 C71 N16 120.3(5) . . ?
C71 C72 C73 119.1(6) . . ?
C74 C73 C72 121.2(6) . . ?
C73 C74 C75 119.2(6) . . ?
C76 C75 C74 120.4(7) . . ?
C71 C76 C75 118.8(6) . . ?
C86 C81 C82 121.2(5) . . ?
C86 C81 N16 117.9(5) . . ?
C82 C81 N16 120.7(5) . . ?
C81 C82 C83 119.4(5) . . ?
C84 C83 C82 119.2(6) . . ?
C83 C84 C85 121.6(6) . . ?
C84 C85 C86 118.9(6) . . ?
C81 C86 C85 119.8(6) . . ?
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
Tc1 O10 1.642(4) . ?
Tc1 O15 2.043(3) . ?
Tc1 O5 2.147(3) . ?
Tc1 S11 2.3232(15) . ?
Tc1 S1 2.3582(14) . ?
Tc1 Cl1 2.4374(15) . ?
S1 C2 1.762(6) . ?
C2 N3 1.320(7) . ?
C2 N6 1.358(6) . ?
N3 C4 1.346(6) . ?
C4 O5 1.266(6) . ?
C4 C31 1.481(8) . ?
C31 C36 1.371(9) . ?
C31 C32 1.390(7) . ?
C32 C33 1.389(8) . ?
C33 C34 1.350(10) . ?
C34 C35 1.390(11) . ?
C35 C36 1.383(10) . ?
N6 C51 1.454(6) . ?
N6 C41 1.461(7) . ?
C41 C42 1.362(8) . ?
C41 C46 1.368(9) . ?
C42 C43 1.397(9) . ?
C43 C44 1.353(11) . ?
C44 C45 1.365(11) . ?
C45 C46 1.385(9) . ?
C51 C56 1.365(8) . ?
C51 C52 1.382(8) . ?
C52 C53 1.398(8) . ?
C53 C54 1.359(10) . ?
C54 C55 1.378(10) . ?
C55 C56 1.393(9) . ?
S11 C12 1.750(5) . ?
C12 N13 1.331(7) . ?
C12 N16 1.352(7) . ?
N13 C14 1.311(7) . ?
C14 O15 1.285(6) . ?
C14 C61 1.476(7) . ?
C61 C66 1.391(7) . ?
C61 C62 1.395(8) . ?
C62 C63 1.368(8) . ?
C63 C64 1.368(10) . ?
C64 C65 1.350(10) . ?
C65 C66 1.390(8) . ?
N16 C81 1.443(6) . ?
N16 C71 1.465(6) . ?
C71 C76 1.361(8) . ?
C71 C72 1.371(8) . ?
C72 C73 1.382(8) . ?
C73 C74 1.350(10) . ?
C74 C75 1.387(10) . ?
C75 C76 1.390(8) . ?
C81 C86 1.359(8) . ?
C81 C82 1.374(7) . ?
C82 C83 1.388(8) . ?
C83 C84 1.367(9) . ?
C84 C85 1.368(9) . ?
C85 C86 1.393(9) . ?
