#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:11:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179049 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/11/4301170.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_4301170
loop_
_publ_author_name
'Hung Huy Nguyen'
'Pedro I. da S. Maia'
'Victor M. Deflon'
'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
;
Oxotechnetium(V) Complexes with a Novel Class of Tridentate
Thiosemicarbazide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              25
_journal_page_last               27
_journal_paper_doi               10.1021/ic802044r
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C19 H27 Cl N5 O S2 Tc'
_chemical_formula_sum            'C19 H27 Cl N5 O S2 Tc'
_chemical_formula_weight         539.03
_chemical_name_common            '[TcOCl(Et2NC(S)NC(Ph)NNC(S)N(CH2)6)]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 106.73(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.213(1)
_cell_length_b                   10.906(1)
_cell_length_c                   11.792(1)
_cell_measurement_reflns_used    14835
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.31
_cell_volume                     1134.7(2)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8841
_diffrn_reflns_theta_full        29.26
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.096
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6053
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1138P)²+0.7096P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                5654
_reflns_number_total             6053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802044r_si_001_1.cif
_cod_data_source_block           hntcscl2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4301170
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
Tc Tc 0.82668(4) 0.05599(3) 0.21409(3) 0.02709(12) Uani 1 1 d . . .
O10 O 0.7158(5) 0.0930(4) 0.0819(4) 0.0385(9) Uani 1 1 d . . .
Cl Cl 0.8434(2) 0.22367(14) 0.34347(18) 0.0502(4) Uani 1 1 d . . .
S1 S 1.07093(16) 0.11675(12) 0.23226(13) 0.0345(3) Uani 1 1 d . . .
C2 C 1.1323(6) 0.0101(5) 0.1455(5) 0.0321(10) Uani 1 1 d . A .
N3 N 1.1127(6) -0.1097(4) 0.1506(5) 0.0363(11) Uani 1 1 d . . .
C4 C 1.0130(6) -0.1684(4) 0.1921(5) 0.0277(9) Uani 1 1 d . . .
N5 N 0.8815(5) -0.1228(4) 0.2054(4) 0.0286(8) Uani 1 1 d . . .
C31 C 1.0501(6) -0.3006(4) 0.2186(5) 0.0293(10) Uani 1 1 d . . .
C32 C 1.0486(7) -0.3538(6) 0.3236(6) 0.0370(12) Uani 1 1 d . . .
H32 H 1.0147 -0.3097 0.3785 0.044 Uiso 1 1 calc R . .
C33 C 1.0981(8) -0.4744(6) 0.3478(6) 0.0468(16) Uani 1 1 d . . .
H33 H 1.0960 -0.5105 0.4187 0.056 Uiso 1 1 calc R . .
C34 C 1.1492(8) -0.5397(6) 0.2690(7) 0.0487(17) Uani 1 1 d . . .
H34 H 1.1801 -0.6205 0.2854 0.058 Uiso 1 1 calc R . .
C35 C 1.1552(7) -0.4858(5) 0.1647(7) 0.0400(13) Uani 1 1 d . . .
H35 H 1.1910 -0.5304 0.1112 0.048 Uiso 1 1 calc R . .
C36 C 1.1083(6) -0.3657(5) 0.1389(6) 0.0338(11) Uani 1 1 d . . .
H36 H 1.1153 -0.3288 0.0696 0.041 Uiso 1 1 calc R . .
N6 N 1.2137(9) 0.0507(6) 0.0756(7) 0.066(2) Uani 1 1 d . . .
C41 C 1.2476(8) 0.1793(5) 0.0637(6) 0.0408(13) Uani 1 1 d . A .
H41A H 1.1626 0.2283 0.0704 0.049 Uiso 1 1 calc R . .
H41B H 1.2588 0.1928 -0.0147 0.049 Uiso 1 1 calc R . .
C42 C 1.3895(8) 0.2224(9) 0.1550(9) 0.0566(19) Uani 1 1 d . . .
H42A H 1.4060 0.3075 0.1423 0.085 Uiso 1 1 calc R A .
H42B H 1.4746 0.1754 0.1479 0.085 Uiso 1 1 calc R . .
H42C H 1.3782 0.2116 0.2328 0.085 Uiso 1 1 calc R . .
C43 C 1.2224(12) -0.0351(12) -0.0314(10) 0.032(3) Uani 0.56(2) 1 d P A 1
H43A H 1.1411 -0.0950 -0.0496 0.039 Uiso 0.56(2) 1 calc PR A 1
H43B H 1.2168 0.0129 -0.1018 0.039 Uiso 0.56(2) 1 calc PR A 1
C44 C 1.3724(13) -0.0958(12) 0.0133(13) 0.046(4) Uani 0.56(2) 1 d P A 1
H44A H 1.3877 -0.1503 -0.0462 0.069 Uiso 0.56(2) 1 calc PR A 1
H44B H 1.3757 -0.1416 0.0835 0.069 Uiso 0.56(2) 1 calc PR A 1
H44C H 1.4508 -0.0347 0.0315 0.069 Uiso 0.56(2) 1 calc PR A 1
C43A C 1.3287(13) -0.0391(11) 0.0498(12) 0.030(3) Uani 0.44(2) 1 d P A 2
H43C H 1.4198 0.0025 0.0448 0.036 Uiso 0.44(2) 1 calc PR A 2
H43D H 1.3557 -0.1039 0.1085 0.036 Uiso 0.44(2) 1 calc PR A 2
C44A C 1.2356(16) -0.0870(15) -0.0696(15) 0.038(3) Uani 0.44(2) 1 d P A 2
H44D H 1.2941 -0.1458 -0.0983 0.056 Uiso 0.44(2) 1 calc PR A 2
H44E H 1.2085 -0.0201 -0.1246 0.056 Uiso 0.44(2) 1 calc PR A 2
H44F H 1.1453 -0.1254 -0.0616 0.056 Uiso 0.44(2) 1 calc PR A 2
N7 N 0.7797(5) -0.2156(4) 0.2181(4) 0.0272(8) Uani 1 1 d . . .
C8 C 0.6838(6) -0.1790(5) 0.2713(4) 0.0266(9) Uani 1 1 d . . .
S9 S 0.68830(16) -0.02775(12) 0.32671(13) 0.0316(3) Uani 1 1 d . . .
N51 N 0.5723(5) -0.2548(4) 0.2825(4) 0.0290(8) Uani 1 1 d . . .
C52 C 0.5640(7) -0.3791(6) 0.2374(5) 0.0384(12) Uani 1 1 d . . .
H52A H 0.5896 -0.3781 0.1632 0.046 Uiso 1 1 calc R . .
H52B H 0.4602 -0.4076 0.2207 0.046 Uiso 1 1 calc R . .
C53 C 0.6670(9) -0.4699(6) 0.3202(7) 0.0475(15) Uani 1 1 d . . .
H53A H 0.7619 -0.4740 0.3002 0.057 Uiso 1 1 calc R . .
H53B H 0.6204 -0.5504 0.3057 0.057 Uiso 1 1 calc R . .
C54 C 0.7026(9) -0.4420(10) 0.4527(7) 0.0579(16) Uani 1 1 d . . .
H54A H 0.7777 -0.3771 0.4715 0.069 Uiso 1 1 calc R . .
H54B H 0.7491 -0.5143 0.4959 0.069 Uiso 1 1 calc R . .
C55 C 0.5705(10) -0.4038(7) 0.4996(7) 0.0513(16) Uani 1 1 d . . .
H55A H 0.4814 -0.4510 0.4591 0.062 Uiso 1 1 calc R . .
H55B H 0.5957 -0.4233 0.5833 0.062 Uiso 1 1 calc R . .
C56 C 0.5328(9) -0.2676(7) 0.4830(6) 0.0446(14) Uani 1 1 d . . .
H56A H 0.4581 -0.2483 0.5238 0.053 Uiso 1 1 calc R . .
H56B H 0.6236 -0.2211 0.5207 0.053 Uiso 1 1 calc R . .
C57 C 0.4725(6) -0.2250(6) 0.3556(6) 0.0355(11) Uani 1 1 d . . .
H57A H 0.3743 -0.2624 0.3206 0.043 Uiso 1 1 calc R . .
H57B H 0.4580 -0.1369 0.3548 0.043 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 Tc N5 106.5(2) . . ?
O10 Tc S9 110.52(16) . . ?
N5 Tc S9 80.39(13) . . ?
O10 Tc S1 109.96(16) . . ?
N5 Tc S1 91.76(14) . . ?
S9 Tc S1 139.35(6) . . ?
O10 Tc Cl 109.22(17) . . ?
N5 Tc Cl 144.00(14) . . ?
S9 Tc Cl 82.94(5) . . ?
S1 Tc Cl 80.56(6) . . ?
C2 S1 Tc 103.1(2) . . ?
N3 C2 N6 117.5(5) . . ?
N3 C2 S1 124.1(4) . . ?
N6 C2 S1 118.2(5) . . ?
C2 N3 C4 127.7(5) . . ?
N3 C4 N5 127.0(5) . . ?
N3 C4 C31 113.7(4) . . ?
N5 C4 C31 119.1(4) . . ?
C4 N5 N7 112.9(4) . . ?
C4 N5 Tc 127.0(4) . . ?
N7 N5 Tc 120.0(3) . . ?
C32 C31 C36 119.7(5) . . ?
C32 C31 C4 122.5(5) . . ?
C36 C31 C4 117.2(5) . . ?
C31 C32 C33 119.8(6) . . ?
C34 C33 C32 120.8(6) . . ?
C33 C34 C35 119.8(6) . . ?
C34 C35 C36 120.6(6) . . ?
C35 C36 C31 119.1(6) . . ?
C2 N6 C41 123.6(6) . . ?
C2 N6 C43A 116.9(7) . . ?
C41 N6 C43A 114.6(7) . . ?
C2 N6 C43 117.3(7) . . ?
C41 N6 C43 115.4(6) . . ?
C43A N6 C43 43.4(7) . . ?
N6 C41 C42 113.4(6) . . ?
C44 C43 N6 103.6(10) . . ?
C44A C43A N6 99.5(10) . . ?
C8 N7 N5 113.5(4) . . ?
N7 C8 N51 120.4(5) . . ?
N7 C8 S9 121.5(4) . . ?
N51 C8 S9 118.0(4) . . ?
C8 S9 Tc 96.65(17) . . ?
C8 N51 C52 119.7(5) . . ?
C8 N51 C57 122.9(5) . . ?
C52 N51 C57 116.5(4) . . ?
N51 C52 C53 114.6(5) . . ?
C52 C53 C54 115.9(6) . . ?
C53 C54 C55 117.6(6) . . ?
C56 C55 C54 113.2(6) . . ?
C57 C56 C55 115.5(6) . . ?
N51 C57 C56 113.7(5) . . ?
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
Tc O10 1.650(4) . ?
Tc N5 2.024(4) . ?
Tc S9 2.2798(13) . ?
Tc S1 2.2958(14) . ?
Tc Cl 2.3580(16) . ?
S1 C2 1.747(6) . ?
C2 N3 1.322(7) . ?
C2 N6 1.340(7) . ?
N3 C4 1.324(7) . ?
C4 N5 1.359(7) . ?
C4 C31 1.494(7) . ?
N5 N7 1.417(6) . ?
C31 C32 1.371(8) . ?
C31 C36 1.402(8) . ?
C32 C33 1.393(9) . ?
C33 C34 1.358(12) . ?
C34 C35 1.379(11) . ?
C35 C36 1.385(8) . ?
N6 C41 1.453(8) . ?
N6 C43A 1.536(12) . ?
N6 C43 1.592(16) . ?
C41 C42 1.510(12) . ?
C43 C44 1.485(16) . ?
C43A C44A 1.52(2) . ?
N7 C8 1.285(7) . ?
C8 N51 1.354(7) . ?
C8 S9 1.771(6) . ?
N51 C52 1.451(7) . ?
N51 C57 1.466(6) . ?
C52 C53 1.516(10) . ?
C53 C54 1.532(11) . ?
C54 C55 1.533(11) . ?
C55 C56 1.524(11) . ?
C56 C57 1.517(10) . ?
