#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:23:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179325 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/22/4322275.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_4322275
loop_
_publ_author_name
'Cristina Bolzati'
'Alessandra Boschi'
'Licia Uccelli'
'Erica Malagò'
'Giuliano Bandoli'
'Francesco Tisato'
'Fiorenzo Refosco'
'Roberto Pasqualini'
'Adriano Duatti'
_publ_section_title
;
 Synthesis of a Novel Class of trigonal Bipyramidal Nitrido Tc(V)
 Complexes with Phosphino-Thiol Ligands. Crystal Structure of
 [99gTc(N)(L1)2] [L1= 2-(Diphenylphosphino)ethanethiolato] and
 [99gTc(N)(L5)2] [L5= 2-(Ditolylphosphino)propanethiolato]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4473
_journal_page_last               4479
_journal_paper_doi               10.1021/ic9903477
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H28 N P2 S2 Tc'
_chemical_formula_weight         602.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.06(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.837(16)
_cell_length_b                   7.327(6)
_cell_length_c                   31.521(20)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      7.8
_cell_volume                     5353(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet Siemens R3m/V'
_diffrn_measurement_method       omega-2theta
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            4787
_diffrn_reflns_theta_max         20.05
_diffrn_reflns_theta_min         2.60
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00000(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         2511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_obs          0.0572
_refine_ls_shift/esd_max         -3.924
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0674P)²+119.4638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1532
_refine_ls_wR_factor_obs         0.1404
_reflns_number_observed          2057
_reflns_number_total             2513
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9903477_1.cif
_cod_data_source_block           1_IC9903477_March30,1999
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+119.4638P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+119.4638P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5353.1(65)
_cod_database_code               4322275
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tc Tc 0.69330(4) 0.17691(13) 0.60876(3) 0.0378(5) Uani 1 d . .
S1 S 0.74768(13) 0.3041(5) 0.67938(11) 0.0577(10) Uani 1 d . .
S2 S 0.66040(12) -0.1181(4) 0.58261(11) 0.0439(9) Uani 1 d . .
P1 P 0.61368(12) 0.2284(4) 0.63417(10) 0.0399(9) Uani 1 d . .
P2 P 0.77962(11) 0.0719(4) 0.59905(9) 0.0298(8) Uani 1 d . .
N1 N 0.6748(4) 0.3283(12) 0.5678(3) 0.046(3) Uani 1 d . .
C1 C 0.6384(5) 0.4162(18) 0.6749(4) 0.056(4) Uani 1 d . .
H1A H 0.6121(5) 0.4332(18) 0.6907(4) 0.067 Uiso 1 d R .
H1B H 0.6389(5) 0.5263(18) 0.6585(4) 0.067 Uiso 1 d R .
C2 C 0.6987(5) 0.3795(21) 0.7073(5) 0.069(4) Uani 1 d . .
H2A H 0.7140(5) 0.4878(21) 0.7246(5) 0.083 Uiso 1 d R .
H2B H 0.6964(5) 0.2865(21) 0.7281(5) 0.083 Uiso 1 d R .
C3 C 0.7564(4) -0.0994(15) 0.5548(4) 0.036(3) Uani 1 d . .
H3A H 0.7894(4) -0.1642(15) 0.5537(4) 0.044 Uiso 1 d R .
H3B H 0.7379(4) -0.0409(15) 0.5259(4) 0.044 Uiso 1 d R .
C4 C 0.7148(5) -0.2312(16) 0.5630(4) 0.047(3) Uani 1 d . .
H4A H 0.6951(5) -0.2986(16) 0.5357(4) 0.057 Uiso 1 d R .
H4B H 0.7364(5) -0.3166(16) 0.5858(4) 0.057 Uiso 1 d R .
C1A C 0.5910(5) 0.0535(16) 0.6651(4) 0.041(3) Uani 1 d . .
C2A C 0.6326(5) -0.0570(17) 0.6954(4) 0.049(3) Uani 1 d . .
H2AA H 0.6724(5) -0.0462(17) 0.6986(4) 0.059 Uiso 1 d R .
C3A C 0.6154(7) -0.1820(18) 0.7217(4) 0.057(4) Uani 1 d . .
H3AA H 0.6442(7) -0.2561(18) 0.7433(4) 0.069 Uiso 1 d R .
C4A C 0.5591(7) -0.2035(19) 0.7165(5) 0.067(4) Uani 1 d . .
H4AA H 0.5487(7) -0.2907(19) 0.7349(5) 0.081 Uiso 1 d R .
C5A C 0.5173(6) -0.0967(20) 0.6845(5) 0.063(4) Uani 1 d . .
H5AA H 0.4774(6) -0.1126(20) 0.6806(5) 0.076 Uiso 1 d R .
C6A C 0.5342(5) 0.0298(18) 0.6595(4) 0.054(3) Uani 1 d . .
H6AA H 0.5053(5) 0.1032(18) 0.6377(4) 0.064 Uiso 1 d R .
C1B C 0.5478(5) 0.3080(18) 0.5905(4) 0.046(3) Uani 1 d . .
C2B C 0.5274(5) 0.2174(19) 0.5494(5) 0.055(4) Uani 1 d . .
H2BA H 0.5476(5) 0.1126(19) 0.5445(5) 0.066 Uiso 1 d R .
C3B C 0.4771(7) 0.2799(25) 0.5164(5) 0.075(5) Uani 1 d . .
H3BA H 0.4624(7) 0.2191(25) 0.4875(5) 0.089 Uiso 1 d R .
C4B C 0.4479(6) 0.4246(29) 0.5231(7) 0.084(6) Uani 1 d . .
H4BA H 0.4133(6) 0.4650(29) 0.4995(7) 0.101 Uiso 1 d R .
C5B C 0.4677(7) 0.5104(28) 0.5629(7) 0.090(6) Uani 1 d . .
H5BA H 0.4460(7) 0.6131(28) 0.5669(7) 0.108 Uiso 1 d R .
C6B C 0.5167(6) 0.4552(22) 0.5965(5) 0.069(4) Uani 1 d . .
H6BA H 0.5296(6) 0.5200(22) 0.6249(5) 0.083 Uiso 1 d R .
C1C C 0.8190(4) 0.2460(15) 0.5818(4) 0.036(3) Uani 1 d . .
C2C C 0.8315(4) 0.2372(17) 0.5418(4) 0.039(3) Uani 1 d . .
H2CA H 0.8180(4) 0.1356(17) 0.5215(4) 0.047 Uiso 1 d R .
C3C C 0.8634(5) 0.3749(21) 0.5326(4) 0.051(3) Uani 1 d . .
H3CA H 0.8723(5) 0.3695(21) 0.5054(4) 0.062 Uiso 1 d R .
C4C C 0.8816(5) 0.5182(19) 0.5607(5) 0.052(3) Uani 1 d . .
H4CA H 0.9036(5) 0.6126(19) 0.5534(5) 0.062 Uiso 1 d R .
C5C C 0.8699(5) 0.5293(16) 0.5996(5) 0.053(3) Uani 1 d . .
H5CA H 0.8835(5) 0.6318(16) 0.6196(5) 0.063 Uiso 1 d R .
C6C C 0.8379(5) 0.3939(16) 0.6098(4) 0.045(3) Uani 1 d . .
H6CA H 0.8287(5) 0.4026(16) 0.6368(4) 0.054 Uiso 1 d R .
C1D C 0.8344(4) -0.0415(14) 0.6464(3) 0.028(3) Uani 1 d . .
C2D C 0.8171(5) -0.1724(17) 0.6707(4) 0.050(3) Uani 1 d . .
H2DA H 0.7766(5) -0.1923(17) 0.6633(4) 0.060 Uiso 1 d R .
C3D C 0.8560(7) -0.2702(19) 0.7047(4) 0.061(4) Uani 1 d . .
H3DA H 0.8436(7) -0.3625(19) 0.7208(4) 0.073 Uiso 1 d R .
C4D C 0.9139(7) -0.2379(20) 0.7154(4) 0.066(4) Uani 1 d . .
H4DA H 0.9414(7) -0.3083(20) 0.7391(4) 0.080 Uiso 1 d R .
C5D C 0.9324(5) -0.1070(19) 0.6926(4) 0.062(4) Uani 1 d . .
H5DA H 0.9729(5) -0.0816(19) 0.7020(4) 0.074 Uiso 1 d R .
C6D C 0.8927(4) -0.0115(15) 0.6579(4) 0.041(3) Uani 1 d . .
H6DA H 0.9052(4) 0.0752(15) 0.6405(4) 0.049 Uiso 1 d 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'
P P 0.1023 0.0942 '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'
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
N1 Tc S1 112.5(3) . . ?
N1 Tc S2 112.5(3) . . ?
S1 Tc S2 135.03(13) . . ?
N1 Tc P2 97.3(3) . . ?
S1 Tc P2 90.71(13) . . ?
S2 Tc P2 82.78(11) . . ?
N1 Tc P1 97.2(3) . . ?
S1 Tc P1 83.34(13) . . ?
S2 Tc P1 92.12(11) . . ?
P2 Tc P1 165.54(11) . . ?
C2 S1 Tc 108.8(4) . . ?
C4 S2 Tc 108.8(4) . . ?
C1B P1 C1A 105.3(5) . . ?
C1B P1 C1 105.9(6) . . ?
C1A P1 C1 104.2(6) . . ?
C1B P1 Tc 114.9(4) . . ?
C1A P1 Tc 121.1(4) . . ?
C1 P1 Tc 104.0(4) . . ?
C1C P2 C3 108.3(5) . . ?
C1C P2 C1D 104.1(5) . . ?
C3 P2 C1D 104.7(5) . . ?
C1C P2 Tc 114.7(4) . . ?
C3 P2 Tc 105.6(3) . . ?
C1D P2 Tc 118.8(3) . . ?
C2 C1 P1 110.1(9) . . ?
C1 C2 S1 113.6(9) . . ?
C4 C3 P2 111.1(7) . . ?
C3 C4 S2 113.3(8) . . ?
C6A C1A C2A 119.5(11) . . ?
C6A C1A P1 121.6(9) . . ?
C2A C1A P1 118.9(9) . . ?
C1A C2A C3A 118.6(11) . . ?
C4A C3A C2A 121.6(12) . . ?
C3A C4A C5A 119.3(13) . . ?
C6A C5A C4A 119.3(12) . . ?
C1A C6A C5A 121.6(12) . . ?
C2B C1B C6B 118.0(11) . . ?
C2B C1B P1 119.0(10) . . ?
C6B C1B P1 123.0(11) . . ?
C1B C2B C3B 118.3(14) . . ?
C4B C3B C2B 122.3(16) . . ?
C5B C4B C3B 119.0(16) . . ?
C4B C5B C6B 121.3(17) . . ?
C5B C6B C1B 121.0(15) . . ?
C6C C1C C2C 118.7(11) . . ?
C6C C1C P2 117.5(9) . . ?
C2C C1C P2 123.8(9) . . ?
C3C C2C C1C 119.1(11) . . ?
C4C C3C C2C 121.0(11) . . ?
C3C C4C C5C 120.8(12) . . ?
C4C C5C C6C 119.7(12) . . ?
C1C C6C C5C 120.7(12) . . ?
C6D C1D C2D 118.0(10) . . ?
C6D C1D P2 123.3(8) . . ?
C2D C1D P2 118.6(8) . . ?
C3D C2D C1D 121.7(11) . . ?
C2D C3D C4D 119.2(12) . . ?
C5D C4D C3D 120.6(12) . . ?
C4D C5D C6D 119.6(12) . . ?
C5D C6D C1D 120.9(11) . . ?
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 N1 1.638(9) . ?
Tc S1 2.342(4) . ?
Tc S2 2.353(4) . ?
Tc P2 2.399(3) . ?
Tc P1 2.415(3) . ?
S1 C2 1.826(12) . ?
S2 C4 1.869(11) . ?
P1 C1B 1.814(12) . ?
P1 C1A 1.818(12) . ?
P1 C1 1.830(12) . ?
P2 C1C 1.806(11) . ?
P2 C3 1.811(11) . ?
P2 C1D 1.819(11) . ?
C1 C2 1.50(2) . ?
C3 C4 1.503(15) . ?
C1A C6A 1.37(2) . ?
C1A C2A 1.39(2) . ?
C2A C3A 1.40(2) . ?
C3A C4A 1.36(2) . ?
C4A C5A 1.40(2) . ?
C5A C6A 1.38(2) . ?
C1B C2B 1.38(2) . ?
C1B C6B 1.38(2) . ?
C2B C3B 1.39(2) . ?
C3B C4B 1.34(2) . ?
C4B C5B 1.33(2) . ?
C5B C6B 1.36(2) . ?
C1C C6C 1.37(2) . ?
C1C C2C 1.403(15) . ?
C2C C3C 1.38(2) . ?
C3C C4C 1.34(2) . ?
C4C C5C 1.36(2) . ?
C5C C6C 1.38(2) . ?
C1D C6D 1.377(14) . ?
C1D C2D 1.39(2) . ?
C2D C3D 1.36(2) . ?
C3D C4D 1.37(2) . ?
C4D C5D 1.37(2) . ?
C5D C6D 1.37(2) . ?
