#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/40/2004045.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2004045
loop_
_publ_author_name
'Abram, U.'
'Abram, S.'
'Dilworth, J. R.'
_publ_section_title
trans-Dichloro(O,O'-diethyldithiophosphato-S,S')bis(dimethylphenylphosphine)technetium(III)
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1983
_journal_page_last               1985
_journal_paper_doi               10.1107/S0108270195005063
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        '[TcNCl₂(Me₂PhP)₃] + NaEt₂dtp'
_chemical_formula_moiety         '[TcCl~2~(Me~2~PhP)~2~dtp]'
_chemical_formula_sum            'C20 H32 Cl2 O2 P3 S2 Tc'
_chemical_formula_weight         631.39
_chemical_name_systematic
;
 Dichloro(O,O'-diethyldithiophosphato-S,S')-
bis(dimethylphenylphosphine)technetium(III)
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.49(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.885(3)
_cell_length_b                   8.983(2)
_cell_length_c                   19.043(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      12.36
_cell_measurement_theta_min      9.38
_cell_volume                     5512.7(15)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software and SDP (Frenz, 1983)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16374
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.9742
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       needle
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         .488
_refine_diff_density_min         -.559
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    'H atoms refined as riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_obs          0.0271
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0342P)^2^ + 4.1514P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0753
_refine_ls_wR_factor_obs         0.0689
_reflns_number_observed          6117
_reflns_number_total             7314
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1169.cif
_cod_data_source_block           tcdtp
_cod_original_cell_volume        5513.0(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2004045
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_occupancy
_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_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Tc 1 0.63620(1) 0.61629(2) 0.44273(1) 0.02830(5) Uani d . Tc
Cl1 1 0.66109(2) 0.40913(6) 0.38848(3) 0.04564(13) Uani d . Cl
Cl2 1 0.60716(2) 0.82962(6) 0.48531(3) 0.03872(11) Uani d . Cl
P1 1 0.66122(2) 0.78359(6) 0.36090(3) 0.03245(11) Uani d . P
P2 1 0.56885(2) 0.56262(6) 0.36685(3) 0.03434(11) Uani d . P
P3 1 0.67971(2) 0.51596(6) 0.59513(3) 0.03963(12) Uani d . P
S1 1 0.70270(2) 0.64716(7) 0.52775(3) 0.04189(12) Uani d . S
S2 1 0.62249(2) 0.46326(7) 0.54382(3) 0.04367(13) Uani d . S
O1 1 0.70765(6) 0.3771(2) 0.62273(8) 0.0529(4) Uani d . O
O2 1 0.68163(6) 0.5867(2) 0.67110(8) 0.0541(4) Uani d . O
C1 1 0.71739(11) 0.2660(3) 0.57296(15) 0.0685(8) Uani d . C
H1A 1 0.69744(11) 0.2724(3) 0.52808(15) 0.082 Uiso calc R H
H1B 1 0.74475(11) 0.2853(3) 0.56319(15) 0.082 Uiso calc R H
C2 1 0.71633(15) 0.1191(4) 0.6027(2) 0.0949(13) Uani d . C
H2A 1 0.72280(15) 0.0470(4) 0.5693(2) 0.142 Uiso calc R H
H2B 1 0.68913(15) 0.0997(4) 0.6117(2) 0.142 Uiso calc R H
H2C 1 0.73635(15) 0.1126(4) 0.6468(2) 0.142 Uiso calc R H
C3 1 0.66055(10) 0.7269(4) 0.6783(2) 0.0677(8) Uani d . C
H3A 1 0.63461(10) 0.7079(4) 0.6936(2) 0.081 Uiso calc R H
H3B 1 0.65434(10) 0.7776(4) 0.6324(2) 0.081 Uiso calc R H
C4 1 0.68739(11) 0.8203(4) 0.7312(2) 0.0764(9) Uani d . C
H4A 1 0.67366(11) 0.9129(4) 0.7361(2) 0.115 Uiso calc R H
H4B 1 0.71290(11) 0.8394(4) 0.7155(2) 0.115 Uiso calc R H
H4C 1 0.69324(11) 0.7700(4) 0.7765(2) 0.115 Uiso calc R H
C11 1 0.62524(6) 0.8605(2) 0.28477(11) 0.0378(4) Uani d . C
C12 1 0.59969(7) 0.9784(3) 0.29498(15) 0.0495(6) Uani d . C
H12 1 0.60174(7) 1.0197(3) 0.34033(15) 0.059 Uiso calc R H
C13 1 0.57113(10) 1.0345(3) 0.2375(2) 0.0732(9) Uani d . C
H13 1 0.55406(10) 1.1134(3) 0.2445(2) 0.088 Uiso calc R H
C14 1 0.56799(12) 0.9741(5) 0.1708(2) 0.0940(13) Uani d . C
H14 1 0.54872(12) 1.0122(5) 0.1325(2) 0.113 Uiso calc R H
C15 1 0.59304(13) 0.8578(4) 0.1597(2) 0.0858(11) Uani d . C
H15 1 0.59071(13) 0.8174(4) 0.1141(2) 0.103 Uiso calc R H
C16 1 0.62170(9) 0.8010(3) 0.21632(13) 0.0554(6) Uani d . C
H16 1 0.63875(9) 0.7226(3) 0.20866(13) 0.066 Uiso calc R H
C17 1 0.68517(7) 0.9498(3) 0.40579(13) 0.0473(5) Uani d . C
H17A 1 0.70513(7) 0.9216(3) 0.44763(13) 0.071 Uiso calc R H
H17B 1 0.66421(7) 1.0113(3) 0.41964(13) 0.071 Uiso calc R H
H17C 1 0.69881(7) 1.0043(3) 0.37377(13) 0.071 Uiso calc R H
C18 1 0.70283(7) 0.7063(3) 0.32228(14) 0.0535(6) Uani d . C
H18A 1 0.72341(7) 0.6629(3) 0.35951(14) 0.080 Uiso calc R H
H18B 1 0.71526(7) 0.7840(3) 0.29904(14) 0.080 Uiso calc R H
H18C 1 0.69183(7) 0.6312(3) 0.28786(14) 0.080 Uiso calc R H
C21 1 0.53961(6) 0.4185(2) 0.40235(11) 0.0349(4) Uani d . C
C22 1 0.49933(7) 0.4396(3) 0.41263(12) 0.0414(5) Uani d . C
H22 1 0.48594(7) 0.5297(3) 0.39990(12) 0.050 Uiso calc R H
C23 1 0.47906(7) 0.3274(3) 0.44172(13) 0.0476(5) Uani d . C
H23 1 0.45204(7) 0.3423(3) 0.44808(13) 0.057 Uiso calc R H
C24 1 0.49854(8) 0.1938(3) 0.46131(13) 0.0477(5) Uani d . C
H24 1 0.48499(8) 0.1197(3) 0.48191(13) 0.057 Uiso calc R H
C25 1 0.53814(8) 0.1703(3) 0.45030(14) 0.0499(6) Uani d . C
H25 1 0.55111(8) 0.0793(3) 0.46254(14) 0.060 Uiso calc R H
C26 1 0.55869(7) 0.2809(3) 0.42123(13) 0.0447(5) Uani d . C
H26 1 0.58547(7) 0.2640(3) 0.41407(13) 0.054 Uiso calc R H
C27 1 0.53271(7) 0.7176(3) 0.34885(14) 0.0503(6) Uani d . C
H27A 1 0.54579(7) 0.7995(3) 0.32973(14) 0.075 Uiso calc R H
H27B 1 0.52474(7) 0.7477(3) 0.39256(14) 0.075 Uiso calc R H
H27C 1 0.50854(7) 0.6874(3) 0.31476(14) 0.075 Uiso calc R H
C28 1 0.56974(8) 0.4888(3) 0.27797(12) 0.0531(6) Uani d . C
H28A 1 0.58830(8) 0.4053(3) 0.28222(12) 0.080 Uiso calc R H
H28B 1 0.57908(8) 0.5647(3) 0.24941(12) 0.080 Uiso calc R H
H28C 1 0.54233(8) 0.4574(3) 0.25548(12) 0.080 Uiso calc R H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0033 .0016
Cl Cl 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1484 .1585
Tc Tc 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -1.4390 .7593
S S 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1246 .1234
P P 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1023 .0942
O O 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0106 .0060
H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl1 Tc Cl2 174.09(2) yes
Cl1 Tc P1 90.91(2) yes
Cl2 Tc P1 85.97(2) yes
Cl1 Tc P2 86.43(2) yes
Cl2 Tc P2 88.98(2) yes
P1 Tc P2 97.24(2) yes
Cl1 Tc S1 92.10(2) yes
Cl2 Tc S1 92.86(2) yes
P1 Tc S1 88.98(2) yes
P2 Tc S1 173.62(2) yes
Cl1 Tc S2 92.02(2) yes
Cl2 Tc S2 92.00(2) yes
P1 Tc S2 168.73(2) yes
P2 Tc S2 93.80(2) yes
S1 Tc S2 80.04(2) yes
C11 P1 C18 104.23(11) ?
C11 P1 C17 102.43(11) ?
C18 P1 C17 102.31(13) ?
C11 P1 Tc 119.92(7) ?
C18 P1 Tc 113.77(9) ?
C17 P1 Tc 112.17(8) ?
C27 P2 C21 103.94(10) ?
C27 P2 C28 103.55(13) ?
C21 P2 C28 101.14(11) ?
C27 P2 Tc 116.27(8) ?
C21 P2 Tc 113.88(7) ?
C28 P2 Tc 116.17(9) ?
O2 P3 O1 95.70(9) yes
O2 P3 S2 114.08(8) yes
O1 P3 S2 113.92(8) yes
O2 P3 S1 113.70(8) yes
O1 P3 S1 114.27(8) yes
S2 P3 S1 105.41(3) yes
P3 S1 Tc 87.46(3) ?
P3 S2 Tc 87.09(3) ?
C1 O1 P3 121.0(2) ?
C3 O2 P3 120.3(2) ?
C2 C1 O1 110.3(2) ?
O2 C3 C4 109.1(2) ?
C12 C11 C16 118.9(2) ?
C12 C11 P1 119.6(2) ?
C16 C11 P1 121.4(2) ?
C13 C12 C11 120.0(3) ?
C14 C13 C12 120.2(3) ?
C13 C14 C15 120.5(3) ?
C14 C15 C16 119.9(3) ?
C15 C16 C11 120.4(3) ?
C22 C21 C26 118.4(2) ?
C22 C21 P2 122.9(2) ?
C26 C21 P2 118.7(2) ?
C23 C22 C21 120.3(2) ?
C24 C23 C22 120.6(2) ?
C25 C24 C23 119.7(2) ?
C24 C25 C26 120.3(2) ?
C25 C26 C21 120.6(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Tc Cl1 2.3531(6) yes
Tc Cl2 2.3559(6) yes
Tc P1 2.4237(6) yes
Tc P2 2.4397(6) yes
Tc S1 2.4639(7) yes
Tc S2 2.4787(6) yes
P1 C11 1.815(2) ?
P1 C18 1.816(2) ?
P1 C17 1.820(2) ?
P2 C27 1.818(2) ?
P2 C21 1.821(2) ?
P2 C28 1.824(2) ?
P3 O2 1.570(2) yes
P3 O1 1.576(2) yes
P3 S2 1.9969(9) yes
P3 S1 1.9984(8) yes
O1 C1 1.455(3) ?
O2 C3 1.457(3) ?
C1 C2 1.439(4) ?
C3 C4 1.464(4) ?
C11 C12 1.389(3) ?
C11 C16 1.392(3) ?
C12 C13 1.387(4) ?
C13 C14 1.367(5) ?
C14 C15 1.372(6) ?
C15 C16 1.380(4) ?
C21 C22 1.390(3) ?
C21 C26 1.400(3) ?
C22 C23 1.384(3) ?
C23 C24 1.377(4) ?
C24 C25 1.376(3) ?
C25 C26 1.378(3) ?
