#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:43:34 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239897 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/04/4350441.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_4350441
loop_
_publ_author_name
'Hagenbach, Adelheid'
'Yegen, Eda'
'Abram, Ulrich'
_publ_section_title
;
 Technetium tetrachloride as a precursor for small technetium(IV)
 complexes.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7331
_journal_page_last               7338
_journal_paper_doi               10.1021/ic060896u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         TcCl4(OPPh3)2
_chemical_formula_sum            'C36 H30 Cl4 O2 P2 Tc'
_chemical_formula_weight         796.34
_chemical_name_common            TcCl4(OPPh3)2
_chemical_name_systematic
;
tetrachlorobis(triphenylphosphine oxide)technetium(IV)
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.82(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.896(1)
_cell_length_b                   12.993(1)
_cell_length_c                   19.412(2)
_cell_measurement_reflns_used    7324
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.91
_cell_volume                     3486.8(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0826
_diffrn_reflns_av_sigmaI/netI    0.0918
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12299
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.166
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0644P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1166
_reflns_number_gt                2957
_reflns_number_total             4661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060896usi20060523_100113.cif
_cod_data_source_block           tccl4opph3
_cod_original_cell_volume        3486.7(5)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4350441
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tc Tc 0.5000 0.14216(3) -0.2500 0.02717(11) Uani 1 2 d S
Cl3 Cl 0.54606(7) 0.01513(9) -0.32298(6) 0.0537(3) Uani 1 1 d .
Cl1 Cl 0.34259(5) 0.15146(8) -0.30441(5) 0.0413(2) Uani 1 1 d .
O O 0.46168(17) 0.2540(2) -0.18510(13) 0.0424(6) Uani 1 1 d .
P P 0.47734(6) 0.32724(8) -0.12548(5) 0.0347(2) Uani 1 1 d .
C1 C 0.3600(2) 0.3592(3) -0.1004(2) 0.0384(8) Uani 1 1 d .
C2 C 0.2839(3) 0.3657(4) -0.1512(2) 0.0529(10) Uani 1 1 d .
H2 H 0.2932 0.3509 -0.1970 0.063 Uiso 1 1 calc R
C3 C 0.1936(3) 0.3942(4) -0.1343(3) 0.0623(13) Uani 1 1 d .
H3 H 0.1423 0.3999 -0.1687 0.075 Uiso 1 1 calc R
C4 C 0.1798(3) 0.4135(4) -0.0681(3) 0.0697(15) Uani 1 1 d .
H4 H 0.1189 0.4341 -0.0575 0.084 Uiso 1 1 calc R
C5 C 0.2541(4) 0.4036(5) -0.0153(3) 0.0782(17) Uani 1 1 d .
H5 H 0.2427 0.4145 0.0305 0.094 Uiso 1 1 calc R
C6 C 0.3455(3) 0.3773(4) -0.0318(2) 0.0588(12) Uani 1 1 d .
H6 H 0.3967 0.3717 0.0028 0.071 Uiso 1 1 calc R
C11 C 0.5375(3) 0.4419(3) -0.15019(19) 0.0407(8) Uani 1 1 d .
C12 C 0.4975(3) 0.5387(3) -0.1436(3) 0.0560(11) Uani 1 1 d .
H12 H 0.4365 0.5455 -0.1283 0.067 Uiso 1 1 calc R
C13 C 0.5483(4) 0.6243(4) -0.1596(3) 0.0757(16) Uani 1 1 d .
H13 H 0.5222 0.6894 -0.1547 0.091 Uiso 1 1 calc R
C14 C 0.6380(4) 0.6139(4) -0.1831(3) 0.0729(15) Uani 1 1 d .
H14 H 0.6722 0.6722 -0.1940 0.088 Uiso 1 1 calc R
C15 C 0.6776(3) 0.5175(4) -0.1907(3) 0.0585(12) Uani 1 1 d .
H15 H 0.7382 0.5104 -0.2065 0.070 Uiso 1 1 calc R
C16 C 0.6259(3) 0.4329(4) -0.1745(2) 0.0499(10) Uani 1 1 d .
H16 H 0.6516 0.3677 -0.1803 0.060 Uiso 1 1 calc R
C21 C 0.5483(2) 0.2768(3) -0.05025(19) 0.0384(8) Uani 1 1 d .
C22 C 0.6122(3) 0.3380(4) -0.0095(2) 0.0517(11) Uani 1 1 d .
H22 H 0.6226 0.4055 -0.0229 0.062 Uiso 1 1 calc R
C23 C 0.6611(3) 0.3004(4) 0.0508(3) 0.0627(13) Uani 1 1 d .
H23 H 0.7038 0.3424 0.0780 0.075 Uiso 1 1 calc R
C24 C 0.6463(3) 0.2008(5) 0.0703(2) 0.0661(14) Uani 1 1 d .
H24 H 0.6788 0.1753 0.1110 0.079 Uiso 1 1 calc R
C25 C 0.5842(4) 0.1389(5) 0.0304(3) 0.0698(14) Uani 1 1 d .
H25 H 0.5749 0.0711 0.0437 0.084 Uiso 1 1 calc R
C26 C 0.5347(3) 0.1767(4) -0.0300(2) 0.0568(11) Uani 1 1 d .
H26 H 0.4922 0.1342 -0.0570 0.068 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'
O O 0.0106 0.0060 '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'
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
O Tc O 88.56(17) 2_654 .
O Tc Cl3 179.09(7) 2_654 2_654
O Tc Cl3 91.39(9) . 2_654
O Tc Cl3 91.39(9) 2_654 .
O Tc Cl3 179.09(7) . .
Cl3 Tc Cl3 88.67(7) 2_654 .
O Tc Cl1 87.19(7) 2_654 2_654
O Tc Cl1 88.56(7) . 2_654
Cl3 Tc Cl1 93.71(4) 2_654 2_654
Cl3 Tc Cl1 90.53(3) . 2_654
O Tc Cl1 88.56(7) 2_654 .
O Tc Cl1 87.19(7) . .
Cl3 Tc Cl1 90.53(3) 2_654 .
Cl3 Tc Cl1 93.71(4) . .
Cl1 Tc Cl1 174.07(5) 2_654 .
P O Tc 155.28(15) . .
O P C1 106.96(16) . .
O P C11 110.85(17) . .
C1 P C11 109.88(18) . .
O P C21 114.86(17) . .
C1 P C21 107.54(17) . .
C11 P C21 106.66(17) . .
C2 C1 C6 120.2(4) . .
C2 C1 P 118.3(3) . .
C6 C1 P 121.6(3) . .
C1 C2 C3 119.8(4) . .
C4 C3 C2 120.1(4) . .
C3 C4 C5 121.5(4) . .
C6 C5 C4 119.0(5) . .
C5 C6 C1 119.3(4) . .
C16 C11 C12 119.6(4) . .
C16 C11 P 118.7(3) . .
C12 C11 P 121.7(3) . .
C13 C12 C11 119.6(4) . .
C12 C13 C14 120.1(5) . .
C13 C14 C15 120.5(5) . .
C16 C15 C14 118.8(4) . .
C11 C16 C15 121.4(4) . .
C26 C21 C22 118.7(4) . .
C26 C21 P 119.7(3) . .
C22 C21 P 121.6(3) . .
C21 C22 C23 121.0(5) . .
C24 C23 C22 119.6(5) . .
C25 C24 C23 120.3(4) . .
C24 C25 C26 120.2(5) . .
C21 C26 C25 120.3(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc O 2.029(3) 2_654
Tc O 2.029(3) .
Tc Cl3 2.3076(11) 2_654
Tc Cl3 2.3076(11) .
Tc Cl1 2.3337(8) 2_654
Tc Cl1 2.3337(8) .
O P 1.497(3) .
P C1 1.797(3) .
P C11 1.798(4) .
P C21 1.800(4) .
C1 C2 1.374(5) .
C1 C6 1.388(6) .
C2 C3 1.379(6) .
C3 C4 1.341(8) .
C4 C5 1.385(8) .
C5 C6 1.384(6) .
C11 C16 1.365(5) .
C11 C12 1.387(6) .
C12 C13 1.370(7) .
C13 C14 1.377(8) .
C14 C15 1.381(7) .
C15 C16 1.367(6) .
C21 C26 1.377(6) .
C21 C22 1.379(5) .
C22 C23 1.382(6) .
C23 C24 1.369(8) .
C24 C25 1.363(8) .
C25 C26 1.388(6) .
