#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:52:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179267 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/87/4318750.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_4318750
loop_
_publ_author_name
'Evan Freiberg'
'William M. Davis'
'Terrence Nicholson'
'Alan Davison'
'Alun G. Jones'
_publ_section_title
;
 Reduction of the Pertechnetate Anion with Bidentate Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5667
_journal_page_last               5674
_journal_paper_doi               10.1021/ic020032i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         TcCl2(dppm)2
_chemical_formula_sum            'C50 H44 Cl2 P4 Tc'
_chemical_formula_weight         937.63
_chemical_name_systematic
;
  ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                92.771(2)
_cell_angle_beta                 104.474(2)
_cell_angle_gamma                104.771(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0256(11)
_cell_length_b                   11.2695(11)
_cell_length_c                   11.7812(12)
_cell_measurement_temperature    185(2)
_cell_volume                     1360.7(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4126
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.8887
_exptl_absorpt_correction_T_min  0.7920
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             481
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0011(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.182
_refine_ls_goodness_of_fit_obs   1.214
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.231
_refine_ls_restrained_S_obs      1.214
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_obs          0.0755
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0634P)²+11.0815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1901
_refine_ls_wR_factor_obs         0.1767
_reflns_number_observed          2265
_reflns_number_total             2535
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020032i_1.cif
_cod_data_source_block           99113
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+11.0815P] 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^)+(0.0634P)^2^+11.0815P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318750
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tc Tc 0.0000 0.0000 0.0000 0.0191(5) Uani 1 d S .
Cl Cl 0.1366(3) -0.1291(2) -0.0344(2) 0.0418(8) Uani 1 d . .
P1 P 0.1385(3) 0.0445(3) 0.1987(2) 0.0346(8) Uani 1 d . .
P2 P 0.1994(3) 0.1626(3) 0.0136(2) 0.0344(8) Uani 1 d . .
C1 C 0.2856(10) 0.1271(10) 0.1554(9) 0.040(3) Uani 1 d . .
H1A H 0.3374(10) 0.2025(10) 0.2103(9) 0.048 Uiso 1 calc R .
H1B H 0.3418(10) 0.0732(10) 0.1469(9) 0.048 Uiso 1 calc R .
C11 C 0.1118(11) 0.1512(11) 0.3077(9) 0.042(3) Uani 1 d . .
C12 C 0.0200(12) 0.1023(12) 0.3659(11) 0.056(4) Uani 1 d . .
H12A H -0.0237(12) 0.0165(12) 0.3505(11) 0.067 Uiso 1 calc R .
C13 C -0.0096(12) 0.1754(13) 0.4458(11) 0.056(4) Uani 1 d . .
H13A H -0.0743(12) 0.1400(13) 0.4839(11) 0.068 Uiso 1 calc R .
C14 C 0.0531(13) 0.2984(13) 0.4709(11) 0.057(4) Uani 1 d . .
H14A H 0.0340(13) 0.3482(13) 0.5277(11) 0.069 Uiso 1 calc R .
C15 C 0.1433(14) 0.3492(12) 0.4138(11) 0.065(4) Uani 1 d . .
H15A H 0.1855(14) 0.4353(12) 0.4298(11) 0.078 Uiso 1 calc R .
C16 C 0.1754(13) 0.2752(11) 0.3303(10) 0.060(4) Uani 1 d . .
H16A H 0.2392(13) 0.3108(11) 0.2913(10) 0.072 Uiso 1 calc R .
C21 C 0.2943(10) 0.1518(9) -0.0911(10) 0.038(3) Uani 1 d . .
C22 C 0.2465(12) 0.1776(12) -0.2036(12) 0.059(4) Uani 1 d . .
H22A H 0.1667(12) 0.1993(12) -0.2232(12) 0.071 Uiso 1 calc R .
C23 C 0.3130(14) 0.1725(15) -0.2906(12) 0.077(5) Uani 1 d . .
H23A H 0.2779(14) 0.1882(15) -0.3688(12) 0.092 Uiso 1 calc R .
C24 C 0.4290(15) 0.1446(12) -0.2594(13) 0.061(4) Uani 1 d . .
H24A H 0.4757(15) 0.1426(12) -0.3169(13) 0.073 Uiso 1 calc R .
C25 C 0.4796(14) 0.1199(11) -0.1502(15) 0.064(4) Uani 1 d . .
H25A H 0.5602(14) 0.0995(11) -0.1318(15) 0.077 Uiso 1 calc R .
C26 C 0.4124(11) 0.1241(9) -0.0615(11) 0.044(3) Uani 1 d . .
H26A H 0.4484(11) 0.1081(9) 0.0164(11) 0.052 Uiso 1 calc R .
C31 C 0.1904(10) -0.0682(10) 0.2915(10) 0.035(3) Uani 1 d . .
C32 C 0.1326(12) -0.1936(12) 0.2619(11) 0.053(3) Uani 1 d . .
H32A H 0.0646(12) -0.2225(12) 0.1910(11) 0.064 Uiso 1 calc R .
C33 C 0.1730(15) -0.2794(12) 0.3355(12) 0.058(4) Uani 1 d . .
H33A H 0.1308(15) -0.3653(12) 0.3149(12) 0.070 Uiso 1 calc R .
C34 C 0.2729(13) -0.2390(13) 0.4367(11) 0.053(3) Uani 1 d . .
H34A H 0.3007(13) -0.2967(13) 0.4859(11) 0.064 Uiso 1 calc R .
C35 C 0.3331(12) -0.1139(14) 0.4671(11) 0.056(4) Uani 1 d . .
H35A H 0.4033(12) -0.0856(14) 0.5365(11) 0.067 Uiso 1 calc R .
C36 C 0.2899(11) -0.0280(12) 0.3948(10) 0.044(3) Uani 1 d . .
H36A H 0.3295(11) 0.0581(12) 0.4173(10) 0.053 Uiso 1 calc R .
C41 C 0.2292(10) 0.3314(9) 0.0433(9) 0.034(3) Uani 1 d . .
C42 C 0.1291(11) 0.3807(10) 0.0544(10) 0.041(3) Uani 1 d . .
H42A H 0.0429(11) 0.3287(10) 0.0400(10) 0.049 Uiso 1 calc R .
C43 C 0.1565(11) 0.5090(10) 0.0872(11) 0.048(3) Uani 1 d . .
H43A H 0.0891(11) 0.5432(10) 0.0974(11) 0.057 Uiso 1 calc R .
C44 C 0.2784(13) 0.5827(11) 0.1040(11) 0.059(4) Uani 1 d . .
H44A H 0.2955(13) 0.6694(11) 0.1229(11) 0.071 Uiso 1 calc R .
C45 C 0.3804(13) 0.5334(11) 0.0940(11) 0.058(4) Uani 1 d . .
H45A H 0.4667(13) 0.5853(11) 0.1078(11) 0.070 Uiso 1 calc R .
C46 C 0.3525(11) 0.4090(11) 0.0640(11) 0.050(3) Uani 1 d . .
H46A H 0.4211(11) 0.3748(11) 0.0572(11) 0.060 Uiso 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'
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
_geom_angle_publ_flag
P1 Tc P1 180.0 2 . ?
P1 Tc Cl 85.64(9) 2 2 ?
P1 Tc Cl 94.36(9) . 2 ?
P1 Tc Cl 94.36(9) 2 . ?
P1 Tc Cl 85.64(9) . . ?
Cl Tc Cl 180.0 2 . ?
P1 Tc P2 110.95(9) 2 . ?
P1 Tc P2 69.05(9) . . ?
Cl Tc P2 98.75(9) 2 . ?
Cl Tc P2 81.25(9) . . ?
P1 Tc P2 69.05(9) 2 2 ?
P1 Tc P2 110.95(9) . 2 ?
Cl Tc P2 81.25(9) 2 2 ?
Cl Tc P2 98.75(9) . 2 ?
P2 Tc P2 180.0 . 2 ?
C31 P1 C11 101.1(5) . . ?
C31 P1 C1 104.9(5) . . ?
C11 P1 C1 107.4(5) . . ?
C31 P1 Tc 126.1(4) . . ?
C11 P1 Tc 120.4(4) . . ?
C1 P1 Tc 94.3(3) . . ?
C1 P2 C21 108.2(5) . . ?
C1 P2 C41 101.3(5) . . ?
C21 P2 C41 101.9(5) . . ?
C1 P2 Tc 93.9(3) . . ?
C21 P2 Tc 119.7(3) . . ?
C41 P2 Tc 128.3(4) . . ?
P2 C1 P1 96.5(5) . . ?
C16 C11 C12 119.4(10) . . ?
C16 C11 P1 123.5(9) . . ?
C12 C11 P1 117.1(9) . . ?
C13 C12 C11 121.2(12) . . ?
C14 C13 C12 120.5(12) . . ?
C15 C14 C13 119.4(12) . . ?
C14 C15 C16 121.0(12) . . ?
C11 C16 C15 118.4(11) . . ?
C22 C21 C26 119.2(11) . . ?
C22 C21 P2 117.3(9) . . ?
C26 C21 P2 123.5(9) . . ?
C21 C22 C23 121.6(12) . . ?
C24 C23 C22 118.1(13) . . ?
C25 C24 C23 122.1(13) . . ?
C24 C25 C26 120.2(13) . . ?
C21 C26 C25 118.8(12) . . ?
C32 C31 C36 118.6(11) . . ?
C32 C31 P1 121.7(9) . . ?
C36 C31 P1 119.6(8) . . ?
C31 C32 C33 121.0(12) . . ?
C34 C33 C32 120.0(12) . . ?
C33 C34 C35 119.8(12) . . ?
C34 C35 C36 119.9(12) . . ?
C31 C36 C35 120.6(12) . . ?
C46 C41 C42 118.9(10) . . ?
C46 C41 P2 120.5(8) . . ?
C42 C41 P2 120.4(8) . . ?
C41 C42 C43 119.4(10) . . ?
C44 C43 C42 119.9(11) . . ?
C43 C44 C45 121.0(11) . . ?
C46 C45 C44 118.3(11) . . ?
C45 C46 C41 122.5(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 P1 2.402(3) 2 ?
Tc P1 2.402(3) . ?
Tc Cl 2.432(3) 2 ?
Tc Cl 2.432(3) . ?
Tc P2 2.441(3) . ?
Tc P2 2.441(3) 2 ?
P1 C31 1.825(12) . ?
P1 C11 1.844(11) . ?
P1 C1 1.857(10) . ?
P2 C1 1.821(11) . ?
P2 C21 1.823(11) . ?
P2 C41 1.846(11) . ?
C11 C16 1.37(2) . ?
C11 C12 1.38(2) . ?
C12 C13 1.37(2) . ?
C13 C14 1.36(2) . ?
C14 C15 1.36(2) . ?
C15 C16 1.43(2) . ?
C21 C22 1.37(2) . ?
C21 C26 1.381(15) . ?
C22 C23 1.41(2) . ?
C23 C24 1.36(2) . ?
C24 C25 1.34(2) . ?
C25 C26 1.43(2) . ?
C31 C32 1.38(2) . ?
C31 C36 1.383(15) . ?
C32 C33 1.41(2) . ?
C33 C34 1.37(2) . ?
C34 C35 1.38(2) . ?
C35 C36 1.42(2) . ?
C41 C46 1.371(15) . ?
C41 C42 1.386(14) . ?
C42 C43 1.413(15) . ?
C43 C44 1.35(2) . ?
C44 C45 1.40(2) . ?
C45 C46 1.37(2) . ?
