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#$Date: 2016-03-23 00:19:13 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179104 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/66/4306693.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_4306693
loop_
_publ_author_name
'Maaz Zuhayra'
'Ulf Lützen'
'Arne Lützen'
'Laszlo Papp'
'Eberhard Henze'
'Gernot Friedrichs'
'Franz Oberdorfer'
_publ_section_title
;
C-H Bond Activation of Coordinated Pyridine:
Ortho-Pyridyl-Ditechnetiumhydridocarbonyl Metal Cyclus. Crystal Structure
and Dynamic Behavior in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10177
_journal_page_last               10182
_journal_paper_doi               10.1021/ic8015063
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C21 H15 N3 O6 Tc2'
_chemical_formula_weight         601.36
_chemical_name_systematic
μ-(Pyridyl-1,2)-μ-Hydrido-bis(pyridino-tricarbonyltechnetium)
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.0880(10)
_cell_length_b                   10.0880(10)
_cell_length_c                   19.817(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1746.5(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_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  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2840
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.227
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.58(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_obs          0.0259
_refine_ls_shift/esd_max         -0.187
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0346P)²+0.4505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0729
_refine_ls_wR_factor_obs         0.0663
_reflns_number_observed          1886
_reflns_number_total             2044
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic8015063_si_002_2.cif
_cod_data_source_block           zuto
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.4505P] 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^)+(0.0346P)^2^+0.4505P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 3 2 21'
_cod_database_code               4306693
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'-x, -x+y, -z+2/3'
'x-y, -y, -z+1/3'
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
Tc1 Tc 0.40898(4) 0.40863(4) 0.081521(12) 0.04266(12) Uani 1 d . .
N1 N 0.5255(5) 0.2678(5) 0.0739(2) 0.0585(9) Uani 1 d . .
N2 N 0.2121(4) 0.2183(4) 0.0343(2) 0.053(10) Uani 0.50 d P 1
C11 C 0.2121(4) 0.2183(4) 0.0343(2) 0.046(11) Uani 0.50 d P 2
O1 O 0.6888(4) 0.6986(4) 0.1372(2) 0.0835(10) Uani 1 d . .
O2 O 0.2408(5) 0.5888(5) 0.0913(2) 0.0946(13) Uani 1 d . .
O3 O 0.3085(4) 0.2970(5) 0.2269(2) 0.0867(11) Uani 1 d . .
C1 C 0.5877(5) 0.5874(5) 0.1163(2) 0.0543(10) Uani 1 d . .
C2 C 0.3041(6) 0.5206(6) 0.0865(2) 0.0587(10) Uani 1 d . .
C3 C 0.3430(4) 0.3354(5) 0.1721(2) 0.0538(10) Uani 1 d . .
C4 C 0.6786(6) 0.3355(8) 0.0658(3) 0.077(2) Uani 1 d . .
H4 H 0.7359(6) 0.4414(8) 0.0615(3) 0.110(8) Uiso 1 calc R .
C5 C 0.7520(8) 0.2516(11) 0.0638(3) 0.102(2) Uani 1 d . .
H5 H 0.8578(8) 0.3012(11) 0.0588(3) 0.110(8) Uiso 1 calc R .
C6 C 0.6708(12) 0.0966(13) 0.0690(4) 0.128(3) Uani 1 d . .
H6 H 0.7191(12) 0.0386(13) 0.0668(4) 0.110(8) Uiso 1 calc R .
C7 C 0.5201(12) 0.0302(9) 0.0773(3) 0.115(3) Uani 1 d . .
H7 H 0.4626(12) -0.0756(9) 0.0817(3) 0.110(8) Uiso 1 calc R .
C8 C 0.4470(8) 0.1155(7) 0.0795(3) 0.0804(15) Uani 1 d . .
H8 H 0.3413(8) 0.0658(7) 0.0850(3) 0.110(8) Uiso 1 calc R .
C9 C 0.0853(6) 0.1031(6) 0.0677(3) 0.0666(13) Uani 1 d . .
H9 H 0.0779(6) 0.1100(6) 0.1142(3) 0.110(8) Uiso 1 calc R 1
C10 C -0.0291(5) -0.0205(5) 0.0343(3) 0.0713(14) Uani 1 d . .
H10 H -0.1112(5) -0.0973(5) 0.0580(3) 0.110(8) Uiso 1 calc R .
H1 H 0.4912(53) 0.4912(53) 0.0000 0.051(16) Uiso 1 d S .
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'
N N 0.0061 0.0033 '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
C2 Tc1 C3 89.5(2) . . ?
C2 Tc1 C1 87.9(2) . . ?
C3 Tc1 C1 90.5(2) . . ?
C2 Tc1 N2 90.8(2) . . ?
C3 Tc1 N2 94.27(15) . . ?
C1 Tc1 N2 175.07(15) . . ?
C2 Tc1 C11 90.8(2) . . ?
C3 Tc1 C11 94.27(15) . . ?
C1 Tc1 C11 175.07(15) . . ?
C2 Tc1 N1 177.8(2) . . ?
C3 Tc1 N1 90.53(15) . . ?
C1 Tc1 N1 94.3(2) . . ?
N2 Tc1 N1 87.05(14) . . ?
C11 Tc1 N1 87.05(14) . . ?
C8 N1 C4 117.5(4) . . ?
C8 N1 Tc1 121.5(3) . . ?
C4 N1 Tc1 120.9(4) . . ?
N2 N2 C9 118.7(3) 4 . ?
N2 N2 Tc1 115.37(9) 4 . ?
C9 N2 Tc1 125.9(3) . . ?
C11 C11 C9 118.7(3) 4 . ?
C11 C11 Tc1 115.37(9) 4 . ?
C9 C11 Tc1 125.9(3) . . ?
O1 C1 Tc1 175.7(4) . . ?
O2 C2 Tc1 178.2(4) . . ?
O3 C3 Tc1 177.3(4) . . ?
N1 C4 C5 121.6(6) . . ?
C6 C5 C4 120.3(6) . . ?
C7 C6 C5 118.0(6) . . ?
C6 C7 C8 121.4(8) . . ?
N1 C8 C7 121.2(7) . . ?
C10 C9 N2 122.2(4) . . ?
C10 C9 C11 122.2(4) . . ?
C10 C10 C9 119.0(3) 4 . ?
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
Tc1 C2 1.897(4) . ?
Tc1 C3 1.928(4) . ?
Tc1 C1 1.931(4) . ?
Tc1 N2 2.167(3) . ?
Tc1 C11 2.167(3) . ?
Tc1 N1 2.256(4) . ?
N1 C8 1.335(7) . ?
N1 C4 1.351(6) . ?
N2 N2 1.364(7) 4 ?
N2 C9 1.392(6) . ?
C11 C11 1.364(7) 4 ?
C11 C9 1.392(6) . ?
O1 C1 1.151(5) . ?
O2 C2 1.153(5) . ?
O3 C3 1.147(5) . ?
C4 C5 1.376(8) . ?
C5 C6 1.359(11) . ?
C6 C7 1.330(13) . ?
C7 C8 1.387(8) . ?
C9 C10 1.373(7) . ?
C10 C10 1.368(10) 4 ?
