#------------------------------------------------------------------------------
#$Date: 2010-09-26 12:00:33 +0100 (Sun, 26 Sep 2010) $
#$Revision: 1526 $
#$URL: svn://www.crystallography.net/cod/cif/4/4308514.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_4308514
loop_
_publ_author_name
'Roger Schibli'
'Niklaus Marti'
'Patrick Maurer'
'Bernhard Spingler'
'Marie-Line Lehaire'
'Volker Gramlich'
'Charles L. Barnes'
_publ_section_title
;
Syntheses and Characterization of Dicarbonyl-Nitrosyl Complexes of
Technetium(I) and Rhenium(I) in Aqueous Media: Spectroscopic, Structural,
and DFT Analyses
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              683
_journal_page_last               690
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C4 Cl4 N2 O6 Tc2'
_chemical_formula_weight         509.86
_chemical_name_systematic
; 
 ditechnetium(I)-hexachloro-tetracarbonyl-dinitrosyl 
;
_space_group_IT_number           9
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 105.80(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.82(3)
_cell_length_b                   6.103(6)
_cell_length_c                   12.151(16)
_cell_measurement_temperature    293(2)
_cell_volume                     1343(3)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'PICKER STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            707
_diffrn_reflns_theta_full        49.92
_diffrn_reflns_theta_max         49.92
_diffrn_reflns_theta_min         4.88
_exptl_absorpt_coefficient_mu    24.267
_exptl_absorpt_correction_T_max  .304
_exptl_absorpt_correction_T_min  .125
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          .09
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         707
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                691
_reflns_number_total             707
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    ic049599ksi20041013_083251_1.cif
_[local]_cod_data_source_block   tec2
_cod_database_code               4308514
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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc1 Tc 0.37742(3) 0.07498(12) 0.38582(4) 0.0358(2) Uani 1 1 d DU . .
Tc2 Tc 0.18807(3) 0.04071(11) 0.41511(4) 0.0358(2) Uani 1 1 d DU . .
Cl1 Cl 0.25821(14) -0.0924(4) 0.2840(2) 0.0466(7) Uani 1 1 d U . .
Cl2 Cl 0.30710(14) 0.2133(4) 0.5142(2) 0.0470(6) Uani 1 1 d U . .
Cl3 Cl 0.40671(16) -0.2447(4) 0.5009(2) 0.0555(8) Uani 1 1 d U . .
Cl4 Cl 0.15686(16) 0.3623(5) 0.3017(2) 0.0550(8) Uani 1 1 d U . .
N1 N 0.3630(4) 0.3094(12) 0.3002(7) 0.044(2) Uani 1 1 d DU . .
O4 O 0.1060(4) 0.2606(13) 0.5702(6) 0.061(2) Uani 1 1 d U . .
O1 O 0.4629(5) -0.1560(14) 0.2359(7) 0.073(2) Uani 1 1 d U . .
C4 C 0.1372(5) 0.1831(18) 0.5162(9) 0.044(2) Uani 1 1 d U . .
C1 C 0.4305(6) -0.0660(16) 0.2870(9) 0.048(2) Uani 1 1 d U . .
O3 O 0.0394(4) -0.1438(13) 0.2729(7) 0.062(2) Uani 1 1 d U . .
N2 N 0.2095(5) -0.1990(13) 0.5032(7) 0.0434(19) Uani 1 1 d DU . .
O6 O 0.2170(5) -0.3507(14) 0.5590(6) 0.066(2) Uani 1 1 d U . .
O5 O 0.3558(5) 0.4631(13) 0.2418(7) 0.066(3) Uani 1 1 d U . .
C3 C 0.0974(6) -0.0849(16) 0.3221(9) 0.044(2) Uani 1 1 d U . .
O2 O 0.5257(4) 0.2695(15) 0.5328(6) 0.064(2) Uani 1 1 d U . .
C2 C 0.4703(6) 0.1974(17) 0.4802(9) 0.043(2) Uani 1 1 d U . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tc1 0.0360(4) 0.0339(4) 0.0383(4) 0.0008(3) 0.0116(3) -0.0023(3)
Tc2 0.0360(4) 0.0342(5) 0.0382(4) -0.0017(4) 0.0118(3) -0.0032(4)
Cl1 0.0445(12) 0.0523(15) 0.0451(12) -0.0132(11) 0.0159(10) -0.0109(11)
Cl2 0.0445(12) 0.0518(14) 0.0469(11) -0.0179(12) 0.0161(10) -0.0089(12)
Cl3 0.0627(15) 0.0431(14) 0.0572(15) 0.0126(13) 0.0105(13) 0.0034(13)
Cl4 0.0651(16) 0.0473(15) 0.0501(14) 0.0101(13) 0.0115(12) 0.0028(14)
N1 0.043(4) 0.038(3) 0.051(4) 0.001(3) 0.011(3) -0.001(3)
O4 0.061(4) 0.062(4) 0.067(4) -0.013(4) 0.031(3) 0.003(3)
O1 0.083(5) 0.080(5) 0.064(4) -0.016(4) 0.035(3) 0.005(5)
C4 0.039(4) 0.042(5) 0.052(4) 0.000(3) 0.016(3) 0.002(4)
C1 0.054(4) 0.047(5) 0.047(4) -0.001(3) 0.021(3) 0.003(4)
O3 0.049(4) 0.065(4) 0.064(4) -0.001(4) 0.002(3) -0.017(4)
N2 0.047(4) 0.039(3) 0.043(4) 0.001(3) 0.010(3) 0.004(3)
O6 0.093(5) 0.055(4) 0.048(4) 0.013(3) 0.018(4) 0.007(5)
O5 0.082(6) 0.041(4) 0.073(5) 0.016(3) 0.016(5) 0.008(4)
C3 0.038(4) 0.048(5) 0.047(4) 0.001(4) 0.012(3) 0.000(4)
O2 0.052(4) 0.087(5) 0.052(4) 0.003(4) 0.014(3) -0.020(4)
C2 0.044(4) 0.044(4) 0.045(4) 0.000(4) 0.019(3) -0.010(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc 0.0057 3.0049 '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 Tc1 C2 90.3(4) . . ?
N1 Tc1 C1 91.0(4) . . ?
C2 Tc1 C1 90.2(5) . . ?
N1 Tc1 Cl3 175.4(3) . . ?
C2 Tc1 Cl3 86.7(3) . . ?
C1 Tc1 Cl3 85.7(3) . . ?
N1 Tc1 Cl2 94.3(3) . . ?
C2 Tc1 Cl2 92.7(3) . . ?
C1 Tc1 Cl2 174.0(3) . . ?
Cl3 Tc1 Cl2 89.28(12) . . ?
N1 Tc1 Cl1 93.9(3) . . ?
C2 Tc1 Cl1 174.5(3) . . ?
C1 Tc1 Cl1 93.2(3) . . ?
Cl3 Tc1 Cl1 89.36(15) . . ?
Cl2 Tc1 Cl1 83.51(14) . . ?
N2 Tc2 C3 92.6(4) . . ?
N2 Tc2 C4 93.2(4) . . ?
C3 Tc2 C4 92.2(5) . . ?
N2 Tc2 Cl4 178.1(3) . . ?
C3 Tc2 Cl4 87.1(3) . . ?
C4 Tc2 Cl4 84.9(3) . . ?
N2 Tc2 Cl1 92.5(3) . . ?
C3 Tc2 Cl1 92.0(4) . . ?
C4 Tc2 Cl1 172.7(3) . . ?
Cl4 Tc2 Cl1 89.34(12) . . ?
N2 Tc2 Cl2 91.7(3) . . ?
C3 Tc2 Cl2 173.7(4) . . ?
C4 Tc2 Cl2 92.2(3) . . ?
Cl4 Tc2 Cl2 88.79(15) . . ?
Cl1 Tc2 Cl2 83.18(14) . . ?
Tc2 Cl1 Tc1 96.50(14) . . ?
Tc1 Cl2 Tc2 96.80(14) . . ?
O5 N1 Tc1 177.4(8) . . ?
O4 C4 Tc2 177.1(9) . . ?
O1 C1 Tc1 175.5(10) . . ?
O6 N2 Tc2 174.3(9) . . ?
O3 C3 Tc2 172.3(10) . . ?
O2 C2 Tc1 178.0(9) . . ?
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 N1 1.746(8) . ?
Tc1 C2 1.959(10) . ?
Tc1 C1 1.957(12) . ?
Tc1 Cl3 2.376(3) . ?
Tc1 Cl2 2.454(4) . ?
Tc1 Cl1 2.469(5) . ?
Tc2 N2 1.793(8) . ?
Tc2 C3 1.931(11) . ?
Tc2 C4 1.955(11) . ?
Tc2 Cl4 2.378(3) . ?
Tc2 Cl1 2.467(4) . ?
Tc2 Cl2 2.472(5) . ?
N1 O5 1.161(11) . ?
O4 C4 1.100(13) . ?
O1 C1 1.126(14) . ?
O3 C3 1.151(13) . ?
N2 O6 1.133(11) . ?
O2 C2 1.151(12) . ?