#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:53:12 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179082 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/44/4304402.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_4304402
loop_
_publ_author_name
'Yuji Tooyama'
'Henrik Braband'
'Bernhard Spingler'
'Ulrich Abram'
'Roger Alberto'
_publ_section_title
;
High-Valent Technetium Complexes with the [99TcO3]+ Core from in Situ
Prepared Mixed Anhydrides of [99TcO4]- and Their Reactivities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              257
_journal_page_last               264
_journal_paper_doi               10.1021/ic701908q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '[TcO3Cl(phen)]'
_chemical_formula_sum            'C12 H8 Cl N2 O3 Tc'
_chemical_formula_weight         361.65
_chemical_name_common            '[TcO3Cl(phen)]'
_chemical_name_systematic
;
Chloro-trioxo-1,10-phenanthroline-technetium(VII)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 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                 97.2381(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5144(2)
_cell_length_b                   11.6160(2)
_cell_length_c                   13.9303(3)
_cell_measurement_reflns_used    7878
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      37.5511
_cell_measurement_theta_min      2.2858
_cell_volume                     1206.25(5)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       '/o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15523
_diffrn_reflns_theta_full        36.32
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         31904
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         3039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0285
_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)+(0.0416P)²+0.2366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                2322
_reflns_number_total             3039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701908q-file003.cif
_cod_data_source_block           yt130207
_cod_database_code               4304402
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.07697(3) 0.0000 0.155407(16) 0.02248(7) Uani 0.94 2 d SP . .
Tc2 Tc 0.1512(6) 0.0000 0.1808(3) 0.0211(7) Uiso 0.06 2 d SP . .
C2 C -0.10017(19) 0.06192(14) 0.33901(10) 0.0207(3) Uani 1 1 d . . .
C3 C -0.1800(2) 0.12194(15) 0.40954(11) 0.0234(3) Uani 1 1 d . . .
C4 C -0.1662(2) 0.24331(15) 0.40888(12) 0.0267(3) Uani 1 1 d . . .
H4 H -0.2198 0.2881 0.4546 0.032 Uiso 1 1 calc R . .
C5 C -0.0754(2) 0.29557(15) 0.34227(12) 0.0270(3) Uani 1 1 d . . .
H5 H -0.0636 0.3770 0.3421 0.032 Uiso 1 1 calc R . .
C6 C 0.0004(2) 0.22931(14) 0.27411(12) 0.0249(3) Uani 1 1 d . . .
H6 H 0.0639 0.2669 0.2283 0.030 Uiso 1 1 calc R . .
C7 C -0.2629(2) 0.05872(17) 0.48010(11) 0.0282(3) Uani 1 1 d . . .
H7 H -0.3187 0.0991 0.5276 0.034 Uiso 1 1 calc R . .
N1 N -0.01399(18) 0.11464(12) 0.27158(9) 0.0214(2) Uani 1 1 d . . .
O1 O -0.1494(2) 0.0000 0.10701(11) 0.0223(3) Uani 1 2 d S . .
O2 O 0.16361(18) 0.11883(12) 0.10620(9) 0.0321(3) Uani 1 1 d . . .
Cl1 Cl 0.34458(8) 0.0000 0.28230(4) 0.02675(12) Uani 1 2 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'
N N 0.0061 0.0033 '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'
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
O2 Tc1 O2 107.99(9) 6 . ?
O2 Tc1 O1 104.30(6) . . ?
O2 Tc1 N1 157.92(6) 6 . ?
O2 Tc1 N1 88.64(5) . . ?
O1 Tc1 N1 84.78(5) . . ?
O2 Tc1 N1 88.64(5) 6 6 ?
O2 Tc1 N1 157.92(6) . 6 ?
O1 Tc1 N1 84.78(5) . 6 ?
N1 Tc1 N1 71.96(7) . 6 ?
O2 Tc1 Cl1 88.31(5) . . ?
O1 Tc1 Cl1 158.04(6) . . ?
N1 Tc1 Cl1 77.50(4) . . ?
O2 Tc2 O2 105.2(2) 6 . ?
O2 Tc2 Cl1 110.62(17) . . ?
O2 Tc2 N1 149.4(2) 6 . ?
O2 Tc2 N1 86.70(9) . . ?
Cl1 Tc2 N1 90.34(13) . . ?
Tc1 Tc2 N1 78.8(3) . 6 ?
O2 Tc2 N1 86.70(9) 6 6 ?
O2 Tc2 N1 149.4(2) . 6 ?
Cl1 Tc2 N1 90.34(14) . 6 ?
N1 Tc2 N1 70.62(12) . 6 ?
Tc1 Tc2 O1 8.8(2) . . ?
O2 Tc2 O1 81.97(16) . . ?
Cl1 Tc2 O1 157.86(19) . . ?
N1 Tc2 O1 71.76(12) . . ?
N1 C2 C3 123.15(15) . . ?
N1 C2 C2 116.92(9) . 6 ?
C3 C2 C2 119.87(10) . 6 ?
C2 C3 C4 116.99(15) . . ?
C2 C3 C7 119.25(15) . . ?
C4 C3 C7 123.71(15) . . ?
C5 C4 C3 119.51(16) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 119.95(17) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N1 C6 C5 121.88(16) . . ?
N1 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C7 C7 C3 120.87(10) 6 . ?
C7 C7 H7 119.6 6 . ?
C3 C7 H7 119.6 . . ?
C6 N1 C2 118.49(14) . . ?
C6 N1 Tc1 125.01(11) . . ?
C2 N1 Tc1 116.33(10) . . ?
C6 N1 Tc2 122.90(12) . . ?
C2 N1 Tc2 117.23(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
Tc1 O2 1.7063(13) . ?
Tc1 O1 1.7492(17) . ?
Tc1 N1 2.2667(14) . ?
Tc1 Cl1 2.5045(6) . ?
Tc2 O2 1.737(2) . ?
Tc2 Cl1 1.896(4) . ?
Tc2 N1 2.304(3) . ?
Tc2 O1 2.361(5) . ?
C2 N1 1.353(2) . ?
C2 C3 1.400(2) . ?
C2 C2 1.438(3) 6 ?
C3 C4 1.414(2) . ?
C3 C7 1.431(2) . ?
C4 C5 1.362(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(2) . ?
C5 H5 0.9500 . ?
C6 N1 1.336(2) . ?
C6 H6 0.9500 . ?
C7 C7 1.364(4) 6 ?
C7 H7 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 C4 -0.6(2) . . . . ?
C2 C2 C3 C4 176.41(10) 6 . . . ?
N1 C2 C3 C7 -177.84(14) . . . . ?
C2 C2 C3 C7 -0.86(17) 6 . . . ?
C2 C3 C4 C5 -1.0(2) . . . . ?
C7 C3 C4 C5 176.09(15) . . . . ?
C3 C4 C5 C6 1.2(2) . . . . ?
C4 C5 C6 N1 0.3(2) . . . . ?
C2 C3 C7 C7 0.86(18) . . . 6 ?
C4 C3 C7 C7 -176.20(11) . . . 6 ?
C5 C6 N1 C2 -1.9(2) . . . . ?
C5 C6 N1 Tc1 173.17(11) . . . . ?
C5 C6 N1 Tc2 -168.16(17) . . . . ?
C3 C2 N1 C6 2.1(2) . . . . ?
C2 C2 N1 C6 -175.01(10) 6 . . . ?
C3 C2 N1 Tc1 -173.47(12) . . . . ?
C2 C2 N1 Tc1 9.46(11) 6 . . . ?
C3 C2 N1 Tc2 169.07(17) . . . . ?
C2 C2 N1 Tc2 -8.00(16) 6 . . . ?
O2 Tc1 N1 C6 144.80(16) 6 . . . ?
O2 Tc1 N1 C6 5.05(13) . . . . ?
O1 Tc1 N1 C6 -99.44(13) . . . . ?
N1 Tc1 N1 C6 174.36(11) 6 . . . ?
Cl1 Tc1 N1 C6 93.62(13) . . . . ?
O2 Tc1 N1 C2 -40.0(2) 6 . . . ?
O2 Tc1 N1 C2 -179.74(11) . . . . ?
O1 Tc1 N1 C2 75.76(10) . . . . ?
N1 Tc1 N1 C2 -10.43(12) 6 . . . ?
Cl1 Tc1 N1 C2 -91.17(10) . . . . ?
O2 Tc2 N1 C6 -140.5(3) 6 . . . ?
O2 Tc2 N1 C6 -25.7(2) . . . . ?
Cl1 Tc2 N1 C6 84.90(15) . . . . ?
N1 Tc2 N1 C6 175.14(10) 6 . . . ?
O1 Tc2 N1 C6 -108.36(14) . . . . ?
O2 Tc2 N1 C2 53.1(4) 6 . . . ?
O2 Tc2 N1 C2 167.88(14) . . . . ?
Cl1 Tc2 N1 C2 -81.49(13) . . . . ?
N1 Tc2 N1 C2 8.75(18) 6 . . . ?
O1 Tc2 N1 C2 85.25(13) . . . . ?
