#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:18:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178808 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/62/4106242.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_4106242
loop_
_publ_author_name
'Frederic Poineau'
'Christos D. Malliakas'
'Philippe F. Weck'
'Brian L. Scott'
'Erik V. Johnstone'
'Paul M. Forster'
'Eunja Kim'
'Mercouri G. Kanatzidis'
'Kenneth R. Czerwinski'
'Alfred P. Sattelberger'
_publ_section_title
;
 Technetium Dichloride: A New Binary Halide Containing Metal-Metal
 Multiple Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8814
_journal_page_last               8817
_journal_paper_doi               10.1021/ja201788m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'Cl2 Tc'
_chemical_formula_weight         169.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.557(3)
_cell_length_b                   8.557(3)
_cell_length_c                   3.417(2)
_cell_measurement_temperature    140(1)
_cell_volume                     250.20(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.966
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1302
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.68
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    7.476
_exptl_absorpt_correction_T_max  0.7541
_exptl_absorpt_correction_T_min  0.0315
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_density_diffrn    4.484
_exptl_crystal_F_000             308
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.841
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     13
_refine_ls_number_reflns         168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0312
_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)+(0.0777P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                168
_reflns_number_total             168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201788m_si_001.cif
_cod_data_source_block           apx1105
_cod_original_cell_volume        250.18(19)
_cod_database_code               4106242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Tc1 Tc 0.06287(8) 0.10728(8) 0.0000 0.0093(5) Uani 0.50 2 d SP
Cl1 Cl 0.25404(12) 0.06575(11) 0.5000 0.0070(5) Uani 1 2 d S
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 0.0088(6) 0.0110(6) 0.0080(7) 0.000 0.000 0.0026(3)
Cl1 0.0060(6) 0.0081(6) 0.0068(7) 0.000 0.000 -0.0004(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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
Tc1 Tc1 Tc1 90.0 11 3
Tc1 Tc1 Tc1 45.0 11 9
Tc1 Tc1 Tc1 45.0 3 9
Tc1 Tc1 Cl1 128.68(3) 11 3
Tc1 Tc1 Cl1 71.76(5) 3 3
Tc1 Tc1 Cl1 102.74(4) 9 3
Tc1 Tc1 Cl1 128.68(3) 11 3_554
Tc1 Tc1 Cl1 71.76(5) 3 3_554
Tc1 Tc1 Cl1 102.74(4) 9 3_554
Cl1 Tc1 Cl1 91.31(6) 3 3_554
Tc1 Tc1 Cl1 71.55(5) 11 .
Tc1 Tc1 Cl1 128.62(3) 3 .
Tc1 Tc1 Cl1 102.57(4) 9 .
Cl1 Tc1 Cl1 83.24(4) 3 .
Cl1 Tc1 Cl1 154.69(5) 3_554 .
Tc1 Tc1 Cl1 71.55(5) 11 1_554
Tc1 Tc1 Cl1 128.62(3) 3 1_554
Tc1 Tc1 Cl1 102.57(4) 9 1_554
Cl1 Tc1 Cl1 154.69(5) 3 1_554
Cl1 Tc1 Cl1 83.24(4) 3_554 1_554
Cl1 Tc1 Cl1 91.17(6) . 1_554
Tc1 Cl1 Tc1 91.31(6) 11 11_556
Tc1 Cl1 Tc1 102.70(6) 11 1_556
Tc1 Cl1 Tc1 36.69(3) 11_556 1_556
Tc1 Cl1 Tc1 36.69(3) 11 .
Tc1 Cl1 Tc1 102.70(6) 11_556 .
Tc1 Cl1 Tc1 91.17(6) 1_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc1 Tc1 1.5048(11) 11
Tc1 Tc1 1.5048(11) 3
Tc1 Tc1 2.1280(15) 9
Tc1 Cl1 2.3889(12) 3
Tc1 Cl1 2.3889(12) 3_554
Tc1 Cl1 2.3918(13) .
Tc1 Cl1 2.3918(13) 1_554
Cl1 Tc1 2.3889(12) 11
Cl1 Tc1 2.3889(12) 11_556
Cl1 Tc1 2.3918(13) 1_556
