#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:47:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179394 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/91/4329156.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_4329156
loop_
_publ_author_name
'Frederic Poineau'
'Erik V. Johnstone'
'Philippe F. Weck'
'Paul M. Forster'
'Eunja Kim'
'Kenneth R. Czerwinski'
'Alfred P. Sattelberger'
_publ_section_title
;
 β-Technetium Trichloride: Formation, Structure, and First-Principles
 Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4915
_journal_page_last               4917
_journal_paper_doi               10.1021/ic300612k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'Cl3 Tc'
_chemical_formula_weight         204.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.687(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.986(3)
_cell_length_b                   9.725(5)
_cell_length_c                   6.194(3)
_cell_measurement_temperature    100(2)
_cell_volume                     341.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            447
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    6.270
_exptl_absorpt_correction_T_max  0.746513
_exptl_absorpt_correction_T_min  0.515241
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.974
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.321
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.524
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0703
_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)+(0.0922P)²+13.8396P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                432
_reflns_number_total             447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300612k_si_002.cif
_cod_data_source_block           beta-TcCl3_0m
_cod_database_code               4329156
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tc1 Tc 0.0000 0.14708(13) 0.0000 0.0253(5) Uani 1 2 d S
Cl1 Cl 0.2495(6) 0.0000 0.2624(6) 0.0239(7) Uani 1 2 d S
Cl2 Cl 0.7409(4) 0.1691(2) 0.2247(4) 0.0235(6) Uani 1 1 d .
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 0.0235(7) 0.0376(8) 0.0133(6) 0.000 0.0039(4) 0.000
Cl1 0.0223(14) 0.0276(15) 0.0214(15) 0.000 0.0063(11) 0.000
Cl2 0.0221(11) 0.0307(12) 0.0178(11) 0.0007(8) 0.0066(8) 0.0015(8)
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
Cl1 Tc1 Cl1 103.71(12) 5 .
Cl1 Tc1 Cl2 92.25(10) 5 2_655
Cl1 Tc1 Cl2 94.07(10) . 2_655
Cl1 Tc1 Cl2 94.07(10) 5 1_455
Cl1 Tc1 Cl2 92.25(10) . 1_455
Cl2 Tc1 Cl2 169.75(13) 2_655 1_455
Cl1 Tc1 Cl2 170.25(9) 5 8_455
Cl1 Tc1 Cl2 85.50(8) . 8_455
Cl2 Tc1 Cl2 83.78(9) 2_655 8_455
Cl2 Tc1 Cl2 88.69(8) 1_455 8_455
Cl1 Tc1 Cl2 85.50(8) 5 7
Cl1 Tc1 Cl2 170.25(9) . 7
Cl2 Tc1 Cl2 88.69(8) 2_655 7
Cl2 Tc1 Cl2 83.78(9) 1_455 7
Cl2 Tc1 Cl2 85.51(12) 8_455 7
Cl1 Tc1 Tc1 51.85(6) 5 5
Cl1 Tc1 Tc1 51.85(6) . 5
Cl2 Tc1 Tc1 95.13(6) 2_655 5
Cl2 Tc1 Tc1 95.13(6) 1_455 5
Cl2 Tc1 Tc1 137.25(6) 8_455 5
Cl2 Tc1 Tc1 137.24(6) 7 5
Tc1 Cl1 Tc1 76.29(12) . 5
Tc1 Cl2 Tc1 96.22(9) 1_655 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc1 Cl1 2.316(3) 5
Tc1 Cl1 2.316(3) .
Tc1 Cl2 2.403(2) 2_655
Tc1 Cl2 2.403(2) 1_455
Tc1 Cl2 2.434(3) 8_455
Tc1 Cl2 2.434(3) 7
Tc1 Tc1 2.861(3) 5
Cl1 Tc1 2.316(3) 5
Cl2 Tc1 2.403(2) 1_655
Cl2 Tc1 2.434(3) 7
