#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:58:48 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329921.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_4329921
loop_
_publ_author_name
'Erik V. Johnstone'
'Frederic Poineau'
'Paul M. Forster'
'Longzou Ma'
'Thomas Hartmann'
'Andrew Cornelius'
'Daniel Antonio'
'Alfred P. Sattelberger'
'Kenneth R. Czerwinski'
_publ_section_title
;
 Technetium Tetrachloride Revisited: A Precursor to Lower-Valent Binary
 Technetium Chlorides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8462
_journal_page_last               8467
_journal_paper_doi               10.1021/ic301011c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'Cl4 Tc'
_chemical_formula_weight         239.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.0111(4)
_cell_length_b                   11.5308(9)
_cell_length_c                   13.9334(10)
_cell_measurement_temperature    100(2)
_cell_volume                     965.76(12)
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15226
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    4.997
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.299
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         1608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0224
_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/[σ²(Fo²)+(0.0228P)²+2.7520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0595
_reflns_number_gt                1476
_reflns_number_total             1608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301011c_si_002.cif
_cod_data_source_block           TcCl4
_cod_database_code               4329921
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-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
Tc1 Tc 0.09853(3) 0.628361(17) 0.178578(14) 0.00751(7) Uani 1 1 d
Cl4 Cl -0.05136(11) 0.74768(5) 0.06990(4) 0.01203(12) Uani 1 1 d
Cl3 Cl 0.24870(10) 0.50924(5) 0.06958(4) 0.01201(12) Uani 1 1 d
Cl1 Cl -0.07530(10) 0.74409(5) 0.30843(4) 0.00953(12) Uani 1 1 d
Cl2 Cl -0.22738(10) 0.51212(5) 0.19162(4) 0.00978(12) 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 0.00472(10) 0.00880(10) 0.00901(10) 0.00000(6) 0.00001(7) -0.00007(6)
Cl4 0.0097(3) 0.0137(3) 0.0126(3) 0.0034(2) -0.00161(19) 0.0010(2)
Cl3 0.0095(3) 0.0140(3) 0.0125(3) -0.0031(2) 0.0014(2) 0.0012(2)
Cl1 0.0064(2) 0.0103(3) 0.0118(3) -0.00179(19) 0.00068(18) -0.00107(19)
Cl2 0.0065(2) 0.0104(2) 0.0125(3) -0.00189(19) 0.00082(18) -0.00091(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Tc Tc -1.4390 0.7593 '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'
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
Cl4 Tc1 Cl3 94.63(2) . .
Cl4 Tc1 Cl1 92.21(2) . 6_656
Cl3 Tc1 Cl1 93.64(2) . 6_656
Cl4 Tc1 Cl2 93.82(2) . .
Cl3 Tc1 Cl2 92.19(2) . .
Cl1 Tc1 Cl2 171.26(2) 6_656 .
Cl4 Tc1 Cl1 89.61(2) . .
Cl3 Tc1 Cl1 174.67(2) . .
Cl1 Tc1 Cl1 89.42(2) 6_656 .
Cl2 Tc1 Cl1 84.29(2) . .
Cl4 Tc1 Cl2 174.66(2) . 6_656
Cl3 Tc1 Cl2 89.60(2) . 6_656
Cl1 Tc1 Cl2 84.26(2) 6_656 6_656
Cl2 Tc1 Cl2 89.27(2) . 6_656
Cl1 Tc1 Cl2 86.37(2) . 6_656
Tc1 Cl1 Tc1 95.80(2) 6_556 .
Tc1 Cl2 Tc1 95.65(2) . 6_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc1 Cl4 2.2355(6) .
Tc1 Cl3 2.2379(6) .
Tc1 Cl1 2.3786(6) 6_656
Tc1 Cl2 2.3806(6) .
Tc1 Cl1 2.4791(6) .
Tc1 Cl2 2.4825(6) 6_656
Cl1 Tc1 2.3786(6) 6_556
Cl2 Tc1 2.4825(6) 6_556
