#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/59/2005911.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005911
loop_
_publ_author_name
'Rabinovich, D.'
'Schimek, G. L.'
'Pennington, W. T.'
'Nielsen, J. B.'
'Abney, K. D.'
_publ_contact_author
;
        Dr. George L. Schimek
        379 H.L. Hunter Chem. Lab.
        Clemson University
        Clemson, South Carolina 29634-1905
        USA
;
_publ_section_title
Tetrachlorobis(N,N,N',N'-tetramethylethylenediamine-N,N')thorium(IV)
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              191
_journal_page_last               193
_journal_paper_doi               10.1107/S0108270196012796
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         '[Th1 Cl4 (C6 H16 N2)2]'
_chemical_formula_sum            'C12 H32 Cl4 N4 Th'
_chemical_formula_weight         606.3
_chemical_name_systematic
Bis[1,2-bis(dimethylamino)ethane]tetrachlorothorium(IV)
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           'International Tables (Cromer & Waber, 1974)'
_audit_creation_method           'manual editting of form.cif'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.098(3)
_cell_length_b                   13.211(3)
_cell_length_c                   12.578(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    150
_cell_measurement_theta_max      13.96
_cell_measurement_theta_min      10.30
_cell_volume                     2176.5(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1988)
;
_computing_data_reduction
'TEXSAN  (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_structure_refinement  'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device       'Rigaku AFC7R diffractometer'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4403
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        1.4
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.342
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_type
'empirical via \y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.75
_refine_diff_density_min         -2.29
_refine_ls_extinction_coef       0.000131(8)
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_obs   1.65
_refine_ls_hydrogen_treatment
'H atoms riding, overall U for H atoms refined: 0.078(7)\%A^2^'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_obs          0.0313
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F)+0.008F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0360
_refine_ls_wR_factor_obs         0.0356
_reflns_number_observed          3586
_reflns_number_total             3828
_reflns_observed_criterion       F>4\s(F)
_cod_data_source_file            bk1289.cif
_cod_data_source_block           globalBD0625
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F)+0.008F^2^]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(F)+0.008F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C12 H32 N4 Cl4 Th1'
_cod_database_code               2005911
loop_
_symmetry_equiv_pos_as_xyz
'  +x, +y,   +z'
'  -x+0.5,   -y,   +z+0.5'
'  -x,  y+0.5,  -z+0.5'
'  +x+0.5,   -y+0.5,  -z'
loop_
_atom_site_label
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
Th(1) a 0.7155(1) 0.2397(1) 0.2341(1) 0.026(1) Uani d .
Cl(1) a 0.6234(2) 0.0580(2) 0.2380(2) 0.048(1) Uani d .
Cl(2) a 0.8019(2) 0.1866(2) 0.4200(2) 0.041(1) Uani d .
Cl(3) a 0.8612(2) 0.3630(2) 0.1563(3) 0.059(1) Uani d .
Cl(4) a 0.5794(2) 0.3517(2) 0.1265(2) 0.047(1) Uani d .
N(1) a 0.7181(8) 0.1715(6) 0.0233(6) 0.053(3) Uani d .
N(2) a 0.8814(7) 0.1108(6) 0.1864(7) 0.051(3) Uani d .
N(3) a 0.7121(7) 0.4183(5) 0.3568(6) 0.040(3) Uani d .
N(4) a 0.5477(5) 0.2544(6) 0.3715(5) 0.038(2) Uani d .
C(1) a 0.6146(11) 0.1343(9) -0.0123(9) 0.078(6) Uani d .
C(2) a 0.7512(11) 0.2504(8) -0.0528(7) 0.082(5) Uani d .
C(3) a 0.7899(11) 0.0849(7) 0.0145(8) 0.062(4) Uani d .
C(4) a 0.8903(10) 0.1054(8) 0.0675(9) 0.059(4) Uani d .
C(5) a 0.9813(7) 0.1518(8) 0.2263(11) 0.073(5) Uani d .
C(6) a 0.8712(8) 0.0107(7) 0.2303(9) 0.063(4) Uani d .
C(7) a 0.6864(9) 0.5093(7) 0.2934(9) 0.066(4) Uani d .
C(8) a 0.8095(8) 0.4403(7) 0.4103(9) 0.055(4) Uani d .
C(9) a 0.6346(10) 0.4028(9) 0.4455(10) 0.062(5) Uani d .
C(10) a 0.5396(10) 0.3609(8) 0.4099(10) 0.061(5) Uani d .
C(11) a 0.5524(9) 0.1858(7) 0.4634(9) 0.056(4) Uani d .
C(12) a 0.4483(7) 0.2344(9) 0.3197(8) 0.064(4) Uani d .
H(1A) a 0.6158 0.1183 -0.0866 0.078(7) Uovl calc UR
H(1B) a 0.5639 0.1852 0.0011 0.078(7) Uovl calc UR
H(1C) a 0.5969 0.0750 0.0279 0.078(7) Uovl calc UR
H(2A) a 0.7015 0.3040 -0.0529 0.078(7) Uovl calc UR
H(2B) a 0.7578 0.2230 -0.1231 0.078(7) Uovl calc UR
H(2C) a 0.8163 0.2764 -0.0314 0.078(7) Uovl calc UR
H(3A) a 0.8007 0.0690 -0.0591 0.078(7) Uovl calc UR
H(3B) a 0.7591 0.0271 0.0477 0.078(7) Uovl calc UR
H(4A) a 0.9376 0.0526 0.0494 0.078(7) Uovl calc UR
H(4B) a 0.9171 0.1681 0.0407 0.078(7) Uovl calc UR
H(5A) a 1.0348 0.1344 0.1774 0.078(7) Uovl calc UR
H(5B) a 0.9959 0.1236 0.2949 0.078(7) Uovl calc UR
H(5C) a 0.9774 0.2241 0.2334 0.078(7) Uovl calc UR
H(6A) a 0.8315 -0.0325 0.1832 0.078(7) Uovl calc UR
H(6B) a 0.8346 0.0134 0.2983 0.078(7) Uovl calc UR
H(6C) a 0.9359 -0.0228 0.2437 0.078(7) Uovl calc UR
H(7A) a 0.6882 0.5673 0.3392 0.078(7) Uovl calc UR
H(7B) a 0.6192 0.5044 0.2633 0.078(7) Uovl calc UR
H(7C) a 0.7359 0.5170 0.2375 0.078(7) Uovl calc UR
H(8A) a 0.8632 0.4559 0.3576 0.078(7) Uovl calc UR
H(8B) a 0.8351 0.3846 0.4512 0.078(7) Uovl calc UR
H(8C) a 0.8073 0.5001 0.4559 0.078(7) Uovl calc UR
H(9A) a 0.6228 0.4659 0.4812 0.078(7) Uovl calc UR
H(9B) a 0.6630 0.3565 0.4963 0.078(7) Uovl calc UR
H(10A) a 0.4907 0.3636 0.4667 0.078(7) Uovl calc UR
H(10B) a 0.5148 0.4026 0.3529 0.078(7) Uovl calc UR
H(11A) a 0.4933 0.1848 0.5054 0.078(7) Uovl calc UR
H(11B) a 0.6128 0.2037 0.5046 0.078(7) Uovl calc UR
H(11C) a 0.5663 0.1184 0.4329 0.078(7) Uovl calc UR
H(12A) a 0.4467 0.2695 0.2519 0.078(7) Uovl calc UR
H(12B) a 0.3928 0.2625 0.3633 0.078(7) Uovl calc UR
H(12C) a 0.4379 0.1648 0.3105 0.078(7) Uovl calc UR
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 1 3
-3 -1 1
-1 -1 3
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl(1) Th(1) Cl(2) 86.50(10) yes
Cl(1) Th(1) Cl(3) 149.90(10) yes
Cl(1) Th(1) Cl(4) 101.70(10) yes
Cl(2) Th(1) Cl(3) 100.10(10) yes
Cl(2) Th(1) Cl(4) 149.50(10) yes
Cl(3) Th(1) Cl(4) 87.40(10) yes
Cl(1) Th(1) N(1) 74.6(2) yes
Cl(1) Th(1) N(2) 79.1(2) yes
Cl(1) Th(1) N(3) 136.9(2) yes
Cl(1) Th(1) N(4) 72.5(2) yes
Cl(2) Th(1) N(1) 137.2(2) yes
Cl(2) Th(1) N(2) 72.8(2) yes
Cl(2) Th(1) N(3) 75.5(2) yes
Cl(2) Th(1) N(4) 79.10(10) yes
Cl(3) Th(1) N(1) 80.9(2) yes
Cl(3) Th(1) N(2) 75.1(2) yes
Cl(3) Th(1) N(3) 72.8(2) yes
Cl(3) Th(1) N(4) 137.5(2) yes
Cl(4) Th(1) N(1) 73.0(2) yes
Cl(4) Th(1) N(2) 137.4(2) yes
Cl(4) Th(1) N(3) 78.7(2) yes
Cl(4) Th(1) N(4) 75.6(2) yes
N(1) Th(1) N(2) 66.2(3) yes
N(1) Th(1) N(3) 142.0(2) yes
N(1) Th(1) N(4) 128.0(3) yes
N(2) Th(1) N(3) 129.3(3) yes
N(2) Th(1) N(4) 140.9(2) yes
N(3) Th(1) N(4) 65.9(2) yes
Th(1) N(1) C(1) 112.0(6) ?
Th(1) N(1) C(2) 112.9(5) ?
C(1) N(1) C(2) 107.5(8) ?
Th(1) N(1) C(3) 109.0(6) ?
C(1) N(1) C(3) 107.2(8) ?
C(2) N(1) C(3) 107.9(9) ?
Th(1) N(2) C(4) 107.5(6) ?
Th(1) N(2) C(5) 112.4(6) ?
C(4) N(2) C(5) 106.3(9) ?
Th(1) N(2) C(6) 113.7(6) ?
C(4) N(2) C(6) 110.2(8) ?
C(5) N(2) C(6) 106.5(8) ?
Th(1) N(3) C(7) 112.8(6) ?
Th(1) N(3) C(8) 113.7(6) ?
C(7) N(3) C(8) 106.4(7) ?
Th(1) N(3) C(9) 107.4(6) ?
C(7) N(3) C(9) 110.6(8) ?
C(8) N(3) C(9) 105.6(8) ?
Th(1) N(4) C(10) 108.7(6) ?
Th(1) N(4) C(11) 114.2(6) ?
C(10) N(4) C(11) 109.3(8) ?
Th(1) N(4) C(12) 113.9(5) ?
C(10) N(4) C(12) 104.4(8) ?
C(11) N(4) C(12) 105.8(8) ?
N(1) C(3) C(4) 112.6(8) ?
N(2) C(4) C(3) 112.5(9) ?
N(3) C(9) C(10) 113.7(10) ?
H(9A) C(9) C(10) 110.0(7) ?
H(9B) C(9) C(10) 107.4(7) ?
N(4) C(10) C(9) 113.8(10) ?
N(1) C(1) H(1A) 110.2(5) ?
N(1) C(1) H(1B) 109.9(5) ?
H(1A) C(1) H(1B) 109.70(10) ?
N(1) C(1) H(1C) 109.0(5) ?
H(1A) C(1) H(1C) 109.70(10) ?
H(1B) C(1) H(1C) 108.20(10) ?
N(1) C(2) H(2A) 108.8(6) ?
N(1) C(2) H(2B) 110.9(5) ?
H(2A) C(2) H(2B) 109.70(10) ?
N(1) C(2) H(2C) 109.4(6) ?
H(2A) C(2) H(2C) 109.70(10) ?
H(2B) C(2) H(2C) 108.30(10) ?
N(1) C(3) H(3A) 109.6(5) ?
N(1) C(3) H(3B) 108.3(6) ?
H(3A) C(3) H(3B) 107.90(10) ?
H(3A) C(3) C(4) 109.8(6) ?
H(3B) C(3) C(4) 108.6(6) ?
N(2) C(4) H(4A) 108.7(6) ?
C(3) C(4) H(4A) 109.3(6) ?
N(2) C(4) H(4B) 109.7(5) ?
C(3) C(4) H(4B) 108.6(6) ?
H(4A) C(4) H(4B) 107.90(10) ?
N(2) C(5) H(5A) 109.6(6) ?
N(2) C(5) H(5B) 109.4(6) ?
H(5A) C(5) H(5B) 109.70(10) ?
N(2) C(5) H(5C) 110.1(5) ?
H(5A) C(5) H(5C) 109.70(10) ?
H(5B) C(5) H(5C) 108.30(10) ?
N(2) C(6) H(6A) 110.7(6) ?
N(2) C(6) H(6B) 110.3(6) ?
H(6A) C(6) H(6B) 106.90(10) ?
N(2) C(6) H(6C) 113.9(6) ?
H(6A) C(6) H(6C) 107.80(10) ?
H(6B) C(6) H(6C) 107.00(10) ?
N(3) C(7) H(7A) 108.6(5) ?
N(3) C(7) H(7B) 111.5(6) ?
H(7A) C(7) H(7B) 108.20(10) ?
N(3) C(7) H(7C) 109.1(6) ?
H(7A) C(7) H(7C) 109.70(10) ?
H(7B) C(7) H(7C) 109.70(10) ?
N(3) C(8) H(8A) 110.6(5) ?
N(3) C(8) H(8B) 113.4(5) ?
H(8A) C(8) H(8B) 105.60(10) ?
N(3) C(8) H(8C) 113.8(5) ?
H(8A) C(8) H(8C) 104.40(10) ?
H(8B) C(8) H(8C) 108.30(10) ?
N(3) C(9) H(9A) 109.4(5) ?
N(3) C(9) H(9B) 108.3(5) ?
H(9A) C(9) H(9B) 107.80(10) ?
N(4) C(10) H(10A) 108.8(6) ?
C(9) C(10) H(10A) 109.4(7) ?
N(4) C(10) H(10B) 108.9(6) ?
C(9) C(10) H(10B) 107.8(7) ?
H(10A) C(10) H(10B) 108.00(10) ?
N(4) C(11) H(11A) 114.7(5) ?
N(4) C(11) H(11B) 107.6(5) ?
H(11A) C(11) H(11B) 112.00(10) ?
N(4) C(11) H(11C) 105.0(5) ?
H(11A) C(11) H(11C) 111.00(10) ?
H(11B) C(11) H(11C) 106.00(10) ?
N(4) C(12) H(12A) 108.7(5) ?
N(4) C(12) H(12B) 109.7(5) ?
H(12A) C(12) H(12B) 107.10(10) ?
N(4) C(12) H(12C) 111.0(5) ?
H(12A) C(12) H(12C) 110.90(10) ?
H(12B) C(12) H(12C) 109.40(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Th(1) Cl(1) 2.688(2) yes
Th(1) Cl(2) 2.690(2) yes
Th(1) Cl(3) 2.692(3) yes
Th(1) Cl(4) 2.683(3) yes
Th(1) N(1) 2.800(7) yes
Th(1) N(2) 2.825(9) yes
Th(1) N(3) 2.820(7) yes
Th(1) N(4) 2.803(7) yes
N(1) C(1) 1.510(17) ?
N(1) C(2) 1.480(13) ?
N(1) C(3) 1.485(15) ?
N(2) C(4) 1.501(15) ?
N(2) C(5) 1.504(14) ?
N(2) C(6) 1.440(13) ?
N(3) C(7) 1.481(12) ?
N(3) C(8) 1.471(14) ?
N(3) C(9) 1.523(15) ?
N(4) C(10) 1.491(13) ?
N(4) C(11) 1.470(13) ?
N(4) C(12) 1.479(12) ?
C(3) C(4) 1.500(18) ?
C(9) C(10) 1.433(18) ?
C(1) H(1A) 0.959 ?
C(1) H(1B) 0.960 ?
C(1) H(1C) 0.961 ?
C(2) H(2A) 0.961 ?
C(2) H(2B) 0.959 ?
C(2) H(2C) 0.959 ?
C(3) H(3A) 0.960 ?
C(3) H(3B) 0.960 ?
C(4) H(4A) 0.959 ?
C(4) H(4B) 0.960 ?
C(5) H(5A) 0.960 ?
C(5) H(5B) 0.959 ?
C(5) H(5C) 0.960 ?
C(6) H(6A) 0.973 ?
C(6) H(6B) 0.980 ?
C(6) H(6C) 0.970 ?
C(7) H(7A) 0.960 ?
C(7) H(7B) 0.960 ?
C(7) H(7C) 0.960 ?
C(8) H(8A) 0.988 ?
C(8) H(8B) 0.958 ?
C(8) H(8C) 0.975 ?
C(9) H(9A) 0.960 ?
C(9) H(9B) 0.959 ?
C(10) H(10A) 0.960 ?
C(10) H(10B) 0.960 ?
C(11) H(11A) 0.937 ?
C(11) H(11B) 0.975 ?
C(11) H(11C) 0.987 ?
C(12) H(12A) 0.971 ?
C(12) H(12B) 0.983 ?
C(12) H(12C) 0.937 ?
