#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/65/2006556.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_2006556
loop_
_publ_author_name
'Spry, Marcus P'
'Errington, William'
'Willey, Gerald R'
_publ_section_title
;
 Aquatetrachlorotris(tetrahydrofuran-O)thorium(IV)
 Tetrahydrofuran Solvate (1/1)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1388
_journal_page_last               1390
_journal_paper_doi               10.1107/S0108270197008378
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Th Cl4 (C4 H8 O)3 (H2 O)] , C4 H8 O'
_chemical_formula_sum            'C16 H34 Cl4 O5 Th'
_chemical_formula_weight         680.27
_chemical_name_systematic
;
 Aquatetrachlorotris(tetrahydrofuran)thorium(IV). Tetrahydrofuran Solvate.
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 126.8530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.0856(13)
_cell_length_b                   9.7417(4)
_cell_length_c                   21.1140(9)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.75
_cell_volume                     4787.1(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1995)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       'Siemens SMART diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12793
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.698
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_type   'multi-scan SADABS (Sheldrick, 1996a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4697
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_obs          .0239
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0198P)²+4.4670P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0498
_refine_ls_wR_factor_obs         .0461
_reflns_number_observed          3900
_reflns_number_total             4697
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1151.cif
_cod_data_source_block           mps2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0198P)^2^+4.4670P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0198P)^2^+4.4670P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2006556
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_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
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Th1 .139767(6) .303870(15) .008823(8) .01875(5) Uani d . 1 . Th
Cl1 .10669(5) .23933(11) .10058(6) .0294(2) Uani d . 1 . Cl
Cl2 .21108(5) .08546(10) .05319(6) .0276(2) Uani d . 1 . Cl
Cl3 .11599(5) .29079(12) -.13680(6) .0321(2) Uani d . 1 . Cl
Cl4 .12949(5) .57630(11) .02517(7) .0380(3) Uani d . 1 . Cl
O1 .21889(15) .4103(3) .0167(2) .0325(8) Uani d D 1 . O
H1A .229(2) .395(5) -.011(3) .046(16) Uiso d D 1 . H
H1B .237(2) .474(5) .045(3) .08(2) Uiso d D 1 . H
O11 .22696(12) .3545(3) .15345(16) .0298(7) Uani d . 1 . O
C11 .28632(18) .3087(5) .1956(2) .0339(11) Uani d . 1 . C
H11A .3008 .3289 .1645 .041 Uiso calc R 1 . H
H11B .2894 .2087 .2059 .041 Uiso calc R 1 . H
C12 .3200(2) .3878(6) .2725(3) .0629(18) Uani d . 1 . C
H12A .3348 .3251 .3178 .076 Uiso calc R 1 . H
H12B .3529 .4355 .2798 .076 Uiso calc R 1 . H
C13 .2803(2) .4865(7) .2669(3) .0666(19) Uani d . 1 . C
H13A .2874 .4969 .3188 .080 Uiso calc R 1 . H
H13B .2848 .5772 .2501 .080 Uiso calc R 1 . H
C14 .2231(2) .4331(5) .2088(3) .0435(13) Uani d . 1 . C
H14A .1951 .5089 .1812 .052 Uiso calc R 1 . H
H14B .2110 .3735 .2343 .052 Uiso calc R 1 . H
O21 .03345(12) .3619(3) -.08483(16) .0271(7) Uani d . 1 . O
C21 -.01082(19) .3351(5) -.0740(3) .0362(11) Uani d . 1 . C
H21A -.0019 .3834 -.0265 .043 Uiso calc R 1 . H
H21B -.0138 .2355 -.0677 .043 Uiso calc R 1 . H
C22 -.0655(2) .3882(6) -.1473(3) .0469(13) Uani d . 1 . C
H22A -.0844 .3177 -.1894 .056 Uiso calc R 1 . H
H22B -.0926 .4185 -.1363 .056 Uiso calc R 1 . H
C23 -.0456(2) .5066(5) -.1699(3) .0475(14) Uani d . 1 . C
H23A -.0393 .5890 -.1382 .057 Uiso calc R 1 . H
H23B -.0737 .5288 -.2268 .057 Uiso calc R 1 . H
C24 .0097(2) .4560(5) -.1518(3) .0398(12) Uani d . 1 . C
H24A .0028 .4075 -.1980 .048 Uiso calc R 1 . H
H24B .0364 .5333 -.1375 .048 Uiso calc R 1 . H
O31 .07503(12) .0851(3) -.05627(15) .0294(7) Uani d . 1 . O
C31 .0306(2) .0580(5) -.1395(3) .0390(12) Uani d . 1 . C
H31A .0479 .0451 -.1677 .047 Uiso calc R 1 . H
H31B .0034 .1360 -.1641 .047 Uiso calc R 1 . H
C32 .0005(3) -.0676(7) -.1444(3) .079(2) Uani d . 1 . C
H32A -.0399 -.0468 -.1667 .095 Uiso calc R 1 . H
H32B .0008 -.1364 -.1786 .095 Uiso calc R 1 . H
C33 .0306(2) -.1189(6) -.0654(4) .075(2) Uani d . 1 . C
H33A .0397 -.2172 -.0641 .090 Uiso calc R 1 . H
H33B .0059 -.1107 -.0477 .090 Uiso calc R 1 . H
C34 .0827(2) -.0425(4) -.0131(3) .0436(13) Uani d . 1 . C
H34A .1163 -.0949 -.0010 .052 Uiso calc R 1 . H
H34B .0885 -.0215 .0372 .052 Uiso calc R 1 . H
O41 .21392(14) .1141(3) .3954(2) .0458(9) Uani d . 1 . O
C41 .1554(2) .1100(5) .3675(3) .0529(15) Uani d . 1 . C
H41A .1526 .0672 .4076 .063 Uiso calc R 1 . H
H41B .1320 .0556 .3181 .063 Uiso calc R 1 . H
C42 .1346(2) .2535(6) .3526(4) .0575(16) Uani d . 1 . C
H42A .0945 .2599 .3042 .069 Uiso calc R 1 . H
H42B .1367 .2904 .3980 .069 Uiso calc R 1 . H
C43 .1737(2) .3279(5) .3426(4) .0557(16) Uani d . 1 . C
H43A .1785 .4242 .3606 .067 Uiso calc R 1 . H
H43B .1590 .3275 .2864 .067 Uiso calc R 1 . H
C44 .2294(2) .2516(5) .3929(3) .0405(12) Uani d . 1 . C
H44A .2502 .2550 .3691 .049 Uiso calc R 1 . H
H44B .2542 .2914 .4467 .049 Uiso calc R 1 . H
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'
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'
Th Th -7.2400 8.8979 '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_publ_flag
O1 Th1 O21 128.10(10) y
O1 Th1 O11 67.79(10) y
O21 Th1 O11 138.51(9) y
O1 Th1 O31 137.17(10) y
O21 Th1 O31 67.47(9) y
O11 Th1 O31 131.32(9) y
O1 Th1 Cl1 141.02(8) y
O21 Th1 Cl1 79.60(7) y
O11 Th1 Cl1 73.57(7) y
O31 Th1 Cl1 74.59(7) y
O1 Th1 Cl2 79.35(9) y
O21 Th1 Cl2 139.81(7) y
O11 Th1 Cl2 74.77(7) y
O31 Th1 Cl2 72.76(7) y
Cl1 Th1 Cl2 95.57(3) y
O1 Th1 Cl4 75.35(9) y
O21 Th1 Cl4 72.91(7) y
O11 Th1 Cl4 76.62(7) y
O31 Th1 Cl4 139.64(7) y
Cl1 Th1 Cl4 91.29(4) y
Cl2 Th1 Cl4 147.27(3) y
O1 Th1 Cl3 71.72(8) y
O21 Th1 Cl3 76.41(7) y
O11 Th1 Cl3 138.33(7) y
O31 Th1 Cl3 75.73(7) y
Cl1 Th1 Cl3 147.21(3) y
Cl2 Th1 Cl3 88.68(3) y
Cl4 Th1 Cl3 102.52(3) y
C14 O11 C11 107.6(3) ?
C14 O11 Th1 123.7(2) ?
C11 O11 Th1 128.7(2) ?
O11 C11 C12 105.5(4) ?
C13 C12 C11 106.2(4) ?
C14 C13 C12 106.5(5) ?
C13 C14 O11 105.6(4) ?
C21 O21 C24 108.3(3) ?
C21 O21 Th1 127.9(2) ?
C24 O21 Th1 122.6(2) ?
O21 C21 C22 105.4(4) ?
C23 C22 C21 102.8(4) ?
C22 C23 C24 103.2(4) ?
O21 C24 C23 105.4(4) ?
C31 O31 C34 106.9(3) ?
C31 O31 Th1 128.3(2) ?
C34 O31 Th1 124.4(2) ?
O31 C31 C32 107.2(4) ?
C33 C32 C31 106.7(4) ?
C32 C33 C34 109.9(5) ?
C33 C34 O31 105.2(4) ?
C44 O41 C41 109.7(3) ?
O41 C41 C42 107.1(4) ?
C43 C42 C41 104.1(5) ?
C42 C43 C44 104.8(4) ?
O41 C44 C43 105.2(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Th1 O1 . 2.437(3) y
Th1 O21 . 2.541(3) y
Th1 O11 . 2.590(3) y
Th1 O31 . 2.622(3) y
Th1 Cl1 . 2.7038(10) y
Th1 Cl2 . 2.7159(10) y
Th1 Cl4 . 2.7158(11) y
Th1 Cl3 . 2.7198(10) y
O11 C14 . 1.455(5) ?
O11 C11 . 1.459(5) ?
C11 C12 . 1.510(6) ?
C12 C13 . 1.452(7) ?
C13 C14 . 1.446(7) ?
O21 C21 . 1.460(5) ?
O21 C24 . 1.464(5) ?
C21 C22 . 1.497(6) ?
C22 C23 . 1.491(7) ?
C23 C24 . 1.496(7) ?
O31 C31 . 1.451(5) ?
O31 C34 . 1.476(5) ?
C31 C32 . 1.472(7) ?
C32 C33 . 1.430(7) ?
C33 C34 . 1.438(7) ?
O41 C44 . 1.424(5) ?
O41 C41 . 1.429(6) ?
C41 C42 . 1.480(7) ?
C42 C43 . 1.467(7) ?
C43 C44 . 1.496(6) ?
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_publ_flag
O1 Th1 O11 C14 126.1(3) ?
O21 Th1 O11 C14 3.2(4) ?
O31 Th1 O11 C14 -99.8(3) ?
Cl1 Th1 O11 C14 -48.7(3) ?
Cl2 Th1 O11 C14 -149.3(3) ?
Cl4 Th1 O11 C14 46.7(3) ?
Cl3 Th1 O11 C14 140.6(3) ?
O1 Th1 O11 C11 -56.5(3) ?
O21 Th1 O11 C11 -179.5(3) ?
O31 Th1 O11 C11 77.5(4) ?
Cl1 Th1 O11 C11 128.6(3) ?
Cl2 Th1 O11 C11 28.0(3) ?
Cl4 Th1 O11 C11 -136.0(3) ?
Cl3 Th1 O11 C11 -42.1(4) ?
C14 O11 C11 C12 -11.7(5) ?
Th1 O11 C11 C12 170.7(3) ?
O11 C11 C12 C13 -6.7(7) ?
C11 C12 C13 C14 22.7(7) ?
C12 C13 C14 O11 -30.1(7) ?
C11 O11 C14 C13 25.9(6) ?
Th1 O11 C14 C13 -156.3(4) ?
O1 Th1 O21 C21 -157.0(3) ?
O11 Th1 O21 C21 -57.8(4) y
O31 Th1 O21 C21 69.8(3) y
Cl1 Th1 O21 C21 -7.7(3) y
Cl2 Th1 O21 C21 78.6(3) y
Cl4 Th1 O21 C21 -102.3(3) ?
Cl3 Th1 O21 C21 149.8(3) ?
O1 Th1 O21 C24 9.1(3) ?
O11 Th1 O21 C24 108.4(3) ?
O31 Th1 O21 C24 -124.0(3) ?
Cl1 Th1 O21 C24 158.5(3) ?
Cl2 Th1 O21 C24 -115.2(3) ?
Cl4 Th1 O21 C24 63.9(3) ?
Cl3 Th1 O21 C24 -44.0(3) ?
C24 O21 C21 C22 13.1(5) ?
Th1 O21 C21 C22 -179.2(3) ?
O21 C21 C22 C23 -32.1(5) ?
C21 C22 C23 C24 38.6(5) ?
C21 O21 C24 C23 11.2(5) ?
Th1 O21 C24 C23 -157.3(3) ?
C22 C23 C24 O21 -31.1(5) ?
O1 Th1 O31 C31 -70.6(4) ?
O21 Th1 O31 C31 51.7(3) ?
O11 Th1 O31 C31 -172.6(3) ?
Cl1 Th1 O31 C31 136.7(3) ?
Cl2 Th1 O31 C31 -122.3(3) ?
Cl4 Th1 O31 C31 63.4(4) ?
Cl3 Th1 O31 C31 -29.2(3) ?
O1 Th1 O31 C34 101.7(4) ?
O21 Th1 O31 C34 -135.9(4) ?
O11 Th1 O31 C34 -0.3(4) ?
Cl1 Th1 O31 C34 -51.0(3) ?
Cl2 Th1 O31 C34 50.0(3) ?
Cl4 Th1 O31 C34 -124.2(3) ?
Cl3 Th1 O31 C34 143.1(3) ?
C34 O31 C31 C32 16.0(6) ?
Th1 O31 C31 C32 -170.6(4) ?
O31 C31 C32 C33 -5.0(7) ?
C31 C32 C33 C34 -8.3(9) ?
C32 C33 C34 O31 17.9(8) ?
C31 O31 C34 C33 -20.7(6) ?
Th1 O31 C34 C33 165.6(4) ?
C44 O41 C41 C42 -4.6(6) ?
O41 C41 C42 C43 21.8(6) ?
C41 C42 C43 C44 -30.0(6) ?
C41 O41 C44 C43 -14.2(6) ?
C42 C43 C44 O41 27.6(6) ?
