#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/47/2014704.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_2014704
loop_
_publ_author_name
'Villiers, Claude'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;Tri-μ₂-chloro-tetrachloro-μ₃-oxo-hexakis(tetrahydrofuran-κO)dititanium(III)samarium(III):
 a novel trinuclear Sm--Ti mixed species
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m64
_journal_page_last               m66
_journal_paper_doi               10.1107/S0108270104032986
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Sm Ti2 Cl7 O (C4 H8 O)6]'
_chemical_formula_moiety         'C24 H48 Cl7 O7 Sm Ti2'
_chemical_formula_sum            'C24 H48 Cl7 O7 Sm Ti2'
_chemical_formula_weight         942.92
_chemical_name_systematic
;
Tri-μ₂-chloro-tetrachloro-μ₃-oxo-hexakis(tetrahydrofuran-
\kO)dititanium(III)samarium(III)
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.435(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1224(4)
_cell_length_b                   34.3476(16)
_cell_length_c                   10.9696(4)
_cell_measurement_reflns_used    11856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.77
_cell_volume                     3618.2(3)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  'SHELXTL and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'φ scans'
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11856
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.587
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DELABS in PLATON; Spek, 2003)'
_exptl_crystal_colour            'translucent dark pink'
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.952
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3384
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0228
_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)+(0.0144P)²+7.993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                3155
_reflns_number_total             3384
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hj1036.cif
_cod_data_source_block           I
_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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014704
_cod_database_fobs_code          2014704
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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Sm 0.0000 0.317956(5) 0.7500 0.01553(7) Uani d S 1 . . Sm
Ti 0.11227(5) 0.413820(13) 0.67121(4) 0.01413(11) Uani d . 1 . . Ti
Cl1 0.19553(8) 0.30847(2) 0.97409(7) 0.03111(17) Uani d . 1 . . Cl
Cl2 0.18901(7) 0.349295(18) 0.62322(6) 0.02101(14) Uani d . 1 . . Cl
Cl3 0.24466(7) 0.452407(19) 0.57216(6) 0.02106(14) Uani d . 1 . . Cl
Cl4 0.0000 0.46933(2) 0.7500 0.01523(17) Uani d S 1 . . Cl
O1 0.0000 0.38507(7) 0.7500 0.0142(5) Uani d S 1 . . O
O2 -0.1165(2) 0.26149(5) 0.80837(18) 0.0225(4) Uani d . 1 . . O
O3 0.28789(19) 0.41877(5) 0.84123(17) 0.0193(4) Uani d . 1 . . O
O4 -0.04677(19) 0.41585(5) 0.49025(17) 0.0180(4) Uani d . 1 . . O
C1 -0.0463(3) 0.23190(8) 0.9010(3) 0.0292(7) Uani d . 1 . . C
H1A 0.0458 0.2265 0.8957 0.035 Uiso calc R 1 . . H
H1B -0.0377 0.2401 0.9879 0.035 Uiso calc R 1 . . H
C2 -0.1391(4) 0.19659(9) 0.8632(4) 0.0371(8) Uani d . 1 . . C
H2A -0.1247 0.1788 0.9350 0.045 Uiso calc R 1 . . H
H2B -0.1229 0.1829 0.7920 0.045 Uiso calc R 1 . . H
C3 -0.2840(3) 0.21429(9) 0.8244(3) 0.0342(7) Uani d . 1 . . C
H3A -0.3149 0.2182 0.8987 0.041 Uiso calc R 1 . . H
H3B -0.3506 0.1979 0.7629 0.041 Uiso calc R 1 . . H
C4 -0.2658(3) 0.25301(8) 0.7643(3) 0.0287(6) Uani d . 1 . . C
H4A -0.3001 0.2512 0.6713 0.034 Uiso calc R 1 . . H
H4B -0.3168 0.2734 0.7914 0.034 Uiso calc R 1 . . H
C5 0.3867(5) 0.38849(11) 0.8945(4) 0.0646(13) Uani d U 1 . . C
H5A 0.4365 0.3817 0.8351 0.077 Uiso calc R 1 . . H
H5B 0.3391 0.3654 0.9102 0.077 Uiso calc R 1 . . H
C6 0.4859(3) 0.40306(9) 1.0175(3) 0.0275(6) Uani d . 1 . . C
H6A 0.5814 0.3994 1.0187 0.033 Uiso calc R 1 . . H
H6B 0.4727 0.3894 1.0901 0.033 Uiso calc R 1 . . H
C7 0.4529(3) 0.44639(8) 1.0223(3) 0.0241(6) Uani d . 1 . . C
H7A 0.4039 0.4513 1.0838 0.029 Uiso calc R 1 . . H
H7B 0.5373 0.4619 1.0452 0.029 Uiso calc R 1 . . H
C8 0.3613(3) 0.45524(8) 0.8866(3) 0.0215(6) Uani d . 1 . . C
H8A 0.2961 0.4760 0.8861 0.026 Uiso calc R 1 . . H
H8B 0.4170 0.4629 0.8331 0.026 Uiso calc R 1 . . H
C9 -0.1040(3) 0.45283(8) 0.4284(3) 0.0208(6) Uani d . 1 . . C
H9A -0.0295 0.4709 0.4307 0.025 Uiso calc R 1 . . H
H9B -0.1636 0.4647 0.4721 0.025 Uiso calc R 1 . . H
C10 -0.1874(3) 0.44287(8) 0.2900(3) 0.0235(6) Uani d . 1 . . C
H10A -0.1383 0.4510 0.2314 0.028 Uiso calc R 1 . . H
H10B -0.2781 0.4553 0.2652 0.028 Uiso calc R 1 . . H
C11 -0.2017(3) 0.39867(8) 0.2907(3) 0.0263(6) Uani d . 1 . . C
H11A -0.2818 0.3909 0.3155 0.032 Uiso calc R 1 . . H
H11B -0.2098 0.3877 0.2073 0.032 Uiso calc R 1 . . H
C12 -0.0676(3) 0.38654(8) 0.3902(3) 0.0247(6) Uani d . 1 . . C
H12A -0.0758 0.3608 0.4232 0.030 Uiso calc R 1 . . H
H12B 0.0088 0.3866 0.3546 0.030 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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Sm Cl1 . 2_556 165.84(3) yes
Cl2 Sm O1 . . 68.247(12) yes
Cl2 Sm O2 . 2_556 74.03(5) yes
O2 Sm O2 . 2_556 75.77(9) yes
Cl2 Ti Cl4 . . 165.12(3) yes
Cl3 Ti O1 . . 177.10(6) yes
O3 Ti O4 . . 170.97(7) yes
Sm Cl2 Ti . . 86.04(2) yes
Ti Cl4 Ti . 2_556 81.09(3) yes
Sm O1 Ti . . 121.19(6) yes
Ti O1 Ti . 2_556 117.61(12) yes
Ti O1 Sm 2_556 . 121.19(6) ?
O1 Sm O2 . 2_556 142.11(5) ?
O1 Sm O2 . . 142.12(5) ?
O2 Sm O2 2_556 . 75.77(9) ?
O1 Sm Cl1 . 2_556 97.078(17) ?
O2 Sm Cl1 2_556 2_556 86.57(5) ?
O2 Sm Cl1 . 2_556 82.26(5) ?
O1 Sm Cl1 . . 97.081(17) ?
O2 Sm Cl1 2_556 . 82.25(5) ?
O2 Sm Cl1 . . 86.57(5) ?
O2 Sm Cl2 . . 149.34(5) ?
Cl1 Sm Cl2 2_556 . 90.76(2) ?
Cl1 Sm Cl2 . . 94.48(2) ?
O1 Sm Cl2 . 2_556 68.246(12) ?
O2 Sm Cl2 2_556 2_556 149.34(5) ?
O2 Sm Cl2 . 2_556 74.03(5) ?
Cl1 Sm Cl2 2_556 2_556 94.48(2) ?
Cl1 Sm Cl2 . 2_556 90.76(2) ?
Cl2 Sm Cl2 . 2_556 136.49(2) ?
Ti Sm Ti . 2_556 52.697(14) ?
O1 Ti O4 . . 93.23(5) ?
O1 Ti O3 . . 95.52(5) ?
O4 Ti Cl3 . . 85.69(5) ?
O3 Ti Cl3 . . 85.47(5) ?
O1 Ti Cl2 . . 84.51(6) ?
O4 Ti Cl2 . . 91.54(5) ?
O3 Ti Cl2 . . 91.53(5) ?
Cl3 Ti Cl2 . . 98.20(3) ?
O1 Ti Cl4 . . 80.65(6) ?
O4 Ti Cl4 . . 90.29(5) ?
O3 Ti Cl4 . . 88.93(5) ?
Cl3 Ti Cl4 . . 96.66(2) ?
Ti Ti Sm 2_556 . 63.652(7) ?
C1 O2 C4 . . 108.5(2) ?
C1 O2 Sm . . 124.43(16) ?
C4 O2 Sm . . 126.98(15) ?
C5 O3 C8 . . 105.6(2) ?
C5 O3 Ti . . 125.34(19) ?
C8 O3 Ti . . 123.93(15) ?
C12 O4 C9 . . 107.93(19) ?
C12 O4 Ti . . 124.64(16) ?
C9 O4 Ti . . 122.06(15) ?
O2 C1 C2 . . 104.2(2) ?
O2 C1 H1A . . 110.9 ?
C2 C1 H1A . . 110.9 ?
O2 C1 H1B . . 110.9 ?
C2 C1 H1B . . 110.9 ?
H1A C1 H1B . . 108.9 ?
C1 C2 C3 . . 102.5(2) ?
C1 C2 H2A . . 111.3 ?
C3 C2 H2A . . 111.3 ?
C1 C2 H2B . . 111.3 ?
C3 C2 H2B . . 111.3 ?
H2A C2 H2B . . 109.2 ?
C2 C3 C4 . . 103.5(3) ?
C2 C3 H3A . . 111.1 ?
C4 C3 H3A . . 111.1 ?
C2 C3 H3B . . 111.1 ?
C4 C3 H3B . . 111.1 ?
H3A C3 H3B . . 109.0 ?
O2 C4 C3 . . 106.5(2) ?
O2 C4 H4A . . 110.4 ?
C3 C4 H4A . . 110.4 ?
O2 C4 H4B . . 110.4 ?
C3 C4 H4B . . 110.4 ?
H4A C4 H4B . . 108.6 ?
O3 C5 C6 . . 108.0(3) ?
O3 C5 H5A . . 110.1 ?
C6 C5 H5A . . 110.1 ?
O3 C5 H5B . . 110.1 ?
C6 C5 H5B . . 110.1 ?
H5A C5 H5B . . 108.4 ?
C5 C6 C7 . . 105.4(2) ?
C5 C6 H6A . . 110.7 ?
C7 C6 H6A . . 110.7 ?
C5 C6 H6B . . 110.7 ?
C7 C6 H6B . . 110.7 ?
H6A C6 H6B . . 108.8 ?
C8 C7 C6 . . 103.5(2) ?
C8 C7 H7A . . 111.1 ?
C6 C7 H7A . . 111.1 ?
C8 C7 H7B . . 111.1 ?
C6 C7 H7B . . 111.1 ?
H7A C7 H7B . . 109.0 ?
O3 C8 C7 . . 104.5(2) ?
O3 C8 H8A . . 110.9 ?
C7 C8 H8A . . 110.9 ?
O3 C8 H8B . . 110.9 ?
C7 C8 H8B . . 110.9 ?
H8A C8 H8B . . 108.9 ?
O4 C9 C10 . . 106.2(2) ?
O4 C9 H9A . . 110.5 ?
C10 C9 H9A . . 110.5 ?
O4 C9 H9B . . 110.5 ?
C10 C9 H9B . . 110.5 ?
H9A C9 H9B . . 108.7 ?
C9 C10 C11 . . 104.0(2) ?
C9 C10 H10A . . 111.0 ?
C11 C10 H10A . . 111.0 ?
C9 C10 H10B . . 111.0 ?
C11 C10 H10B . . 111.0 ?
H10A C10 H10B . . 109.0 ?
C12 C11 C10 . . 102.3(2) ?
C12 C11 H11A . . 111.3 ?
C10 C11 H11A . . 111.3 ?
C12 C11 H11B . . 111.3 ?
C10 C11 H11B . . 111.3 ?
H11A C11 H11B . . 109.2 ?
O4 C12 C11 . . 103.7(2) ?
O4 C12 H12A . . 111.0 ?
C11 C12 H12A . . 111.0 ?
O4 C12 H12B . . 111.0 ?
C11 C12 H12B . . 111.0 ?
H12A C12 H12B . . 109.0 ?
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
Sm O1 . 2.305(2) yes
Sm O2 2_556 2.4573(18) ?
Sm O2 . 2.4573(18) yes
Sm Cl1 2_556 2.6437(7) ?
Sm Cl1 . 2.6437(7) yes
Sm Cl2 . 2.9045(7) yes
Sm Cl2 2_556 2.9045(7) ?
Sm Ti . 3.6745(5) ?
Sm Ti 2_556 3.6745(5) ?
Ti O1 . 1.9065(13) yes
Ti O3 . 2.1379(18) yes
Ti O4 . 2.1250(18) yes
Ti Cl2 . 2.4599(7) yes
Ti Cl3 . 2.3778(7) yes
Ti Cl4 . 2.5089(7) yes
Ti Ti 2_556 3.2617(9) ?
Cl4 Ti 2_556 2.5088(7) ?
O1 Ti 2_556 1.9064(13) ?
O2 C1 . 1.454(3) ?
O2 C4 . 1.463(3) ?
O3 C5 . 1.433(4) ?
O3 C8 . 1.461(3) ?
O4 C12 . 1.455(3) ?
O4 C9 . 1.470(3) ?
C1 C2 . 1.510(4) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 C3 . 1.519(5) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.521(4) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 C6 . 1.491(5) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 C7 . 1.530(4) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C8 . 1.515(4) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C10 . 1.524(4) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 C11 . 1.525(4) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 C12 . 1.506(4) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1A Cl1 7_557 0.97 2.82 3.651(3) 144
