#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/17/2001709.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_2001709
loop_
_publ_author_name
'Gao, Y.'
'Guery, J.'
'Jacoboni, C.'
_publ_section_title
;
 Structures of [Zr₂F₈(dmso)₄] and [ZrF₄(dmso)(H₂O)₂].2H₂O
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              963
_journal_page_last               965
_journal_paper_doi               10.1107/S0108270192012472
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         'C2 H10 F4 O3 S1 Zr,H4 O2'
_chemical_formula_structural     '[Zr F4 (dmso) (H2O)2 ],2H2O'
_chemical_formula_sum            'C2 H14 F4 O5 S Zr'
_chemical_formula_weight         317.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                99.95(2)
_cell_angle_beta                 98.76(2)
_cell_angle_gamma                108.61(2)
_cell_formula_units_Z            2
_cell_length_a                   7.357(4)
_cell_length_b                   8.318(4)
_cell_length_c                   9.627(5)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     536.2(5)
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'STOE-Siemens AED2'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Fine focus Siemens Mo X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5076
_diffrn_reflns_theta_max         36
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        5.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.8601
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_type   'Gaussian (SHELX76; Sheldrick, 1976)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_description       Prism
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.501
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.21
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.021
_refine_ls_shift/esd_max         0.014
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.021
_reflns_number_observed          4559
_reflns_number_total             4946
_reflns_observed_criterion       I>3.0\s(I)
_cod_data_source_file            du1016.cif
_cod_data_source_block           zrdmsow
_cod_original_cell_volume        536.15
_cod_database_code               2001709
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
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_calc_attached_atom
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_type_symbol
Zr 0.32138(2) 0.18397(2) 0.26166(5) 0.02130(10) Uani ? ? ? ? Zr
S 0.49163(6) 0.86829(5) 0.13942(4) 0.0265(2) Uani ? ? ? ? S
F1 0.4827(2) 0.3406(2) 0.15660(10) 0.0390(9) Uani ? ? ? ? F
F2 0.2888(2) 0.38870(10) 0.39250(10) 0.0407(8) Uani ? ? ? ? F
F3 0.1903(2) -0.00550(10) 0.07800(10) 0.0384(8) Uani ? ? ? ? F
F4 0.1623(2) 0.0409(2) 0.37630(10) 0.0460(10) Uani ? ? ? ? F
O1 0.5011(2) 0.0202(2) 0.26030(10) 0.0356(9) Uani ? ? ? ? O
O2 0.5843(2) 0.2977(2) 0.4437(2) 0.0381(9) Uani ? ? ? ? O
O3 0.0568(2) 0.2259(2) 0.1546(2) 0.0420(10) Uani ? ? ? ? O
O4 0.0636(2) 0.7451(2) 0.4741(2) 0.0390(10) Uani ? ? ? ? O
O5 0.8918(2) 0.4581(2) 0.2272(2) 0.0480(10) Uani ? ? ? ? O
C1 0.6967(3) 0.8153(3) 0.2116(3) 0.050(2) Uani ? ? ? ? C
C2 0.3011(3) 0.6822(3) 0.1562(3) 0.046(2) Uani ? ? ? ? C
H1 0.673(5) 0.790(4) 0.309(4) 0.080(10) Uiso ? ? ? ? H
H2 0.700(5) 0.715(4) 0.139(4) 0.080(10) Uiso ? ? ? ? H
H3 0.812(6) 0.900(5) 0.198(4) 0.100(10) Uiso ? ? ? ? H
H4 0.177(5) 0.697(4) 0.135(3) 0.070(9) Uiso ? ? ? ? H
H5 0.309(4) 0.572(4) 0.095(3) 0.067(9) Uiso ? ? ? ? H
H6 0.329(5) 0.679(4) 0.250(4) 0.070(10) Uiso ? ? ? ? H
H21 0.680(5) 0.268(4) 0.459(3) 0.073(9) Uiso ? ? ? ? H
H22 0.607(5) 0.377(4) 0.494(3) 0.070(10) Uiso ? ? ? ? H
H31 0.002(5) 0.296(4) 0.187(3) 0.080(10) Uiso ? ? ? ? H
H32 -0.012(5) 0.165(4) 0.073(4) 0.090(10) Uiso ? ? ? ? H
H41 -0.010(5) 0.752(4) 0.539(4) 0.080(10) Uiso ? ? ? ? H
H42 0.092(5) 0.829(4) 0.454(4) 0.070(10) Uiso ? ? ? ? H
H51 0.778(5) 0.423(4) 0.219(3) 0.070(10) Uiso ? ? ? ? H
H52 0.923(5) 0.537(5) 0.317(4) 0.090(10) Uiso ? ? ? ? H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zr Zr4+ -2.965 0.560 International_Tables_Vol_IV_Table_2.2B
F F1- 0.014 0.010 International_Tables_Vol_IV_Table_2.2B
S S 0.110 0.124 International_Tables_Vol_IV_Table_2.2B
C C 0.002 0.002 International_Tables_Vol_IV_Table_2.2B
H H 0.0 0.0 International_Tables_Vol_IV_Table_2.2B
O O 0.008 0.006 International_Tables_Vol_IV_Table_2.2B
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -5 1
-1 0 7
5 0 0
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F4 Zr F1 . . . 176.32(5) yes
F4 Zr F3 . . . 91.70(5) yes
F4 Zr F2 . . . 84.50(5) yes
F4 Zr O1 . . . 88.87(6) yes
F4 Zr O3 . . . 90.25(6) yes
F4 Zr O2 . . . 92.60(5) yes
F1 Zr F3 . . . 91.67(5) yes
F1 Zr F2 . . . 91.92(5) yes
F1 Zr O1 . . . 93.39(5) yes
F1 Zr O3 . . . 89.42(6) yes
F1 Zr O2 . . . 85.52(5) yes
F3 Zr F2 . . . 143.02(5) yes
F3 Zr O1 . . . 75.89(5) yes
F3 Zr O3 . . . 71.43(5) yes
F3 Zr O2 . . . 144.27(6) yes
F2 Zr O1 . . . 140.51(4) yes
F2 Zr O3 . . . 71.82(5) yes
F2 Zr O2 . . . 72.71(5) yes
O1 Zr O3 . . . 147.27(5) yes
O1 Zr O2 . . . 68.76(5) yes
O3 Zr O2 . . . 143.95(6) yes
O1 S C2 1_565 . . 105.80(10) yes
O1 S C1 1_565 . . 102.20(10) yes
C2 S C1 . . . 98.40(10) yes
H2 C1 H1 . . . 115(3) no
H3 C1 H1 . . . 125(3) no
H3 C1 H2 . . . 96(3) no
H5 C2 H4 . . . 115(2) no
H6 C2 H4 . . . 109(3) no
H6 C2 H5 . . . 108(2) no
H22 O2 H21 . . . 106(3) no
H32 O3 H31 . . . 108(3) no
H42 O4 H41 . . . 107(4) no
H42 O4 H21 . . . 101(3) no
H42 O4 H52 . . 1_455 116(3) no
H41 O4 H21 . . . 118(2) no
H41 O4 H52 . . 1_455 110(2) no
H21 O4 H52 . . 1_455 106(2) no
H51 O5 H52 . . . 98(3) no
H51 O5 H31 . . 1_655 116(3) no
H52 O5 H31 . . 1_655 124(3) no
O2 H22 F2 . . . 166(3) no
O3 H31 O5 . . . 168(4) no
O3 H32 F3 . . 1_455 170(3) no
O4 H42 F4 . . 2_665 174(4) no
O5 H51 F1 . . 1_565 169(4) no
O5 H52 O4 . . 1_655 160(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr F4 . . 1.9900(10) yes
Zr F1 . . 1.9910(10) yes
Zr F3 . . 2.0220(10) yes
Zr F2 . . 2.0390(10) yes
Zr O1 . . 2.180(2) yes
Zr O3 . . 2.218(2) yes
Zr O2 . . 2.2210(10) yes
S O1 . 1_565 1.5390(10) yes
S C2 . . 1.777(2) yes
S C1 . . 1.779(3) yes
C1 H1 . . 1.02(3) no
C1 H2 . . 1.00(3) no
C1 H3 . . 0.96(4) no
C2 H4 . . 0.96(3) no
C2 H5 . . 1.02(3) no
C2 H6 . . 0.91(3) no
F1 H51 . . 2.01(3) no
F2 H22 . . 1.91(3) no
F3 H32 . 2_555 1.80(3) no
F4 H42 . 1_545 1.98(4) no
O2 H22 . . 0.70(3) no
O2 H21 . . 0.82(4) no
O3 H32 . . 0.84(3) no
O3 H31 . . 0.85(4) no
O4 H42 . . 0.73(4) no
O4 H41 . . 0.89(4) no
O4 H21 . . 1.94(4) no
O4 H52 . 1_455 1.96(3) no
O5 H51 . . 0.78(3) no
O5 H52 . . 0.94(3) no
O5 H31 1_655 . 1.80(4) no
