#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/52/2215247.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_2215247
loop_
_publ_author_name
'Wen-Jie Feng'
'Zhan Shu'
'Xin-Jü Ma'
'Zhi-Min Jin '
_publ_section_title
;
 Bis(dimethyloxonium) pentachloridoantimonate(III)
;
_journal_coeditor_code           PV2024
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2411
_journal_page_last               m2411
_journal_paper_doi               10.1107/S1600536807040901
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C2 H7 O)2 [Sb Cl5]'
_chemical_formula_moiety         '2C2 H7 O + , Sb Cl5 2-'
_chemical_formula_sum            'C4 H14 Cl5 O2 Sb'
_chemical_formula_weight         393.16
_chemical_name_systematic
;
Bis(dimethyloxonium) pentachloridoantimonate(III)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5731(15)
_cell_length_b                   11.858(2)
_cell_length_c                   14.899(3)
_cell_measurement_reflns_used    5451
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.2
_cell_volume                     1514.6(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13634
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    2.675
_exptl_absorpt_correction_T_max  0.448
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760.0
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.484
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0289
_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)+(0.0272P)²+1.5075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                1408
_reflns_number_total             1462
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pv2024.cif
_cod_data_source_block           I
_cod_database_code               2215247
_cod_database_fobs_code          2215247
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z+1/2'
'x, -y+1/2, z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z-1/2'
'-x, y-1/2, -z'
'x-1/2, y, -z-1/2'
loop_
_atom_site_type_symbol
_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
Sb Sb1 0.80313(3) 0.7500 0.602413(18) 0.03087(12) Uani d S 1
Cl Cl1 0.81044(10) 0.53013(7) 0.59403(6) 0.0446(2) Uani d . 1
Cl Cl2 0.60634(14) 0.7500 0.48064(8) 0.0487(3) Uani d S 1
Cl Cl3 1.00870(13) 0.7500 0.49238(7) 0.0419(3) Uani d S 1
Cl Cl4 1.06504(14) 0.7500 0.72397(8) 0.0437(3) Uani d S 1
O O1 0.8051(3) 0.4769(3) 0.3795(2) 0.0707(9) Uani d . 1
C C1 0.6423(5) 0.4401(4) 0.3866(3) 0.0746(14) Uani d . 1
H H1C 0.6068 0.4128 0.3288 0.112 Uiso calc R 1
H H1D 0.5779 0.5031 0.4053 0.112 Uiso calc R 1
H H1E 0.6346 0.3800 0.4306 0.112 Uiso calc R 1
C C2 0.8291(5) 0.5704(4) 0.3151(3) 0.0618(11) Uani d . 1
H H2A 0.7672 0.6349 0.3333 0.093 Uiso calc R 1
H H2B 0.7974 0.5463 0.2556 0.093 Uiso calc R 1
H H2C 0.9386 0.5911 0.3142 0.093 Uiso calc R 1
H H1 0.848(5) 0.500(3) 0.441(3) 0.074 Uiso d . 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sb1 0.03218(19) 0.03316(19) 0.02726(19) 0.000 0.00403(11) 0.000
Cl1 0.0512(5) 0.0344(5) 0.0483(5) -0.0028(3) 0.0036(4) 0.0002(4)
Cl2 0.0398(6) 0.0594(7) 0.0470(7) 0.000 -0.0087(5) 0.000
Cl3 0.0392(6) 0.0542(7) 0.0323(6) 0.000 0.0098(5) 0.000
Cl4 0.0496(7) 0.0451(7) 0.0363(6) 0.000 -0.0014(5) 0.000
O1 0.0618(19) 0.086(2) 0.0644(19) -0.0030(15) -0.0056(14) -0.0033(18)
C1 0.052(2) 0.084(3) 0.088(3) -0.019(2) 0.006(2) -0.035(3)
C2 0.081(3) 0.063(3) 0.042(2) 0.007(2) -0.003(2) -0.0039(19)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'
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
Cl3 Sb1 Cl2 . . 89.99(4) yes
Cl3 Sb1 Cl1 . . 87.126(19) yes
Cl2 Sb1 Cl1 . . 88.93(2) yes
Cl3 Sb1 Cl1 . 3_565 87.126(19) ?
Cl2 Sb1 Cl1 . 3_565 88.930(19) ?
Cl1 Sb1 Cl1 . 3_565 173.87(4) ?
Cl3 Sb1 Cl4 . . 81.82(4) yes
Cl2 Sb1 Cl4 . . 171.81(4) yes
Cl1 Sb1 Cl4 . . 90.65(2) yes
Cl1 Sb1 Cl4 3_565 . 90.65(2) ?
C1 O1 C2 . . 113.8(3) yes
C1 O1 H1 . . 111(2) ?
C2 O1 H1 . . 109(2) ?
O1 C1 H1C . . 109.5 ?
O1 C1 H1D . . 109.5 ?
H1C C1 H1D . . 109.5 ?
O1 C1 H1E . . 109.5 ?
H1C C1 H1E . . 109.5 ?
H1D C1 H1E . . 109.5 ?
O1 C2 H2A . . 109.5 ?
O1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
O1 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
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
Sb1 Cl3 . 2.4070(11) yes
Sb1 Cl2 . 2.4775(12) yes
Sb1 Cl1 . 2.6110(10) yes
Sb1 Cl1 3_565 2.6110(10) ?
Sb1 Cl4 . 2.8847(12) yes
O1 C1 . 1.466(5) yes
O1 C2 . 1.480(5) yes
O1 H1 . 1.03(5) ?
C1 H1C . 0.9700 ?
C1 H1D . 0.9700 ?
C1 H1E . 0.9700 ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 H2C . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 Cl1 1.03(5) 2.32(5) 3.258(4) 150(3) yes
