#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/46/2214653.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_2214653
loop_
_publ_author_name
'Lin-Lin Qiu'
'Jun-Shan Sun'
'Ji-Kun Li'
'Ru-Fen Zhang'
_publ_section_title
Di-μ₃-oxo-bis(μ₂-2,3,4,5-tetrafluorobenzoato-κ²O:O')bis(2,3,4,5-tetrafluorobenzoato-κO)tetrakis[dimethyltin(IV)]
_journal_coeditor_code           GG2018
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2035
_journal_page_last               m2036
_journal_paper_doi               10.1107/S1600536807031030
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Sn4 (C H3)8 (C7 H F4 O2)4 O2]'
_chemical_formula_moiety         'C36 H28 F16 O10 Sn4'
_chemical_formula_sum            'C36 H28 F16 O10 Sn4'
_chemical_formula_weight         1399.34
_chemical_name_systematic
;
Di-μ₃-oxo-bis(μ₂-2,3,4,5-tetrafluorobenzoato-κ²O:O')bis(2,3,4,5-
tetrafluorobenzoato-\kO)tetrakis[dimethyltin(IV)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                107.634(15)
_cell_angle_beta                 100.296(16)
_cell_angle_gamma                100.185(16)
_cell_formula_units_Z            1
_cell_length_a                   7.6590(9)
_cell_length_b                   11.1358(13)
_cell_length_c                   14.6746(17)
_cell_measurement_reflns_used    2453
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.67
_cell_measurement_theta_min      2.82
_cell_volume                     1137.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'φ and ω 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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5695
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    2.288
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         2.05
_refine_diff_density_min         -2.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0982P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                2795
_reflns_number_total             3908
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg2018.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2214653
_cod_database_fobs_code          2214653
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Sn Sn1 0.91008(8) 0.35427(5) 0.49974(4) 0.0401(2) Uani d . 1
Sn Sn2 0.95074(8) 0.38429(6) 0.25786(4) 0.0410(2) Uani d . 1
O O1 0.9747(10) 0.5044(6) 0.1239(4) 0.0672(17) Uani d U 1
O O2 1.0227(8) 0.5943(6) 0.2837(4) 0.0514(15) Uani d U 1
O O3 0.9703(8) 0.4488(5) 0.4047(4) 0.0435(13) Uani d U 1
O O4 0.7690(7) 0.1671(5) 0.3715(4) 0.0401(2) Uani d U 1
O O5 0.9078(10) 0.1726(6) 0.2520(5) 0.0646(17) Uani d U 1
F F1 1.1574(10) 0.8538(6) 0.3612(4) 0.083(2) Uani d . 1
F F2 1.2903(10) 1.0721(6) 0.3325(5) 0.093(2) Uani d . 1
F F3 1.3077(12) 1.0710(7) 0.1490(7) 0.116(3) Uani d . 1
F F4 1.1862(14) 0.8501(8) -0.0062(6) 0.122(3) Uani d . 1
F F5 0.6430(12) -0.0636(8) 0.3815(6) 0.113(3) Uani d U 1
F F6 0.5008(9) -0.3119(6) 0.2845(5) 0.0814(19) Uani d . 1
F F7 0.5109(11) -0.4186(6) 0.0952(6) 0.104(3) Uani d . 1
F F8 0.6718(10) -0.2728(7) 0.0024(4) 0.097(2) Uani d . 1
C C1 1.0236(16) 0.6013(10) 0.1976(7) 0.0672(17) Uani d . 1
C C2 1.0997(12) 0.7292(9) 0.1896(6) 0.045(2) Uani d . 1
C C3 1.1112(15) 0.7308(10) 0.0985(8) 0.064(3) Uani d . 1
H H3 1.0701 0.6538 0.0446 0.076 Uiso calc R 1
C C4 1.1825(17) 0.8445(12) 0.0850(9) 0.072(3) Uani d . 1
C C5 1.2464(15) 0.9593(11) 0.1635(11) 0.077(4) Uani d . 1
C C6 1.2274(14) 0.9605(10) 0.2543(8) 0.063(3) Uani d . 1
C C7 1.1614(13) 0.8462(9) 0.2689(7) 0.055(2) Uani d . 1
C C8 1.2081(14) 0.3590(10) 0.2339(8) 0.066(3) Uani d . 1
H H8A 1.3010 0.4031 0.2944 0.099 Uiso calc R 1
H H8B 1.2354 0.3944 0.1845 0.099 Uiso calc R 1
H H8C 1.2048 0.2680 0.2119 0.099 Uiso calc R 1
C C9 0.6708(14) 0.3455(12) 0.1955(8) 0.087(4) Uani d . 1
H H9A 0.6119 0.3854 0.2450 0.130 Uiso calc R 1
H H9B 0.6196 0.2532 0.1699 0.130 Uiso calc R 1
H H9C 0.6521 0.3799 0.1430 0.130 Uiso calc R 1
C C10 1.1306(15) 0.2745(12) 0.5321(8) 0.074(3) Uani d . 1
H H10A 1.2302 0.3099 0.5088 0.110 Uiso calc R 1
H H10B 1.0937 0.1818 0.5000 0.110 Uiso calc R 1
H H10C 1.1692 0.2951 0.6021 0.110 Uiso calc R 1
C C11 0.6381(12) 0.3513(10) 0.5138(7) 0.056(2) Uani d . 1
H H11A 0.5921 0.4102 0.4855 0.085 Uiso calc R 1
H H11B 0.6375 0.3774 0.5823 0.085 Uiso calc R 1
H H11C 0.5618 0.2649 0.4798 0.085 Uiso calc R 1
C C12 0.8051(12) 0.1130(9) 0.2903(7) 0.049(2) Uani d . 1
C C13 0.7312(11) -0.0276(8) 0.2416(6) 0.041(2) Uani d . 1
C C14 0.6521(12) -0.1085(10) 0.2872(6) 0.050(2) Uani d U 1
C C15 0.5775(13) -0.2391(9) 0.2366(8) 0.056(3) Uani d . 1
C C16 0.5824(14) -0.2943(10) 0.1427(7) 0.060(3) Uani d . 1
C C17 0.6605(15) -0.2171(11) 0.0972(7) 0.067(3) Uani d . 1
C C18 0.7351(13) -0.0850(10) 0.1422(7) 0.052(2) Uani d . 1
H H18 0.7863 -0.0356 0.1083 0.063 Uiso calc R 1
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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
O3 Sn1 C10 . . 106.3(3) ?
O3 Sn1 C11 . . 110.2(3) ?
C10 Sn1 C11 . . 142.7(4) yes
O3 Sn1 O3 . 2_766 76.6(2) ?
C10 Sn1 O3 . 2_766 98.8(4) ?
C11 Sn1 O3 . 2_766 96.5(3) ?
O3 Sn1 O4 . . 91.1(2) ?
C10 Sn1 O4 . . 89.5(4) ?
C11 Sn1 O4 . . 82.8(3) ?
O3 Sn1 O4 2_766 . 166.7(2) ?
O3 Sn1 Sn1 . 2_766 39.25(15) ?
C10 Sn1 Sn1 . 2_766 106.0(3) ?
C11 Sn1 Sn1 . 2_766 106.8(3) ?
O3 Sn1 Sn1 2_766 2_766 37.36(13) ?
O4 Sn1 Sn1 . 2_766 130.19(13) ?
O3 Sn2 C9 . . 103.5(4) ?
O3 Sn2 C8 . . 109.1(4) ?
C8 Sn2 C9 . . 146.4(5) yes
O3 Sn2 O2 . . 82.0(2) ?
C9 Sn2 O2 . . 98.5(4) ?
C8 Sn2 O2 . . 93.8(3) ?
O3 Sn2 O5 . . 91.7(2) ?
C9 Sn2 O5 . . 88.4(4) ?
C8 Sn2 O5 . . 82.9(3) ?
O2 Sn2 O5 . . 171.6(2) ?
C1 O2 Sn2 . . 104.4(6) ?
Sn2 O3 Sn1 . . 132.2(3) yes
Sn2 O3 Sn1 . 2_766 124.2(2) yes
Sn1 O3 Sn1 . 2_766 103.4(2) yes
C12 O4 Sn1 . . 132.8(5) ?
C12 O5 Sn2 . . 129.0(6) ?
O1 C1 O2 . . 121.3(9) ?
O1 C1 C2 . . 119.4(9) ?
O2 C1 C2 . . 119.1(9) ?
C3 C2 C7 . . 118.2(8) ?
C3 C2 C1 . . 117.3(8) ?
C7 C2 C1 . . 124.4(8) ?
C2 C3 C4 . . 121.0(10) ?
C2 C3 H3 . . 119.5 ?
C4 C3 H3 . . 119.5 ?
F4 C4 C3 . . 122.2(11) ?
F4 C4 C5 . . 117.1(10) ?
C3 C4 C5 . . 120.7(10) ?
F3 C5 C6 . . 120.3(12) ?
F3 C5 C4 . . 120.3(12) ?
C6 C5 C4 . . 118.9(9) ?
F2 C6 C5 . . 119.8(10) ?
F2 C6 C7 . . 119.4(10) ?
C5 C6 C7 . . 120.4(10) ?
F1 C7 C6 . . 117.1(9) ?
F1 C7 C2 . . 122.5(8) ?
C6 C7 C2 . . 120.4(9) ?
Sn2 C8 H8A . . 109.5 ?
Sn2 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
Sn2 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
Sn2 C9 H9A . . 109.5 ?
Sn2 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
Sn2 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
Sn1 C10 H10A . . 109.5 ?
Sn1 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
Sn1 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
Sn1 C11 H11A . . 109.5 ?
Sn1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
Sn1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
O5 C12 O4 . . 123.3(8) ?
O5 C12 C13 . . 118.5(8) ?
O4 C12 C13 . . 118.1(7) ?
C14 C13 C18 . . 117.6(8) ?
C14 C13 C12 . . 123.6(8) ?
C18 C13 C12 . . 118.8(8) ?
F5 C14 C15 . . 116.6(9) ?
F5 C14 C13 . . 122.2(9) ?
C15 C14 C13 . . 121.2(8) ?
C16 C15 F6 . . 120.2(9) ?
C16 C15 C14 . . 121.5(9) ?
F6 C15 C14 . . 118.4(9) ?
F7 C16 C15 . . 121.0(11) ?
F7 C16 C17 . . 120.8(10) ?
C15 C16 C17 . . 118.2(9) ?
C16 C17 F8 . . 118.8(10) ?
C16 C17 C18 . . 123.8(9) ?
F8 C17 C18 . . 117.4(10) ?
C17 C18 C13 . . 117.8(9) ?
C17 C18 H18 . . 121.1 ?
C13 C18 H18 . . 121.1 ?
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
Sn1 O3 . 2.053(5) yes
Sn1 O3 2_766 2.140(6) yes
Sn1 O4 . 2.270(5) yes
Sn1 C10 . 2.090(9) ?
Sn1 C11 . 2.125(9) ?
Sn2 O2 . 2.202(6) yes
Sn2 O3 . 2.022(5) yes
Sn2 O5 . 2.295(7) yes
Sn2 C8 . 2.115(9) ?
Sn2 C9 . 2.086(10) ?
O1 C1 . 1.216(11) ?
O2 C1 . 1.291(11) ?
O3 Sn1 2_766 2.140(6) no
O4 C12 . 1.265(10) ?
O5 C12 . 1.255(10) ?
F1 C7 . 1.337(11) ?
F2 C6 . 1.350(12) ?
F3 C5 . 1.342(11) ?
F4 C4 . 1.363(12) ?
F5 C14 . 1.341(11) ?
F6 C15 . 1.348(11) ?
F7 C16 . 1.309(12) ?
F8 C17 . 1.366(11) ?
C1 C2 . 1.488(13) ?
C2 C3 . 1.359(12) ?
C2 C7 . 1.394(13) ?
C3 C4 . 1.373(14) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.374(17) ?
C5 C6 . 1.362(15) ?
C6 C7 . 1.378(14) ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 C13 . 1.466(12) ?
C13 C14 . 1.394(12) ?
C13 C18 . 1.412(12) ?
C14 C15 . 1.376(13) ?
C15 C16 . 1.339(14) ?
C16 C17 . 1.361(15) ?
C17 C18 . 1.380(14) ?
C18 H18 . 0.9300 ?
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
C3 H3 O1 2_765 0.93 2.49 3.375(12) 160
C8 H8C F3 1_545 0.96 2.44 3.347(14) 159
C11 H11B F6 2_656 0.96 2.61 3.441(11) 145
