#------------------------------------------------------------------------------
#$Date: 2024-03-04 22:16:32 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290174 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/49/7714975.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714975
loop_
_publ_author_name
'Ren, Liying'
'Yin, Zeqiao'
'Wang, Shiyi'
'Lin, Zhengyan'
'Cao, Liling'
'Dong, Xuehua'
'Huang, Ling'
'Zhou, Yuqiao'
'Gao, Daojiang'
'Zou, Guohong'
_publ_section_title
;
 Na₄Sn₄(C₂O₄)₃F₆
 and NaSnC₂O₄F·H₂O: two tin(II)
 fluoride oxalates display large birefringence.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2619
_journal_page_last               2625
_journal_paper_doi               10.1039/d3dt04286c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C2 H2 F Na O5 Sn'
_chemical_formula_sum            'C2 H2 F Na O5 Sn'
_chemical_formula_weight         266.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-24 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                111.020(5)
_cell_angle_beta                 107.986(4)
_cell_angle_gamma                96.873(4)
_cell_formula_units_Z            2
_cell_length_a                   5.9880(3)
_cell_length_b                   7.2468(4)
_cell_length_c                   8.2925(4)
_cell_measurement_reflns_used    2165
_cell_measurement_temperature    299.69(10)
_cell_measurement_theta_max      29.7570
_cell_measurement_theta_min      2.8300
_cell_volume                     308.54(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.69(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     48.00  75.00   0.50    0.05    --    4.52  37.00   0.00   54
  2  ω    -50.00  19.00   0.50    0.05    --    4.52 -57.00-180.00  138
  3  ω    -21.00  11.00   0.50    0.05    --   -5.62 -99.00-150.00   64
  4  ω    -21.00  12.00   0.50    0.05    --   -5.62 -99.00   0.00   66
  5  ω    -78.00  -7.00   0.50    0.05    --   -5.62  -6.00  -0.00  142
  6  ω    -18.00  14.00   0.50    0.05    --   -5.62 -99.00 150.00   64
  7  ω    -19.00  67.00   0.50    0.05    --   -5.62   6.00 175.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1191137000
_diffrn_orient_matrix_UB_12      0.0101528000
_diffrn_orient_matrix_UB_13      -0.0003697000
_diffrn_orient_matrix_UB_21      -0.0022345000
_diffrn_orient_matrix_UB_22      0.0940078000
_diffrn_orient_matrix_UB_23      -0.0080705000
_diffrn_orient_matrix_UB_31      0.0493678000
_diffrn_orient_matrix_UB_32      0.0533678000
_diffrn_orient_matrix_UB_33      0.0987124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3829
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_min         2.844
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.871
_exptl_crystal_description       block
_exptl_crystal_F_000             248
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0270
_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)+(0.0315P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1380
_reflns_number_total             1504
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt04286c2.cif
_cod_data_source_block           8rly_auto
_cod_depositor_comments
'Adding full bibliography for 7714974--7714975.cif.'
_cod_original_cell_volume        308.53(3)
_cod_database_code               7714975
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.660
_oxdiff_exptl_absorpt_empirical_full_min 0.621
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 1.08082(4) 0.73359(3) 0.95651(3) 0.02332(10) Uani 1 1 d . . . . .
Na1 Na 0.9074(3) 0.2384(2) 0.5096(2) 0.0289(3) Uani 1 1 d . . . . .
F1 F 0.9720(4) 0.4253(3) 0.8203(3) 0.0281(5) Uani 1 1 d . . . . .
O1 O 0.8639(5) 0.7385(4) 0.6887(3) 0.0252(5) Uani 1 1 d . . . . .
O2 O 0.4999(5) 0.7417(4) 0.5116(4) 0.0299(6) Uani 1 1 d . . . . .
O3 O 0.6842(5) 0.7004(4) 0.9355(3) 0.0297(6) Uani 1 1 d . . . . .
O4 O 0.3099(5) 0.6682(5) 0.7450(4) 0.0341(6) Uani 1 1 d . . . . .
O5 O 0.7518(6) -0.1233(5) 0.3303(4) 0.0333(7) Uani 1 1 d . . . . .
C1 C 0.5316(7) 0.6951(5) 0.7879(5) 0.0239(7) Uani 1 1 d . . . . .
C2 C 0.6369(6) 0.7276(5) 0.6482(5) 0.0212(7) Uani 1 1 d . . . . .
H5A H 0.702(10) -0.168(8) 0.228(8) 0.050(17) Uiso 1 1 d . . . . .
H5B H 0.656(12) -0.162(10) 0.364(9) 0.07(2) Uiso 1 1 d . . . . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Sn1 O1 86.59(9) . . ?
F1 Sn1 O3 83.50(10) . . ?
F1 Sn1 O4 78.50(9) . 1_655 ?
O1 Sn1 O3 72.33(9) . . ?
O1 Sn1 O4 69.91(9) . 1_655 ?
O3 Sn1 O4 138.82(9) . 1_655 ?
Na1 Na1 Na1 144.31(8) 2_756 2_766 ?
F1 Na1 Na1 86.78(8) . 2_766 ?
F1 Na1 Na1 105.30(8) . 2_756 ?
F1 Na1 O1 133.55(11) . 2_766 ?
F1 Na1 O2 78.67(10) . 2_666 ?
F1 Na1 O4 123.32(11) . 2_666 ?
F1 Na1 O5 78.66(10) . 2_756 ?
F1 Na1 O5 127.91(11) . . ?
O1 Na1 Na1 61.20(7) 2_766 2_766 ?
O1 Na1 Na1 87.82(8) 2_766 2_756 ?
O1 Na1 O4 66.23(9) 2_766 2_666 ?
O1 Na1 O5 85.60(11) 2_766 2_756 ?
O2 Na1 Na1 95.21(9) 2_666 2_766 ?
O2 Na1 Na1 119.86(10) 2_666 2_756 ?
O2 Na1 O1 132.82(10) 2_666 2_766 ?
O2 Na1 O4 66.87(9) 2_666 2_666 ?
O2 Na1 O5 140.46(11) 2_666 2_756 ?
O4 Na1 Na1 55.06(8) 2_666 2_766 ?
O4 Na1 Na1 130.53(10) 2_666 2_756 ?
O4 Na1 O5 151.56(12) 2_666 2_756 ?
O5 Na1 Na1 39.35(8) 2_756 2_756 ?
O5 Na1 Na1 115.34(10) 2_756 2_766 ?
O5 Na1 Na1 145.02(11) . 2_766 ?
O5 Na1 Na1 41.13(9) . 2_756 ?
O5 Na1 O1 91.18(11) . 2_766 ?
O5 Na1 O2 88.54(11) . 2_666 ?
O5 Na1 O4 95.66(12) . 2_666 ?
O5 Na1 O5 80.48(12) . 2_756 ?
Sn1 F1 Na1 125.40(10) . . ?
Sn1 O1 Na1 115.15(11) . 2_766 ?
C2 O1 Sn1 119.0(2) . . ?
C2 O1 Na1 125.8(2) . 2_766 ?
C2 O2 Na1 118.8(2) . 2_666 ?
C1 O3 Sn1 116.5(2) . . ?
Na1 O4 Sn1 105.65(11) 2_666 1_455 ?
C1 O4 Sn1 128.1(2) . 1_455 ?
C1 O4 Na1 116.2(2) . 2_666 ?
Na1 O5 Na1 99.52(12) . 2_756 ?
Na1 O5 H5A 121(4) . . ?
Na1 O5 H5A 118(5) 2_756 . ?
Na1 O5 H5B 108(5) . . ?
Na1 O5 H5B 98(5) 2_756 . ?
H5A O5 H5B 108(6) . . ?
O3 C1 C2 116.0(3) . . ?
O4 C1 O3 126.8(3) . . ?
O4 C1 C2 117.2(3) . . ?
O1 C2 C1 115.9(3) . . ?
O2 C2 O1 125.8(3) . . ?
O2 C2 C1 118.3(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 F1 2.020(2) . ?
Sn1 O1 2.215(3) . ?
Sn1 O3 2.304(3) . ?
Sn1 O4 2.496(2) 1_655 ?
Na1 Na1 3.895(3) 2_766 ?
Na1 Na1 3.718(3) 2_756 ?
Na1 F1 2.318(2) . ?
Na1 O1 2.479(3) 2_766 ?
Na1 O2 2.416(3) 2_666 ?
Na1 O4 2.480(3) 2_666 ?
Na1 O5 2.480(4) 2_756 ?
Na1 O5 2.390(3) . ?
O1 Na1 2.479(3) 2_766 ?
O1 C2 1.280(4) . ?
O2 Na1 2.416(3) 2_666 ?
O2 C2 1.223(4) . ?
O3 C1 1.266(5) . ?
O4 Sn1 2.496(2) 1_455 ?
O4 Na1 2.480(3) 2_666 ?
O4 C1 1.234(5) . ?
O5 Na1 2.480(4) 2_756 ?
O5 H5A 0.73(6) . ?
O5 H5B 0.78(7) . ?
C1 C2 1.551(5) . ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sn1 O1 C2 O2 175.1(3) . . . . ?
Sn1 O1 C2 C1 -4.5(4) . . . . ?
Sn1 O3 C1 O4 176.2(3) . . . . ?
Sn1 O3 C1 C2 -4.3(4) . . . . ?
Sn1 O4 C1 O3 23.6(6) 1_455 . . . ?
Sn1 O4 C1 C2 -155.9(2) 1_455 . . . ?
Na1 O1 C2 O2 -5.7(5) 2_766 . . . ?
Na1 O1 C2 C1 174.8(2) 2_766 . . . ?
Na1 O2 C2 O1 -171.8(3) 2_666 . . . ?
Na1 O2 C2 C1 7.8(4) 2_666 . . . ?
Na1 O4 C1 O3 163.8(3) 2_666 . . . ?
Na1 O4 C1 C2 -15.7(4) 2_666 . . . ?
O3 C1 C2 O1 5.9(5) . . . . ?
O3 C1 C2 O2 -173.7(3) . . . . ?
O4 C1 C2 O1 -174.5(3) . . . . ?
O4 C1 C2 O2 5.9(5) . . . . ?
