#------------------------------------------------------------------------------
#$Date: 2023-03-04 20:21:08 +0200 (Sat, 04 Mar 2023) $
#$Revision: 281458 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/59/7245937.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_7245937
loop_
_publ_author_name
'Liu, Zhiqing'
'Wu, Ying'
'Zhong, Yuan-Hui'
'Chung, Lai-Hon'
'Liao, Wei-Ming'
'Yang, Xianghua'
'He, Jun'
_publ_section_title
;
 Elucidating phase transformation of Eu-based metal organic framework with
 intermediate isolation and theoretical calculations
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              347
_journal_page_last               351
_journal_paper_doi               10.1039/D2CE01466A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '2(C4 F O2 S), 4(H4 N), H2 O'
_chemical_formula_sum            'C8 H18 F2 N4 O5 S2'
_chemical_formula_weight         352.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2d4fss
_audit_creation_date             2022-09-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-22 deposited with the CCDC.	2022-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.725(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6143(5)
_cell_length_b                   10.5019(3)
_cell_length_c                   8.8282(3)
_cell_measurement_reflns_used    8953
_cell_measurement_temperature    240.01(10)
_cell_measurement_theta_max      29.7930
_cell_measurement_theta_min      3.7190
_cell_volume                     1496.38(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  40.00   1.00   10.00    --   10.66 -77.00-150.00   70
  2  ω    -48.00   2.00   1.00   10.00    --  -11.13 -57.00 -30.00   50
  3  ω     14.00  66.00   1.00   10.00    --   10.66  38.00 150.00   52
  4  ω    -33.00  17.00   1.00   10.00    --  -11.13 -77.00-150.00   50
  5  ω    -40.00  20.00   1.00   10.00    --  -11.13  77.00  90.00   60
  6  ω    -48.00  41.00   1.00   10.00    --  -11.13  19.00  30.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0297481000
_diffrn_orient_matrix_UB_12      0.0154691000
_diffrn_orient_matrix_UB_13      -0.0695221000
_diffrn_orient_matrix_UB_21      0.0151452000
_diffrn_orient_matrix_UB_22      0.0633613000
_diffrn_orient_matrix_UB_23      0.0045022000
_diffrn_orient_matrix_UB_31      0.0285445000
_diffrn_orient_matrix_UB_32      -0.0175894000
_diffrn_orient_matrix_UB_33      -0.0446335000
_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  0.0220
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14979
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.885
_diffrn_reflns_theta_min         3.525
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       cube
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0306
_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)+(0.0408P)²+0.5988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3345
_reflns_number_total             3744
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce01466a2.cif
_cod_data_source_block           exp_5969
_cod_depositor_comments
'Adding full bibliography for 7245936--7245937.cif.'
_cod_database_code               7245937
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Restrained distances
 H4A-H4B \\sim H4A-H4C \\sim H4A-H4D \\sim H4B-H4C \\sim H4B-H4D \\sim H4C-H4D
 with sigma of 0.02
;
_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 1.244
_oxdiff_exptl_absorpt_empirical_full_min 0.808
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
S1 S 0.44821(2) -0.17115(3) -0.30815(4) 0.02129(10) Uani 1 1 d . . . . .
F1 F 0.33975(5) -0.07053(8) -0.10742(10) 0.0285(2) Uani 1 1 d . . . . .
O1 O 0.35839(7) 0.01207(11) 0.26177(12) 0.0315(2) Uani 1 1 d . . . . .
O2 O 0.33197(6) 0.17758(9) 0.09839(13) 0.0268(2) Uani 1 1 d . . . . .
C1 C 0.37142(8) 0.07797(12) 0.15370(15) 0.0194(3) Uani 1 1 d . . . . .
C2 C 0.44011(7) 0.03826(12) 0.07729(15) 0.0173(2) Uani 1 1 d . . . . .
C3 C 0.42103(7) -0.03609(12) -0.05534(15) 0.0180(2) Uani 1 1 d . . . . .
C4 C 0.47762(7) -0.07763(12) -0.13862(14) 0.0169(2) Uani 1 1 d . . . . .
S2 S 0.07246(2) 0.15795(3) 0.31337(4) 0.02082(10) Uani 1 1 d . . . . .
F003 F 0.16404(5) 0.05236(9) 0.08631(10) 0.0297(2) Uani 1 1 d . . . . .
O4 O 0.12246(6) -0.01253(9) -0.29194(12) 0.0258(2) Uani 1 1 d . . . . .
O3 O 0.15200(6) -0.18707(9) -0.14556(12) 0.0268(2) Uani 1 1 d . . . . .
C5 C 0.11410(7) -0.08287(12) -0.18427(15) 0.0180(2) Uani 1 1 d . . . . .
C6 C 0.05296(7) -0.04235(12) -0.09010(15) 0.0171(2) Uani 1 1 d . . . . .
C7 C 0.08123(7) 0.02696(12) 0.04533(15) 0.0186(2) Uani 1 1 d . . . . .
C8 C 0.03189(7) 0.07179(12) 0.14089(14) 0.0170(2) Uani 1 1 d . . . . .
N2 N 0.24045(8) 0.18883(14) -0.22798(18) 0.0277(3) Uani 1 1 d . . . . .
N1 N 0.44574(9) 0.37573(13) 0.07069(16) 0.0276(3) Uani 1 1 d . . . . .
N3 N 0.03872(9) -0.36577(13) -0.07876(16) 0.0257(3) Uani 1 1 d . . . . .
N4 N 0.25798(9) -0.2365(2) 0.1590(2) 0.0487(5) Uani 1 1 d . . . . .
O5 O 0.25258(9) 0.01136(18) -0.53112(19) 0.0610(5) Uani 1 1 d . . . . .
H2A H 0.2693(13) 0.1805(18) -0.130(3) 0.038(5) Uiso 1 1 d . . . . .
H2B H 0.2707(12) 0.235(2) -0.281(2) 0.043(5) Uiso 1 1 d . . . . .
H1A H 0.4853(15) 0.346(2) 0.153(3) 0.053(6) Uiso 1 1 d . . . . .
H1B H 0.4029(14) 0.322(2) 0.064(3) 0.050(6) Uiso 1 1 d . . . . .
H1C H 0.4635(12) 0.3686(19) -0.015(3) 0.040(5) Uiso 1 1 d . . . . .
H1D H 0.4331(13) 0.454(2) 0.085(3) 0.048(6) Uiso 1 1 d . . . . .
H2C H 0.1936(14) 0.228(2) -0.227(2) 0.048(6) Uiso 1 1 d . . . . .
H2D H 0.2249(13) 0.116(2) -0.272(3) 0.051(6) Uiso 1 1 d . . . . .
H3A H 0.0249(13) -0.350(2) 0.006(3) 0.045(6) Uiso 1 1 d . . . . .
H3B H 0.0791(13) -0.3086(19) -0.089(2) 0.040(5) Uiso 1 1 d . . . . .
H3C H -0.0054(16) -0.359(2) -0.157(3) 0.066(7) Uiso 1 1 d . . . . .
H3D H 0.0591(14) -0.441(2) -0.080(3) 0.056(6) Uiso 1 1 d . . . . .
H4A H 0.2285(12) -0.2133(19) 0.072(2) 0.042(5) Uiso 1 1 d D . . . .
H4B H 0.2254(12) -0.260(2) 0.223(2) 0.054(6) Uiso 1 1 d D . . . .
H4C H 0.2933(14) -0.290(2) 0.157(3) 0.079(9) Uiso 1 1 d D . . . .
H4D H 0.285(2) -0.165(3) 0.210(4) 0.24(3) Uiso 1 1 d D . . . .
H5A H 0.204(2) 0.040(3) -0.580(3) 0.091(10) Uiso 1 1 d . . . . .
H5B H 0.2776(19) 0.000(3) -0.600(4) 0.095(10) 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
O1 C1 O2 126.04(12) . . ?
O1 C1 C2 118.48(12) . . ?
O2 C1 C2 115.49(11) . . ?
C3 C2 C1 119.19(11) . . ?
C3 C2 C4 119.94(11) . 3_655 ?
C4 C2 C1 120.87(11) 3_655 . ?
F1 C3 C2 116.39(10) . . ?
F1 C3 C4 118.40(11) . . ?
C2 C3 C4 125.21(11) . . ?
C2 C4 S1 122.65(9) 3_655 . ?
C3 C4 S1 122.50(10) . . ?
C3 C4 C2 114.85(11) . 3_655 ?
O4 C5 O3 125.66(11) . . ?
O4 C5 C6 117.71(11) . . ?
O3 C5 C6 116.63(11) . . ?
C7 C6 C5 119.13(11) . . ?
C7 C6 C8 119.97(11) . 3 ?
C8 C6 C5 120.88(11) 3 . ?
F003 C7 C6 116.53(10) . . ?
F003 C7 C8 118.41(11) . . ?
C6 C7 C8 125.06(11) . . ?
C6 C8 S2 122.45(9) 3 . ?
C7 C8 S2 122.58(9) . . ?
C7 C8 C6 114.97(11) . 3 ?
H2A N2 H2B 108.4(18) . . ?
H2A N2 H2C 108.2(19) . . ?
H2A N2 H2D 112.8(19) . . ?
H2B N2 H2C 110.7(18) . . ?
H2B N2 H2D 112.5(18) . . ?
H2C N2 H2D 104.2(19) . . ?
H1A N1 H1B 104.6(19) . . ?
H1A N1 H1C 109.4(19) . . ?
H1A N1 H1D 111(2) . . ?
H1B N1 H1C 108.2(18) . . ?
H1B N1 H1D 112.8(19) . . ?
H1C N1 H1D 110.4(19) . . ?
H3A N3 H3B 108.1(18) . . ?
H3A N3 H3C 109(2) . . ?
H3A N3 H3D 112(2) . . ?
H3B N3 H3C 111(2) . . ?
H3B N3 H3D 107.3(18) . . ?
H3C N3 H3D 108(2) . . ?
H4A N4 H4B 110.1(16) . . ?
H4A N4 H4C 116.3(19) . . ?
H4A N4 H4D 109(2) . . ?
H4B N4 H4C 111.4(18) . . ?
H4B N4 H4D 102.2(18) . . ?
H4C N4 H4D 107.3(19) . . ?
H5A O5 H5B 105(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
S1 C4 1.7597(13) . ?
F1 C3 1.3679(14) . ?
O1 C1 1.2386(16) . ?
O2 C1 1.2690(16) . ?
C1 C2 1.5154(16) . ?
C2 C3 1.3803(18) . ?
C2 C4 1.4075(17) 3_655 ?
C3 C4 1.3938(16) . ?
S2 C8 1.7620(13) . ?
F003 C7 1.3633(13) . ?
O4 C5 1.2374(16) . ?
O3 C5 1.2684(16) . ?
C5 C6 1.5181(16) . ?
C6 C7 1.3833(18) . ?
C6 C8 1.4086(16) 3 ?
C7 C8 1.3905(16) . ?
N2 H2A 0.89(2) . ?
N2 H2B 0.90(2) . ?
N2 H2C 0.88(2) . ?
N2 H2D 0.87(2) . ?
N1 H1A 0.91(2) . ?
N1 H1B 0.90(2) . ?
N1 H1C 0.88(2) . ?
N1 H1D 0.86(2) . ?
N3 H3A 0.85(2) . ?
N3 H3B 0.92(2) . ?
N3 H3C 0.88(3) . ?
N3 H3D 0.86(3) . ?
N4 H4A 0.842(18) . ?
N4 H4B 0.906(18) . ?
N4 H4C 0.82(2) . ?
N4 H4D 0.94(2) . ?
O5 H5A 0.87(3) . ?
O5 H5B 0.82(3) . ?
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
F1 C3 C4 S1 0.52(17) . . . . ?
F1 C3 C4 C2 -179.92(11) . . . 3_655 ?
O1 C1 C2 C3 94.33(16) . . . . ?
O1 C1 C2 C4 -86.54(16) . . . 3_655 ?
O2 C1 C2 C3 -85.37(15) . . . . ?
O2 C1 C2 C4 93.76(15) . . . 3_655 ?
C1 C2 C3 F1 -0.95(18) . . . . ?
C1 C2 C3 C4 178.93(12) . . . . ?
C2 C3 C4 S1 -179.37(10) . . . . ?
C2 C3 C4 C2 0.2(2) . . . 3_655 ?
C4 C2 C3 F1 179.91(11) 3_655 . . . ?
C4 C2 C3 C4 -0.2(2) 3_655 . . . ?
F003 C7 C8 S2 -0.85(17) . . . . ?
F003 C7 C8 C6 179.60(11) . . . 3 ?
O4 C5 C6 C7 -93.45(15) . . . . ?
O4 C5 C6 C8 85.02(16) . . . 3 ?
O3 C5 C6 C7 86.90(15) . . . . ?
O3 C5 C6 C8 -94.62(15) . . . 3 ?
C5 C6 C7 F003 -1.10(18) . . . . ?
C5 C6 C7 C8 178.87(12) . . . . ?
C6 C7 C8 S2 179.18(10) . . . . ?
C6 C7 C8 C6 -0.4(2) . . . 3 ?
C8 C6 C7 F003 -179.59(11) 3 . . . ?
C8 C6 C7 C8 0.4(2) 3 . . . ?
