Elucidating phase transformation of Eu-based metal organic framework with intermediate isolation and theoretical calculations
Liu, Zhiqing; Wu, Ying; Zhong, Yuan-Hui; Chung, Lai-Hon; Liao, Wei-Ming; Yang, Xianghua; He, Jun; CrystEngComm 25 (2023) 347–351; doi:10.1039/D2CE01466A

data_7245937
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -30.00  40.00   1.00   10.00    --   10.66 -77.00-150.00   70
  2  \w    -48.00   2.00   1.00   10.00    --  -11.13 -57.00 -30.00   50
  3  \w     14.00  66.00   1.00   10.00    --   10.66  38.00 150.00   52
  4  \w    -33.00  17.00   1.00   10.00    --  -11.13 -77.00-150.00   50
  5  \w    -40.00  20.00   1.00   10.00    --  -11.13  77.00  90.00   60
  6  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0408P)^2^+0.5988P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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
;
_shelx_res_checksum              55015
_shelx_hkl_checksum              57290
_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