Fluorine Extraction from Organofluorine Molecules to Make Fluorinated Clusters in Yttrium MOFs
Balkus, Kenneth J.; Abbas, Muhammad; Maceda, Amanda M.; Firouzi, Hamid R.; Xiao, Zhifeng; Arman, Hadi; Shi, Yanshu; Zhou, Hong-Cai; Chemical Science  (2022) –; doi:10.1039/D2SC05143E

data_1568020
_publ_section_title
;
 &#x000D; Fluorine Extraction from Organofluorine Molecules to Make
 Fluorinated Clusters in Yttrium MOFs&#x000D;
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC05143E
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H15 F2 N3 O6.625 Y1.5'
_chemical_formula_sum            'C30 H15 F2 N3 O6.62 Y1.5'
_chemical_formula_weight         694.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-13 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.74780(10)
_cell_length_b                   17.74780(10)
_cell_length_c                   25.9278(2)
_cell_measurement_reflns_used    19731
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4120
_cell_measurement_theta_min      3.0090
_cell_volume                     8166.85(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.928
_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   -120.00 -62.00   0.50    0.42    --  -46.87-142.00  32.00  116
  2  \w    -80.00 -15.00   0.50    1.68    --  -88.50 102.00  22.00  130
  3  \w     36.00 113.00   0.50    1.68    --  106.69-127.00-157.00  154
  4  \w   -120.00 -88.00   0.50    0.42    --  -46.87-125.00-180.00   64
  5  \w    -30.00  29.00   0.50    0.42    --  -46.87  19.00 -30.00  118
  6  \w   -120.00 -83.00   0.50    0.42    --  -46.87 -57.00-180.00   74
  7  \w    -28.00  30.00   0.50    0.42    --   46.87 -19.00-120.00  116
  8  \w   -164.00 -74.00   0.50    1.68    --  -88.50 -22.00  57.00  180
  9  \w     34.00 105.00   0.50    1.68    --  106.69 -94.00 -60.00  142
 10  \w     34.00 101.00   0.50    1.68    --  106.69 -77.00 -90.00  134
 11  \w     34.00  71.00   0.50    1.68    --  106.69 -61.00  30.00   74
 12  \w     34.00  71.00   0.50    1.68    --  106.69 -61.00  90.00   74
 13  \w     34.00  71.00   0.50    1.68    --  106.69 -61.00 150.00   74
 14  \w     34.00  71.00   0.50    1.68    --  106.69 -61.00 120.00   74
 15  \w     34.00  71.00   0.50    1.68    --  106.69 -61.00 -90.00   74
 16  \w     34.00  71.00   0.50    1.68    --  106.69 -61.00  60.00   74
 17  \w   -121.00 -40.00   0.50    0.42    --  -46.87 -37.00-150.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0728566000
_diffrn_orient_matrix_UB_12      -0.0194474000
_diffrn_orient_matrix_UB_13      0.0294207000
_diffrn_orient_matrix_UB_21      -0.0400063000
_diffrn_orient_matrix_UB_22      0.0163753000
_diffrn_orient_matrix_UB_23      0.0515019000
_diffrn_orient_matrix_UB_31      -0.0250125000
_diffrn_orient_matrix_UB_32      -0.0830212000
_diffrn_orient_matrix_UB_33      0.0032809000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26165
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.683
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2764
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.085
_refine_diff_density_max         4.608
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0100P)^2^+155.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4009
_reflns_number_total             4100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05143e2.cif
_cod_data_source_block           hpd476
_cod_original_cell_volume        8166.85(11)
_cod_original_formula_sum        'C30 H15 F2 N3 O6.62 Y1.50'
_cod_database_code               1568020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O F Y'
_chemical_oxdiff_usercomment     PB479
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C14) = Uanis(C13) = Uanis(C12) = Uanis(C17) = Uanis(C16)
Uanis(C11) = Uanis(C19) = Uanis(C18) = Uanis(N2)
3. Others
 Fixed Sof: O6(0.25) O5(0.0625) C16(0.5) H16(0.5) C15(0.5) H15(0.5) C14(0.5)
 H14(0.5) C13(0.5) H13(0.5) C12(0.5) C11(0.5) C19(0.5) H19(0.5) C18(0.5)
 N2(0.5) C17(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C16(H16), C15(H15), C14(H14),
 C13(H13), C19(H19)
4.b Fitted hexagon refined as free rotating group:
 C12(C11,C19,C18,N2,C17)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77064
_shelx_fab_checksum              50084
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.655
_oxdiff_exptl_absorpt_empirical_full_min 0.675