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_1568019
_publ_section_title
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 &#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_formula_moiety         'C72 H58 N10 O16 Y2, C3 H7 N O, H2 O'
_chemical_formula_sum            'C75 H67 N11 O18 Y2'
_chemical_formula_weight         1588.21
_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   mixed
_audit_creation_date             2022-06-21
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-12 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                78.447(3)
_cell_angle_beta                 75.155(3)
_cell_angle_gamma                89.692(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8512(12)
_cell_length_b                   16.2294(16)
_cell_length_c                   19.309(2)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      36.41
_cell_measurement_theta_min      2.46
_cell_volume                     3513.0(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            335216
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.873
_diffrn_reflns_theta_min         1.780
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1131 before and 0.0635 after correction.
The Ratio of minimum to maximum transmission is 0.7857.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.954
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         32879
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+7.1266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22971
_reflns_number_total             32879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05143e2.cif
_cod_data_source_block           balkus_ab829_2_0m
_cod_original_cell_volume        3512.9(6)
_cod_database_code               1568019
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.846
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 C6, N11, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C4) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C4) = Uanis(N11) = Uanis(C5) = Uanis(C6)
4.a Free rotating group:
 O1(H1D,H1E)
4.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C30(H30), C27(H27), C47(H47), C45(H45), C42(H42), C67(H67),
 C22(H22), C39(H39), C20(H20), C25(H25), C9(H9), C19(H19), C3(H3), C21(H21),
 C31(H31), C70(H70), C71(H71), C41(H41), C51(H51), C73(H73), C12(H12), C72(H72),
  C54(H54), C40(H40), C53(H53), C32(H32), C33(H33), C59(H59), C52(H52),
 C62(H62), C61(H61), C60(H60), C14(H14), C4(H4)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C11(H11A,
 H11B,H11C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C),
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_original_sample_id AB829
_olex2_submission_special_instructions 'No special instructions were received'