Novel Fluorine-Pillared Metal-Organic Framework for Highly Effective Lithium Enrichment from Brine.
Jiang, Xue; Wu, Ben; Bai, Peng; Lyu, Jiafei; Guo, Xianghai; ACS applied materials & interfaces 13 (2021) 47793–47799; doi:10.1021/acsami.1c17080

data_4519090
_publ_section_title
;
 Novel Fluorine-Pillared Metal-Organic Framework for Highly Effective
 Lithium Enrichment from Brine.
;
_journal_issue                   40
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              47793
_journal_page_last               47799
_journal_paper_doi               10.1021/acsami.1c17080
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         '0.25(C36 H12 F12 Fe12 O36), 0.5(H4 O2)'
_chemical_formula_sum            'C9 H5 F3 Fe3 O10'
_chemical_formula_weight         497.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.8110(5)
_cell_length_b                   25.004(5)
_cell_length_c                   14.5850(13)
_cell_measurement_reflns_used    665
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.5980
_cell_measurement_theta_min      4.5820
_cell_volume                     1389.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -23.00  38.00   1.00   14.00    --    0.00  82.00 -60.00   61
  2  \w     32.00 126.00   1.00   14.00    --  101.30 -82.00 -60.00   94
  3  \w    -24.00  19.00   1.00   14.00    --    0.00  82.00  90.00   43
  4  \w     16.00 130.00   1.00   14.00    --  101.30 -82.00-180.00  114
  5  \w     82.00 123.00   1.00   14.00    --  101.30  82.00-180.00   41
  6  \w    147.00 177.00   1.00   14.00    --  101.30  82.00-180.00   30
  7  \w     15.00 127.00   1.00   14.00    --  101.30 -19.00   0.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0198278000
_diffrn_orient_matrix_UB_12      0.0764136000
_diffrn_orient_matrix_UB_13      -0.0423475000
_diffrn_orient_matrix_UB_21      0.0303839000
_diffrn_orient_matrix_UB_22      -0.0728444000
_diffrn_orient_matrix_UB_23      -0.0444107000
_diffrn_orient_matrix_UB_31      -0.4028106000
_diffrn_orient_matrix_UB_32      -0.0017459000
_diffrn_orient_matrix_UB_33      -0.0054339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4397
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         3.535
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    25.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    2.378
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.338
_refine_diff_density_min         -3.378
_refine_diff_density_rms         0.591
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.860
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1236
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.842
_refine_ls_R_factor_all          0.2050
_refine_ls_R_factor_gt           0.1848
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4317
_refine_ls_wR_factor_ref         0.4500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                930
_reflns_number_total             1236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c17080_si_002.cif
_cod_data_source_block           3717
_cod_database_code               4519090
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.513
_shelx_estimated_absorpt_t_min   0.206
_reflns_odcompleteness_completeness 98.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O5)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
3. Others
 Fixed Sof: H6A(0.5) H6B(0.5)
4.a Riding coordinates:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              79508
_shelx_hkl_checksum              46115
_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 2.385
_oxdiff_exptl_absorpt_empirical_full_min 0.511