Selective, Fast-Response, and Regenerable Metal-Organic Framework for Sampling Excess Fluoride Levels in Drinking Water.
Ebrahim, Fatmah Mish; Nguyen, Tu N.; Shyshkanov, Serhii; Gładysiak, Andrzej; Favre, Patrick; Zacharia, Anna; Itskos, Grigorios; Dyson, Paul J.; Stylianou, Kyriakos C.; Journal of the American Chemical Society 141 (2019) 3052–3058; doi:10.1021/jacs.8b11907

data_4128435
_publ_section_title
;
 Selective, Fast-Response, and Regenerable Metal-Organic Framework for
 Sampling Excess Fluoride Levels in Drinking Water.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3052
_journal_page_last               3058
_journal_paper_doi               10.1021/jacs.8b11907
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'[Eu1 (C33 H36 B1 O6) (H2 O1)].2(C3 H7 N1 O1)'
_chemical_formula_sum            'C39 H52 B Eu N2 O9'
_chemical_formula_weight         855.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.022(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.1523(12)
_cell_length_b                   8.6704(2)
_cell_length_c                   32.0714(15)
_cell_measurement_reflns_used    15801
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.9530
_cell_measurement_theta_min      2.4430
_cell_modulation_dimension       1
_cell_volume                     8101.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.756
_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      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0178369000
_diffrn_orient_matrix_UB_12      0.0149379000
_diffrn_orient_matrix_UB_13      0.0071701000
_diffrn_orient_matrix_UB_21      0.0003132000
_diffrn_orient_matrix_UB_22      0.0797288000
_diffrn_orient_matrix_UB_23      -0.0054483000
_diffrn_orient_matrix_UB_31      -0.0168125000
_diffrn_orient_matrix_UB_32      -0.0143606000
_diffrn_orient_matrix_UB_33      -0.0228655000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.889
_diffrn_reflns_Laue_measured_fraction_max 0.756
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            29535
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.756
_diffrn_reflns_theta_full        25.374
_diffrn_reflns_theta_max         30.673
_diffrn_reflns_theta_min         1.511
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.183
_refine_diff_density_min         -7.584
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9366
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.1294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+364.9518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2641
_refine_ls_wR_factor_ref         0.2665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8895
_reflns_number_total             9366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11907_si_002.cif
_cod_data_source_block           SION-105
_cod_database_code               4128435
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.844
_reflns_odcompleteness_completeness 69.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 C12, C13, C14, C15, C16, C17, C18, C19, C21, C22
 with sigma of 0.1
 C23, C24, C25, C26, C27, C28, C29, C30, C32, C33
 with sigma of 0.1
 C1, C2, C3, C4, C5, C6, C7, C8, C10, C11
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(B1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Eu1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C)
;
_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 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.876