Transmembrane Fluoride Transport: Direct Measurement and Selectivity Studies.
Clarke, Harriet J.; Howe, Ethan N. W.; Wu, Xin; Sommer, Fabian; Yano, Masafumi; Light, Mark E.; Kubik, Stefan; Gale, Philip A.; Journal of the American Chemical Society 138 (2016) 16515–16522; doi:10.1021/jacs.6b10694

data_4131202
_publ_section_title
;
 Transmembrane Fluoride Transport: Direct Measurement and Selectivity
 Studies.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16515
_journal_page_last               16522
_journal_paper_doi               10.1021/jacs.6b10694
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '1(Cs), F, C38 H48 N10, 2(C2 H6 O)'
_chemical_formula_sum            'C42 H60 Cs F N10 O2'
_chemical_formula_weight         888.91
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                117.361(2)
_cell_angle_beta                 97.175(2)
_cell_angle_gamma                90.5504(18)
_cell_formula_units_Z            4
_cell_length_a                   11.5405(3)
_cell_length_b                   20.3342(4)
_cell_length_c                   20.4173(5)
_cell_measurement_reflns_used    55544
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.699
_cell_measurement_theta_min      2.966
_cell_volume                     4209.71(19)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-HF'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55544
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the 
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_exptl_crystal_colour            'clear grayish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848
_exptl_crystal_preparation
'slow diffusion of a CsF solution in ethanol into the DCM solution of calix'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.354
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         21736
_refine_ls_number_restraints     890
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+10.7966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17410
_reflns_number_total             21736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10694_si_005.cif
_cod_data_source_block           2016sot0010a_r_100k
_cod_original_cell_volume        4209.68(19)
_cod_database_code               4131202
_diffrn_measurement_device_type2 'Rigaku AFC12 (Right)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C77-C78
 1.54 with sigma of 0.02
 C78-O3A
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cs2C) = Uanis(Cs2A) = Uanis(Cs2B) = Uanis(Cs2D)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H78C(0.5) H78D(0.5) H78A(0.5) H78B(0.5) O3A(0.5) H3A(0.5)
 Cs2A(0.85) Cs2D(0.05) Cs2B(0.05) Cs2C(0.05) O3B(0.5) H3B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C65(H65A,H65B), C76(H76A,H76B), C27(H27A,H27B), C28(H28A,
 H28B), C37(H37A,H37B), C66(H66A,H66B), C75(H75A,H75B), C72(H72A,H72B),
 C80(H80A,H80B), C31(H31A,H31B), C33(H33A,H33B), C71(H71A,H71B), C70(H70A,H70B),
  C32(H32A,H32B), C69(H69A,H69B), C34(H34A,H34B), C84(H84A,H84B), C78(H78C,
 H78D), C78(H78A,H78B), C82(H82A,H82B)
6.b Aromatic/amide H refined with riding coordinates:
 N11(H11), N1(H1), N3(H3), N4(H4), N2(H2), N14(H14), N13(H13), N12(H12),
 C55(H55), C5(H5), C17(H17), C56(H56), C4(H4A), C42(H42), C43(H43), C25(H25),
 C18(H18), C24(H24), C30(H30), C63(H63), C49(H49), C68(H68), C12(H12A),
 C50(H50), C35(H35), C11(H11A), C73(H73), C62(H62)
6.c Tetrahedral OH refined with riding coordinates:
 O3A(H3A), O3B(H3B)
6.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C60(H60A,H60B,
 H60C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C47(H47A,H47B,H47C), C58(H58A,
 H58B,H58C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C79(H79A,H79B,H79C),
 C83(H83A,H83B,H83C), C77(H77A,H77B,H77C), C81(H81A,H81B,H81C)
6.e Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O1(H1D), O4(H4B)
;
_shelx_res_checksum              13160
_shelx_hkl_checksum              14832
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 2016so0010a_r_100K
_olex2_submission_special_instructions 'No special instructions were received'