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_4131199
_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_absolute_configuration unk
_chemical_formula_moiety         'C37 H46 N10'
_chemical_formula_sum            'C37 H46 N10'
_chemical_formula_weight         630.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-01
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7644(4)
_cell_length_b                   11.6635(2)
_cell_length_c                   32.0041(7)
_cell_measurement_reflns_used    45983
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     6631.1(2)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 9.091
_diffrn_detector_type            'Bruker-Nonius CCD camera'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Bruker Nonius FR591 - HF'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            43299
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.952
_diffrn_source                   'Bruker Nonius FR591 Rotating Anode'
_diffrn_source_current           85.0
_diffrn_source_power             4.250
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_correction_T_min  0.9668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      x
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 4286 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         14672
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0449P)^2^+0.7077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                11434
_reflns_number_total             14672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10694_si_002.cif
_cod_data_source_block           2009sot0971
_cod_database_code               4131199
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C112(H11A,H11B), C126(H12D,H12E), C129(H12I,H12J), C132(H13A,H13B), C133(H13C,
 H13D), C134(H13E,H13F), C137(H13G,H13H), C212(H21A,H21B), C226(H22D,H22E),
 C229(H22I,H22J), C232(H23A,H23B), C233(H23C,H23D), C234(H23E,H23F), C237(H23G,
 H23H)
2.b Aromatic/amide H refined with riding coordinates:
 N101(H101), C109(H109), N103(H103), N104(H104), C102(H102), C103(H10A),
 N102(H10H), C111(H111), C116(H116), C117(H117), C123(H123), C124(H124),
 C131(H131), C135(H135), N201(H201), N202(H202), N203(H203), N204(H204),
 C202(H20A), C203(H20B), C209(H209), C210(H210), C216(H216), C217(H217),
 C223(H223), C224(H224), C231(H231), C235(H235)
2.c Idealised Me refined as rotating group:
 C105(H10B,H10C,H10D), C107(H10E,H10F,H10G), C114(H11C,H11D,H11E), C119(H11F,
 H11G,H11H), C121(H12A,H12B,H12C), C128(H12F,H12G,H12H), C205(H20C,H20D,H20E),
 C207(H20F,H20G,H20H), C214(H21C,H21D,H21E), C219(H21F,H21G,H21H), C221(H22A,
 H22B,H22C), C228(H22F,H22G,H22H)
;
_shelx_res_checksum              80773
_shelx_hkl_checksum              77299
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre with silicon oil'
_olex2_submission_special_instructions 'No special instructions were received'