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_4131200
_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         'F, C37 H46 N10, C16 H36 N'
_chemical_formula_sum            'C53 H82 F N11'
_chemical_formula_weight         892.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.545(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5283(7)
_cell_length_b                   22.8407(8)
_cell_length_c                   18.0121(8)
_cell_measurement_reflns_used    12452
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0910
_cell_measurement_theta_min      2.2520
_cell_volume                     5245.0(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -113.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000    0.0000   60.0000 180

  2 omega  -29.00    7.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000   72.0000  -30.0000 36

  3 omega  -31.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000   72.0000 -180.0000 71

  4 omega  -97.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000    0.0000   90.0000 152
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_UB_11      -0.0351283000
_diffrn_orient_matrix_UB_12      -0.0200203000
_diffrn_orient_matrix_UB_13      -0.0258258000
_diffrn_orient_matrix_UB_21      0.0306764000
_diffrn_orient_matrix_UB_22      0.0005599000
_diffrn_orient_matrix_UB_23      -0.0251478000
_diffrn_orient_matrix_UB_31      0.0303317000
_diffrn_orient_matrix_UB_32      -0.0237194000
_diffrn_orient_matrix_UB_33      0.0211655000
_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  0.0976
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55028
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.932
_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    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.'
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1944
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         13538
_refine_ls_number_restraints     535
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.0869
_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^)+(0.1022P)^2^+3.4727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7248
_reflns_number_total             13538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10694_si_004.cif
_cod_data_source_block           2016sot0005_r_100k
_cod_database_code               4131200
_diffrn_measurement_device_type2 'Rigaku AFC12 (Right)'
_reflns_odcompleteness_completeness 91.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.28
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.021) H4(0.023) H3(0.027) H2(0.029) H37A(0.027) H37B(0.027)
 H34(0.029) H17(0.034) H11(0.029) H18(0.035) H12(0.03) H36A(0.032) H36B(0.032)
 H25(0.04) H15A(0.044) H15B(0.044) H15C(0.044) H31A(0.033) H31B(0.033)
 H24(0.038) H32A(0.032) H32B(0.032) H30(0.038) H33A(0.03) H33B(0.03) H5(0.039)
 H22A(0.044) H22B(0.044) H22C(0.044) H27A(0.036) H27B(0.036) H8A(0.045)
 H8B(0.045) H8C(0.045) H4A(0.041) H40A(0.042) H40B(0.042) H28A(0.04) H28B(0.04)
 H21A(0.053) H21B(0.053) H21C(0.053) H9A(0.051) H9B(0.051) H9C(0.051)
 H1A(0.061) H1B(0.061) H1C(0.061) H39A(0.048) H39B(0.048) H48A(0.049)
 H48B(0.049) H38A(0.072) H38B(0.072) H38C(0.072) H44A(0.058) H44B(0.058)
 H43A(0.067) H43B(0.067) H47A(0.067) H47B(0.067) H54A(0.071) H54B(0.071)
 H54C(0.071) H54D(0.071) H42A(0.104) H42B(0.104) H42C(0.104) H53A(0.056)
 H53B(0.056) H46A(0.109) H46B(0.109) H46C(0.109) H52A(0.098) H52B(0.098)
 H52C(0.098) H51A(0.056) H51B(0.056) H50A(0.098) H50B(0.098) H50C(0.098)
 Fixed X: H1(0.6525) H4(0.5878) H3(0.7102) H2(0.7749) H37A(0.6119)
 H37B(0.5216) H34(0.7783) H17(0.4015) H11(0.3253) H18(0.5397) H12(0.2834)
 H36A(0.5336) H36B(0.5711) H25(0.8327) H15A(0.3137) H15B(0.339) H15C(0.379)
 H31A(0.9704) H31B(1.091) H24(0.7826) H32A(1.0906) H32B(0.9809) H30(0.9222)
 H33A(0.9745) H33B(1.0047) H5(0.5701) H22A(0.8154) H22B(0.8935) H22C(0.8145)
 H27A(0.9373) H27B(0.8786) H8A(0.5864) H8B(0.6697) H8C(0.6694) H4A(0.7139)
 H40A(0.7618) H40B(0.6683) H28A(1.0031) H28B(1.0724) H21A(0.7368) H21B(0.8195)
 H21C(0.6996) H9A(0.4356) H9B(0.5267) H9C(0.4428) H1A(0.955) H1B(0.9096)
 H1C(0.8448) H39A(0.569) H39B(0.6631) H48A(0.9973) H48B(0.9297) H38A(0.5383)
 H38B(0.5545) H38C(0.6456) H44A(0.9394) H44B(1.0169) H43A(0.9103) H43B(0.9673)
 H47A(1.1237) H47B(1.0523) H54A(0.6321) H54B(0.7157) H54C(0.6484) H54D(0.7246)
 H42A(1.1289) H42B(1.0732) H42C(1.0762) H53A(0.6344) H53B(0.7279) H46A(1.0815)
 H46B(1.1899) H46C(1.1469) H52A(0.5258) H52B(0.6191) H52C(0.5678) H51A(0.5539)
 H51B(0.5992) H50A(0.7355) H50B(0.6322) H50C(0.7035)
 Fixed Y: H1(0.2496) H4(0.3434) H3(0.3331) H2(0.2433) H37A(0.3287)
 H37B(0.3628) H34(0.2327) H17(0.1661) H11(0.3875) H18(0.0925) H12(0.3283)
 H36A(0.3092) H36B(0.2532) H25(0.1419) H15A(0.2627) H15B(0.3211) H15C(0.2612)
 H31A(0.3606) H31B(0.3608) H24(0.0791) H32A(0.2644) H32B(0.2539) H30(0.2917)
 H33A(0.2564) H33B(0.3229) H5(0.381) H22A(0.2142) H22B(0.1623) H22C(0.1595)
 H27A(0.3398) H27B(0.3199) H8A(0.4751) H8B(0.4709) H8C(0.4245) H4A(0.31)
 H40A(0.5044) H40B(0.4809) H28A(0.2326) H28B(0.2803) H21A(0.0673) H21B(0.0629)
 H21C(0.0565) H9A(0.426) H9B(0.4721) H9C(0.4757) H1A(0.2303) H1B(0.2874)
 H1C(0.2291) H39A(0.5638) H39B(0.5899) H48A(0.5737) H48B(0.5566) H38A(0.5491)
 H38B(0.4878) H38C(0.5162) H44A(0.5041) H44B(0.5411) H43A(0.5818) H43B(0.6254)
 H47A(0.503) H47B(0.4758) H54A(0.4919) H54B(0.4965) H54C(0.5042) H54D(0.4881)
 H42A(0.5817) H42B(0.5358) H42C(0.6019) H53A(0.3878) H53B(0.3891) H46A(0.5553)
 H46B(0.5292) H46C(0.586) H52A(0.4301) H52B(0.4255) H52C(0.3685) H51A(0.4407)
 H51B(0.3994) H50A(0.3711) H50B(0.3625) H50C(0.4173)
 Fixed Z: H1(0.3494) H4(0.283) H3(0.2157) H2(0.2855) H37A(0.4085) H37B(0.4259)
 H34(0.5712) H17(0.3522) H11(0.1201) H18(0.3514) H12(0.2234) H36A(0.532)
 H36B(0.4987) H25(0.1307) H15A(0.3338) H15B(0.3822) H15C(0.4239) H31A(0.5387)
 H31B(0.5864) H24(0.226) H32A(0.6175) H32B(0.5529) H30(0.4011) H33A(0.6843)
 H33B(0.6882) H5(-0.0025) H22A(0.4218) H22B(0.4275) H22C(0.4743) H27A(0.2046)
 H27B(0.2618) H8A(0.2365) H8B(0.1937) H8C(0.2578) H4A(0.0013) H40A(0.5446)
 H40B(0.5694) H28A(0.2803) H28B(0.2585) H21A(0.4176) H21B(0.3741) H21C(0.3264)
 H9A(0.045) H9B(0.0643) H9C(0.1066) H1A(0.1252) H1B(0.0777) H1C(0.0589)
 H39A(0.5154) H39B(0.4938) H48A(0.6885) H48B(0.6018) H38A(0.3824) H38B(0.424)
 H38C(0.4009) H44A(0.861) H44B(0.8315) H43A(0.9323) H43B(0.8928) H47A(0.6915)
 H47B(0.6119) H54A(0.7263) H54B(0.8118) H54C(0.7338) H54D(0.8172) H42A(0.9605)
 H42B(0.9978) H42C(1.0216) H53A(0.7336) H53B(0.8136) H46A(0.5436) H46B(0.5953)
 H46C(0.6226) H52A(0.7983) H52B(0.8781) H52C(0.833) H51A(0.7752) H51B(0.7241)
 H50A(0.8343) H50B(0.8543) H50C(0.8864)
;
_shelx_res_checksum              62629
_shelx_hkl_checksum              10677
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'