pH-Regulated Nonelectrogenic Anion Transport by Phenylthiosemicarbazones.
Howe, Ethan N. W.; Busschaert, Nathalie; Wu, Xin; Berry, Stuart N.; Ho, Junming; Light, Mark E.; Czech, Dawid D.; Klein, Harry A.; Kitchen, Jonathan A.; Gale, Philip A.; Journal of the American Chemical Society 138 (2016) 8301–8308; doi:10.1021/jacs.6b04656

data_4125114
_publ_section_title
;
 pH-Regulated Nonelectrogenic Anion Transport by Phenylthiosemicarbazones.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8301
_journal_page_last               8308
_journal_paper_doi               10.1021/jacs.6b04656
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C13 H17 N3 S'
_chemical_formula_sum            'C13 H17 N3 S'
_chemical_formula_weight         247.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.419(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8157(9)
_cell_length_b                   7.5474(4)
_cell_length_c                   11.0448(6)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.1710
_cell_measurement_theta_min      2.9480
_cell_volume                     1317.98(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_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   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000    0.0000  -90.0000 180

  2 omega  -36.00   52.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000   72.0000 -180.0000 88

  3 omega -113.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000    0.0000  -60.0000 180

  4 omega  -68.00  -57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0000  -72.0000 -120.0000 11
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0212082000
_diffrn_orient_matrix_UB_12      -0.0493814000
_diffrn_orient_matrix_UB_13      0.0447177000
_diffrn_orient_matrix_UB_21      0.0395197000
_diffrn_orient_matrix_UB_22      -0.0263591000
_diffrn_orient_matrix_UB_23      0.0258409000
_diffrn_orient_matrix_UB_31      -0.0000539000
_diffrn_orient_matrix_UB_32      0.0755536000
_diffrn_orient_matrix_UB_33      0.0381661000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1006
_diffrn_reflns_av_unetI/netI     0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15727
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         2.991
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.082
_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     159
_refine_ls_number_reflns         4012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0427P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2398
_reflns_number_total             4012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04656_si_002.cif
_cod_data_source_block           2015eh002d_r_100k
_cod_depositor_comments
'Adding full bibliography for 4125111--4125114.cif.'
_cod_original_cell_volume        1318.00(13)
_cod_database_code               4125114
_reflns_odcompleteness_completeness 92.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.28
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              5763
_shelx_hkl_checksum              71215
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'