Sterically geared tris-thioureas; transmembrane chloride transporters with unusual activity and accessibility
Hennie Valkenier; Christopher M. Dias; Kathryn L. Porter Goff; Ondrej Jurcek; Rakesh Puttreddy; Kari Rissanen; Anthony P. Davis; Chem.Commun. 51 (2015) 14235–; doi:10.1039/C5cc05737J

data_7117760
_publ_section_title
;
 Sterically geared tris-thioureas; transmembrane chloride transporters
 with unusual activity and accessibility
;
_journal_name_full               Chem.Commun.
_journal_page_first              14235
_journal_paper_doi               10.1039/C5cc05737J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'2(Cl), 2(C42 H36 F18 N6 S3), 2(H2 O), 0.5(C8 H22 N2)'
_chemical_formula_sum            'C88 H88 Cl2 F36 N13 O2 S6'
_chemical_formula_weight         2306.97
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-08 deposited with the CCDC.
2015-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.951(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3759(13)
_cell_length_b                   35.024(4)
_cell_length_c                   16.9047(10)
_cell_measurement_reflns_used    2887
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.5960
_cell_measurement_theta_min      3.6170
_cell_volume                     11917.0(17)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
  1 omega  -43.00   13.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 56

  2 omega  -49.00   33.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000 -180.0000 82

  3 omega    1.00   83.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9013  -99.0000   30.0000 82

  4 omega   29.00  106.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -150.0000 77

  5 omega   59.00  148.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000   90.0000 89

  6 omega   87.00  178.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -120.0000 91

  7 omega   31.00  109.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   30.0000 78

  8 omega   38.00   91.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0376194500
_diffrn_orient_matrix_UB_12      0.0163772500
_diffrn_orient_matrix_UB_13      0.0787905000
_diffrn_orient_matrix_UB_21      -0.0005969000
_diffrn_orient_matrix_UB_22      0.0398506000
_diffrn_orient_matrix_UB_23      -0.0387095000
_diffrn_orient_matrix_UB_31      -0.0665799500
_diffrn_orient_matrix_UB_32      0.0088990500
_diffrn_orient_matrix_UB_33      0.0284339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.1206
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21625
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.752
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.286
_exptl_crystal_description       plate
_exptl_crystal_F_000             4708
_exptl_crystal_size_max          0.1999
_exptl_crystal_size_mid          0.1238
_exptl_crystal_size_min          0.0524
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1993
_refine_ls_R_factor_gt           0.1378
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3462
_refine_ls_wR_factor_ref         0.4106
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                4589
_reflns_number_total             12014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05737j2.cif
_cod_data_source_block           tepsf2tmacl
_cod_original_cell_volume        11917.2(17)
_cod_database_code               7117760
_chemical_oxdiff_formula         'C20 H20 O7 N2'
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.647
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Others
 Fixed Sof: C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C47(0.5) H47A(0.5)
 H47B(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5) H50A(0.5) H50B(0.5)
 H50C(0.5)
 Fixed U12: Cl01(0) Cl04(0) N8(0)
 Fixed U22: F7(0.196) F8(0.2)
 Fixed U23: Cl01(0) Cl04(0) N8(0)
 Fixed X: Cl01(0.5) Cl04(0.5) N8(0.5)
 Fixed Z: Cl01(0.25) Cl04(0.25) N8(-0.25)
3.a Free rotating group:
 O006(H00A,H00B)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C9(H9A,H9B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N1(H1), N5(H5), N2(H2), N3(H3), N4(H4), C27(H27), C31(H31), C29(H29),
 C22(H22), C18(H18), C36(H36), C40(H40), C38(H38), C20(H20)
3.d X=CH2 refined with riding coordinates:
 C47(H47A,H47B)
3.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              40634
_shelx_hkl_checksum              16541
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'