Finding a receptor design for selective recognition of perrhenate and pertechnetate: hydrogen vs. halogen bonding.
Ravi, Anil; Oshchepkov, Aleksandr S.; German, Konstantin E.; Kirakosyan, Gayana A.; Safonov, Aleksey V.; Khrustalev, Victor N.; Kataev, Evgeny A.; Chemical communications (Cambridge, England) 54 (2018) 4826–4829; doi:10.1039/c8cc02048e

data_7121529
_publ_section_title
;
 Finding a receptor design for selective recognition of perrhenate and
 pertechnetate: hydrogen vs. halogen bonding.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4826
_journal_page_last               4829
_journal_paper_doi               10.1039/c8cc02048e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C40 H44 N4 O4, 4(C2 H6 O S)'
_chemical_formula_sum            'C48 H68 N4 O8 S4'
_chemical_formula_weight         957.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-16
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5470)
;
_audit_update_record
;
2018-03-08 deposited with the CCDC.
2018-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                106.574(3)
_cell_angle_beta                 96.681(3)
_cell_angle_gamma                101.627(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7664(3)
_cell_length_b                   10.1835(4)
_cell_length_c                   14.4361(5)
_cell_measurement_reflns_used    10324
_cell_measurement_temperature    291
_cell_measurement_theta_max      73.2820
_cell_measurement_theta_min      4.6410
_cell_volume                     1324.56(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      291
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      5.00  33.00   1.00    2.50    --   40.00  89.00 178.58   28
  2  \w   -114.00 -18.00   1.00    2.50    --  -43.98 -57.00   0.00   96
  3  \w    -70.00  26.00   1.00    2.50    --  -43.98  57.00 150.00   96
  4  \w    -97.00  -2.00   1.00    2.50    --  -43.98 125.00-120.00   95
  5  \w   -116.00 -20.00   1.00    2.50    --  -43.98 -37.00  90.00   96
  6  \w     20.00 116.00   1.00    2.50    --   43.98  37.00-180.00   96
  7  \w     10.00  38.00   1.00    2.50    --   44.00  84.00 -87.93   28
  8  \w     16.00  46.00   1.00    2.50    --   48.00  80.00-166.94   30
  9  \w     15.00  45.00   1.00    2.50    --   48.00  82.00  18.18   30
 10  \w     19.00  45.00   1.00    2.50    --   52.00  82.00  73.45   26
 11  \w     19.00  46.00   1.00    2.50    --   52.00  81.00-137.01   27
 12  \w     29.00 134.00   1.00    2.50    --   60.00  76.00 -61.09  105
 13  \w     32.00 138.00   1.00    2.50    --   64.00  77.00-105.15  106
 14  \w     32.00 138.00   1.00    2.50    --   64.00  77.00  -7.34  106
 15  \w     37.00 142.00   1.00    2.50    --   68.00  76.00 -48.73  105
 16  \w     37.00 142.00   1.00    2.50    --   68.00  76.00-171.81  105
 17  \w     37.00 142.00   1.00    2.50    --   68.00  76.00 146.60  105
 18  \w     37.00 142.00   1.00    2.50    --   68.00  76.00  46.91  105
 19  \w     41.00 146.00   1.00    2.50    --   72.00  76.00 -90.21  105
 20  \w     40.00 146.00   1.00    2.50    --   72.00  77.00  84.96  106
 21  \w     40.00 146.00   1.00    2.50    --   72.00  77.00   2.72  106
 22  \w     45.00 143.00   1.00   20.00    --   76.00  76.00 116.63   98
 23  \w     50.00  77.00   1.00   20.00    --   76.00  65.00-136.14   27
 24  \w     92.00 118.00   1.00   20.00    --   80.00  73.00  34.84   26
 25  \w     50.00  84.00   1.00   20.00    --   80.00  73.00  34.84   34
 26  \w     56.00  82.00   1.00   20.00    --   84.00  66.00 -66.76   26
 27  \w    133.00 163.00   1.00   20.00    --   92.00  69.00 -55.21   30
 28  \w     63.00  92.00   1.00   20.00    --   92.00  69.00 -55.21   29
 29  \w     74.00 172.00   1.00   20.00    --  104.50  77.00 150.00   98
 30  \w    103.00 145.00   1.00   20.00    --  104.50  77.00-150.00   42
 31  \w     73.00  98.00   1.00   20.00    --  104.50  77.00-150.00   25
 32  \w     25.00 106.00   1.00   20.00    --  104.50 -94.00 150.00   81
 33  \w     52.00 108.00   1.00   20.00    --  104.50 -94.00   0.00   56
 34  \w     74.00 104.00   1.00   20.00    --  104.50  77.00  30.00   30
 35  \w     82.00 168.00   1.00   20.00    --  104.50  45.00 -60.00   86
 36  \w     74.00 168.00   1.00   20.00    --  104.50  77.00   0.00   94
 37  \w     74.00 139.00   1.00   20.00    --  104.50  77.00  90.00   65
 38  \w     78.00 104.00   1.00   20.00    --  104.50  61.00 -30.00   26
 39  \w     73.00 152.00   1.00   20.00    --  104.50  77.00 -30.00   79
 40  \w     31.00 101.00   1.00   20.00    --  104.50 -94.00  90.00   70
 41  \w     45.00 119.00   1.00   20.00    --  104.50-125.00   0.00   74
 42  \w    115.00 164.00   1.00   20.00    --  104.50  77.00-120.00   49
 43  \w     30.00 135.00   1.00   20.00    --  104.50 -77.00-180.00  105
 44  \w     74.00 109.00   1.00   20.00    --  104.50  77.00-120.00   35
 45  \w     73.00 178.00   1.00   20.00    --  104.50  77.00  60.00  105
 46  \w    109.00 170.00   1.00   20.00    --  104.50  77.00  30.00   61
 47  \w    103.00 177.00   1.00   20.00    --  104.50  77.00-180.00   74
 48  \w     73.00  99.00   1.00   20.00    --  104.50  77.00-180.00   26
 49  \w     77.00 170.00   1.00   20.00    --  104.50  77.00 120.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.507
_diffrn_reflns_theta_min         3.250
_exptl_absorpt_coefficient_mu    2.066
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.200
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_recrystallization_method
'The material was recrystallised from DMSO'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5254
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0704P)^2^+0.2261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3865
_reflns_number_total             5254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02048e2.cif
_cod_data_source_block           ar1_7
_cod_depositor_comments          'Adding full bibliography for 7121529.cif.'
_cod_original_cell_volume        1324.56(8)
_cod_database_code               7121529
_shelx_shelxl_version_number     2016/6
_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. Rigid body (RIGU) restrains
 O3A, S2, C24A, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C23A, C24, S2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(O2)=Sof(C21)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=1-FVAR(1)
 Sof(O2S)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(S2)=Sof(C23)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(O3A)=1-FVAR(2)
 Sof(S2A)=Sof(O3)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C10(H10), C14(H14), C12(H12), C4(H4), C3(H3), C7(H7), C6(H6)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C21A(H21A,H21B,
 H21C), C22A(H22A,H22B,H22C), C21(H21D,H21E,H21F), C22(H22D,H22E,H22F),
 C23A(H23A,H23B,H23C), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F), C23(H23D,H23E,
 H23F)
;
_shelx_res_checksum              42273
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre Paraloid'
_olex2_submission_original_sample_id ar1_7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;