Ultra-highly selective trapping of perrhenate/pertechnetate by a flexible cationic coordination framework
Li, Cheng-Peng; Ai, Jin-Yun; Zhou, Hang; Chen, Qi; Yang, Yijie; He, Hongming; Du, Miao; Chemical Communications  (2019) –; doi:10.1039/C8CC09364D

data_7122772
_publ_section_title
;
 Ultra-highly selective trapping of perrhenate/pertechnetate by a flexible
 cationic coordination framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09364D
_journal_year                    2019
_chemical_formula_moiety         'C18 H14 Ag N8, C F3 O3 S, 0.5(C2 H3 N)'
_chemical_formula_sum            'C20 H15.5 Ag F3 N8.5 O3 S'
_chemical_formula_weight         619.84
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.03.09 svn.r3491 for OlexSys, GUI svn.r5479)
;
_audit_update_record
;
2018-10-19 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                113.788(6)
_cell_angle_beta                 93.665(5)
_cell_angle_gamma                107.309(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7133(5)
_cell_length_b                   12.3600(7)
_cell_length_c                   13.3642(8)
_cell_measurement_reflns_used    3882
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.2870
_cell_measurement_theta_min      2.4910
_cell_volume                     1229.18(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0740819000
_diffrn_orient_matrix_UB_12      -0.0139310000
_diffrn_orient_matrix_UB_13      -0.0357968000
_diffrn_orient_matrix_UB_21      0.0071716000
_diffrn_orient_matrix_UB_22      -0.0573248000
_diffrn_orient_matrix_UB_23      -0.0378566000
_diffrn_orient_matrix_UB_31      -0.0454748000
_diffrn_orient_matrix_UB_32      -0.0318834000
_diffrn_orient_matrix_UB_33      0.0283856000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8892
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.893
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         4327
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1160P)^2^+10.3219P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3592
_reflns_number_total             4327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09364d2.cif
_cod_data_source_block           216
_cod_original_cell_volume        1229.18(14)
_cod_original_formula_sum        'C20 H15.50 Ag F3 N8.50 O3 S'
_cod_database_code               7122772
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.794
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-O2 = S1-O1 = S1-O3 = S1'-O2' = S1'-O3' = S1'-O1'
 1.45 with sigma of 0.01
 F2-C21 = F3-C21 = F1-C21 = F1'-C21' = F2'-C21' = F3'-C21'
 1.34 with sigma of 0.01
 S1-C21 = S1'-C21'
 1.75 with sigma of 0.005
 O2-C21
 2.65 with sigma of 0.01
 O2'-C21'
 2.65 with sigma of 0.01
 N9-C20
 1.22 with sigma of 0.01
 C20-C19
 1.52 with sigma of 0.01
 C19-N9
 2.75 with sigma of 0.01
 O3'-O1' \\sim O1'-O2'
 with sigma of 0.001
 O2'-O3' \\sim O3'-O1'
 with sigma of 0.001
 F3-F1 \\sim F1-F2
 with sigma of 0.001
 F2-F3 \\sim F3-F1
 with sigma of 0.001
 O1-O2 \\sim O2-O3
 with sigma of 0.001
 O3-O1 \\sim O1-O2
 with sigma of 0.001
 F3'-F1' \\sim F1'-F2'
 with sigma of 0.001
 F2'-F3' \\sim F3'-F1'
 with sigma of 0.001
 S1-O2' \\sim C21'-O3'
 with sigma of 0.001
 O3'-C21' \\sim C21'-O1'
 with sigma of 0.001
 O1'-C21' \\sim C21'-O2'
 with sigma of 0.001
 F3'-S1' \\sim S1'-F2'
 with sigma of 0.001
 F3'-S1' \\sim S1'-F1'
 with sigma of 0.001
 F1'-S1' \\sim S1'-F2'
 with sigma of 0.001
 O3-C21 \\sim C21-O2
 with sigma of 0.001
 O2-C21 \\sim C21-O1
 with sigma of 0.001
 O1-C21 \\sim C21-O3
 with sigma of 0.001
 F3-S1 \\sim S1-F2
 with sigma of 0.001
 F2-S1 \\sim S1-F1
 with sigma of 0.001
 F1-S1 \\sim S1-F3
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20 \\sim N9: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(F3') \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(F1')
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(F2') \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(S1') \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(O1') \\sim Ueq, Uanis(O3')
\\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(O2') \\sim Ueq, Uanis(F2) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(N9) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.002
Uanis(C21) = Uanis(S1')
Uanis(F3') = Uanis(O3)
Uanis(S1) = Uanis(C21')
Uanis(O2) = Uanis(F2')
Uanis(F1') = Uanis(O1)
Uanis(S1') = Uanis(C21)
Uanis(F2) = Uanis(O2')
Uanis(F1) = Uanis(O1')
Uanis(O3') = Uanis(F3)
4. Others
 Sof(S1')=Sof(O3')=Sof(O2')=Sof(O1')=Sof(F1')=Sof(F2')=Sof(F3')=Sof(C21')=1-
 FVAR(1)
 Sof(S1)=Sof(O3)=Sof(F1)=Sof(O1)=Sof(O2)=Sof(C21)=Sof(F3)=Sof(F2)=FVAR(1)
 Fixed Sof: C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) N9(0.5) C20(0.5)
5.a Riding coordinates:
 C19(H19A,H19B,H19C)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C5(H5), C7(H7), C9(H9), C2(H2), C14(H14), C8(H8), C3(H3), C1(H1),
 C16(H16), C11(H11), C18(H18), C10(H10), C17(H17)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_full_max 1.458
_oxdiff_exptl_absorpt_empirical_full_min 0.630