Adducts of Triangular Silver(I) 3,5-Bis(trifluoromethyl)pyrazolate with Thiophene-Derivatives: A Weak Interaction Model of Desulfurization
Liu, Rongrong; Zhang, Wen-Hua; Wei, Donghui; Chen, Jing-Huo; Yang, Guang; Dalton Transactions  (2019) –; doi:10.1039/C9DT03344K

data_7701379
_publ_section_title
;
 Adducts of Triangular Silver(I) 3,5-Bis(trifluoromethyl)pyrazolate with
 Thiophene-Derivatives: A Weak Interaction Model of Desulfurization
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03344K
_journal_year                    2019
_chemical_formula_moiety         'C15 H3 Ag3 F18 N6, C6 H8 S'
_chemical_formula_sum            'C21 H11 Ag3 F18 N6 S'
_chemical_formula_weight         1045.03
_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   geom
_audit_creation_date             2019-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-02 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2918(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9258(5)
_cell_length_b                   13.2224(3)
_cell_length_c                   23.7561(6)
_cell_measurement_reflns_used    9278
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      27.009
_cell_measurement_theta_min      2.250
_cell_volume                     6643.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      298.15(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            112579
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         15297
_refine_ls_number_restraints     3164
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0742P)^2^+10.4360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7872
_reflns_number_total             15297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03344k5.cif
_cod_data_source_block           Ag3L3DMT
_cod_database_code               7701379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.643
_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
 C1-F1 = C1-F2 = C1-F3 = C5-F4 = C5-F5 = C5-F6 = C6-F7 = C6-F8 = C6-F9 = C10-
 F10 = C10-F11 = C10-F12 = C11-F13 = C11-F14 = C11-F15 = C15-F16 = C15-F17 =
 C15-F18 = C16-F19 = C16-F20 = C16-F21 = C20-F22 = C20-F23 = C20-F24 = C21-F25 =
  C21-F26 = C21-F27 = C25-F28 = C25-F29 = C25-F30 = C26-F31 = C26-F32 = C26-F33
 = C30-F34 = C30-F35 = C30-F36 = C1-F1' = C1-F2' = C1-F3' = C5-F4' = C5-F5' =
 C5-F6' = C6-F7' = C6-F8' = C6-F9' = C10-F10' = C10-F11' = C10-F12' = C11-F13' =
  C11-F14' = C11-F15' = C15-F16' = C15-F17' = C15-F18' = C16-F19' = C16-F20' =
 C16-F21' = C20-F22' = C20-F23' = C20-F24' = C21-F25' = C21-F26' = C21-F27' =
 C25-F28' = C25-F29' = C25-F30' = C26-F31' = C26-F32' = C26-F33' = C30-F34' =
 C30-F35' = C30-F36'
 1.33 with sigma of 0.01
 F1-F2 = F1-F3 = F2-F3 = F4-F5 = F4-F6 = F5-F6 = F7-F8 = F7-F9 = F8-F9 = F10-
 F11 = F10-F12 = F11-F12 = F13-F14 = F13-F15 = F14-F15 = F16-F17 = F16-F18 =
 F17-F18 = F19-F20 = F19-F20 = F20-F21 = F22-F23 = F22-F24 = F23-F24 = F25-F26 =
  F25-F27 = F26-F27 = F28-F29 = F28-F30 = F29-F30 = F31-F32 = F31-F33 = F32-F33
 = F34-F35 = F34-F36 = F35-F36 = F1'-F2' = F1'-F3' = F2'-F3' = F4'-F5' = F4'-
 F6' = F5'-F6' = F7'-F8' = F7'-F9' = F8'-F9' = F10'-F11' = F10'-F12' = F11'-
 F12' = F13'-F14' = F13'-F15' = F14'-F15' = F16'-F17' = F16'-F18' = F17'-F18' =
 F19'-F20' = F19'-F20' = F20'-F21' = F22'-F23' = F22'-F24' = F23'-F24' = F25'-
 F26' = F25'-F27' = F26'-F27' = F28'-F29' = F28'-F30' = F29'-F30' = F31'-F32' =
 F31'-F33' = F32'-F33' = F34'-F35' = F34'-F36' = F35'-F36'
 2.13 with sigma of 0.01
 C31-C32 = C35-C36 = C37-C38 = C41-C42
 1.5 with sigma of 0.01
 S1-C32 = S1-C35 = S2-C38 = S2-C41
 1.74 with sigma of 0.01
 C32-C33 = C34-C35 = C38-C39 = C40-C41
 1.37 with sigma of 0.01
 C33-C34 = C39-C40
 1.43 with sigma of 0.01
 S1-C33 = S1-C34 = S2-C39 = S2-C40
 2.58 with sigma of 0.01
 C32-C35 = C38-C41
 2.49 with sigma of 0.01
 C32-C34 = C33-C35 = C38-C40 = C39-C41
 2.33 with sigma of 0.01
 C2-F1 \\sim C2-F2 \\sim C2-F3 \\sim C4-F4 \\sim C4-F5 \\sim C4-F6 \\sim C7-F7
\\sim C7-F8 \\sim C7-F9 \\sim C9-
 F10 \\sim C9-F11 \\sim C9-F12 \\sim C12-F13 \\sim C12-F14 \\sim C12-F15 \\sim
C14-F16 \\sim C14-F17 \\sim C14-
 F18 \\sim C17-F19 \\sim C17-F20 \\sim C17-F21 \\sim C19-F22 \\sim C19-F23
\\sim C19-F24 \\sim C22-F25 ~
 C22-F26 \\sim C22-F27 \\sim C24-F28 \\sim C24-F29 \\sim C24-F30 \\sim C27-F31
\\sim C27-F32 \\sim C27-F33
 \\sim C29-F34 \\sim C29-F35 \\sim C29-F36 \\sim C2-F1' \\sim C2-F2' \\sim
C2-F3' \\sim C4-F4' \\sim C4-F5' ~
 C4-F6' \\sim C7-F7' \\sim C7-F8' \\sim C7-F9' \\sim C9-F10' \\sim C9-F11'
\\sim C9-F12' \\sim C12-F13' ~
 C12-F14' \\sim C12-F15' \\sim C14-F16' \\sim C14-F17' \\sim C14-F18' \\sim
C17-F19' \\sim C17-F20' ~
 C17-F21' \\sim C19-F22' \\sim C19-F23' \\sim C19-F24' \\sim C22-F25' \\sim
C22-F26' \\sim C22-F27' ~
 C24-F28' \\sim C24-F29' \\sim C24-F30' \\sim C27-F31' \\sim C27-F32' \\sim
C27-F33' \\sim C29-F34' ~
 C29-F35' \\sim C29-F36'
 with sigma of 0.01
3. Restrained planarity
 S1, C31, C32, C33, C34, C35, C36
 with sigma of 0.01
 S2, C37, C38, C39, C40, C41, C42
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq,
Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F25) \\sim Ueq,
Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F28) \\sim Ueq, Uanis(F29)
\\sim Ueq, Uanis(F30) \\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F32) \\sim Ueq,
Uanis(F33) \\sim Ueq, Uanis(F34) \\sim Ueq, Uanis(F35) \\sim Ueq, Uanis(F36)
\\sim Ueq, Uanis(F1') \\sim Ueq, Uanis(F2') \\sim Ueq, Uanis(F3') \\sim Ueq,
Uanis(F4') \\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F6') \\sim Ueq, Uanis(F7')
\\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F10') \\sim Ueq,
Uanis(F11') \\sim Ueq, Uanis(F12') \\sim Ueq, Uanis(F13') \\sim Ueq,
Uanis(F14') \\sim Ueq, Uanis(F15') \\sim Ueq, Uanis(F16') \\sim Ueq,
Uanis(F17') \\sim Ueq, Uanis(F18') \\sim Ueq, Uanis(F19') \\sim Ueq,
Uanis(F20') \\sim Ueq, Uanis(F21') \\sim Ueq, Uanis(F22') \\sim Ueq,
Uanis(F23') \\sim Ueq, Uanis(F24') \\sim Ueq, Uanis(F25') \\sim Ueq,
Uanis(F26') \\sim Ueq, Uanis(F27') \\sim Ueq, Uanis(F28') \\sim Ueq,
Uanis(F29') \\sim Ueq, Uanis(F30') \\sim Ueq, Uanis(F31') \\sim Ueq,
Uanis(F32') \\sim Ueq, Uanis(F33') \\sim Ueq, Uanis(F34') \\sim Ueq,
Uanis(F35') \\sim Ueq, Uanis(F36') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F1) = Uanis(F1')
Uanis(F2) = Uanis(F2')
Uanis(F3) = Uanis(F3')
Uanis(F4) = Uanis(F4')
Uanis(F5) = Uanis(F5')
Uanis(F6) = Uanis(F6')
Uanis(F7) = Uanis(F7')
Uanis(F8) = Uanis(F8')
Uanis(F9) = Uanis(F9')
Uanis(F10) = Uanis(F10')
Uanis(F11) = Uanis(F11')
Uanis(F12) = Uanis(F12')
Uanis(F13) = Uanis(F13')
Uanis(F14) = Uanis(F14')
Uanis(F15) = Uanis(F15')
Uanis(F16) = Uanis(F16')
Uanis(F17) = Uanis(F17')
Uanis(F18) = Uanis(F18')
Uanis(F19) = Uanis(F19')
Uanis(F20) = Uanis(F20')
Uanis(F21) = Uanis(F21')
Uanis(F22) = Uanis(F22')
Uanis(F23) = Uanis(F23')
Uanis(F24) = Uanis(F24')
Uanis(F25) = Uanis(F25')
Uanis(F26) = Uanis(F26')
Uanis(F27) = Uanis(F27')
Uanis(F28) = Uanis(F28')
Uanis(F29) = Uanis(F29')
Uanis(F30) = Uanis(F30')
Uanis(F31) = Uanis(F31')
Uanis(F32) = Uanis(F32')
Uanis(F33) = Uanis(F33')
Uanis(F34) = Uanis(F34')
Uanis(F35) = Uanis(F35')
Uanis(F36) = Uanis(F36')
5. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) F7(0.5) F8(0.5)
 F9(0.5) F10(0.5) F11(0.5) F12(0.5) F13(0.5) F14(0.5) F15(0.5) F16(0.5)
 F17(0.5) F18(0.5) F19(0.5) F20(0.5) F21(0.5) F22(0.5) F23(0.5) F24(0.5)
 F25(0.5) F26(0.5) F27(0.5) F28(0.5) F29(0.5) F30(0.5) F31(0.5) F32(0.5)
 F33(0.5) F34(0.5) F35(0.5) F36(0.5) F1'(0.5) F2'(0.5) F3'(0.5) F4'(0.5)
 F5'(0.5) F6'(0.5) F7'(0.5) F8'(0.5) F9'(0.5) F10'(0.5) F11'(0.5) F12'(0.5)
 F13'(0.5) F14'(0.5) F15'(0.5) F16'(0.5) F17'(0.5) F18'(0.5) F19'(0.5)
 F20'(0.5) F21'(0.5) F22'(0.5) F23'(0.5) F24'(0.5) F25'(0.5) F26'(0.5)
 F27'(0.5) F28'(0.5) F29'(0.5) F30'(0.5) F31'(0.5) F32'(0.5) F33'(0.5)
 F34'(0.5) F35'(0.5) F36'(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C18(H18), C23(H23), C28(H28), C33(H33), C34(H34),
 C39(H39), C40(H40)
6.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C42(H42A,H42B,
 H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'