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_7701378
_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, C8 H6 S'
_chemical_formula_sum            'C23 H9 Ag3 F18 N6 S'
_chemical_formula_weight         1067.03
_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             2019-09-11
_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                 92.2883(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.70080(10)
_cell_length_b                   10.1698(2)
_cell_length_c                   40.8111(7)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      26.433
_cell_measurement_theta_min      2.498
_cell_volume                     3193.60(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            47098
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.942
_diffrn_reflns_theta_min         2.238
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6593
_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    2.219
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7447
_refine_ls_number_restraints     1130
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1077P)^2^+10.6886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4942
_reflns_number_total             7447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03344k5.cif
_cod_data_source_block           Ag3L3BT
_cod_database_code               7701378
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.688
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F5B-C5 = F5A-C5 = F6B-C5 = F6A-C5 = F4A-C5 = F4B-C5
 1.35 with sigma of 0.01
 F7B-C6 = F7A-C6 = F8B-C6 = F8A-C6 = F9A-C6 = F9B-C6
 1.35 with sigma of 0.01
 F9B-C6 = F7B-C6 = F7A-C6 = F8B-C6 = F8A-C6 = F9A-C6
 1.35 with sigma of 0.01
 F12B-C10 = F12A-C10 = F10B-C10 = F10A-C10 = F11B-C10 = F11A-C10
 1.35 with sigma of 0.01
 F14B-C11 = F14A-C11 = F13B-C11 = F13A-C11 = F15B-C11 = F15A-C11
 1.35 with sigma of 0.01
 F16B-C15 = F16A-C15 = F18B-C15 = F18A-C15 = F17A-C15 = F17B-C15
 1.35 with sigma of 0.01
 F1A-C1 = F1B-C1 = F3B-C1 = F3A-C1 = F2A-C1 = F2B-C1
 1.35 with sigma of 0.01
 C22A-C23A = C22B-C23B
 1.35 with sigma of 0.01
 S1A-C16A = S1A-C23A = S1B-C16B = S1B-C23B
 1.75 with sigma of 0.01
 C21A-C22A = C21B-C22B
 1.45 with sigma of 0.01
 F1B-F2B \\sim F1B-F3B \\sim F2B-F3B \\sim F4B-F5B \\sim F4B-F6B \\sim F5B-F6B
\\sim F7B-F8B \\sim F7B-F9B
 \\sim F7B-F8B \\sim F10B-F11B \\sim F10B-F12B \\sim F11B-F12B
 with sigma of 0.01
 F5A-C5 \\sim F5B-C5 \\sim F6B-C5 \\sim F6A-C5 \\sim F4A-C5 \\sim F4B-C5
 with sigma of 0.001
 F9A-C6 \\sim F9B-C6 \\sim F7B-C6 \\sim F7A-C6 \\sim F8B-C6 \\sim F8A-C6
 with sigma of 0.001
 F1A-C1 \\sim F1B-C1 \\sim F3A-C1 \\sim F3B-C1 \\sim F2B-C1 \\sim F2A-C1 \\sim
F4B-C5 \\sim F4A-C5 \\sim F6B-
 C5 \\sim F6A-C5 \\sim F5B-C5 \\sim F5A-C5 \\sim F9B-C6 \\sim F9A-C6 \\sim
F8A-C6 \\sim F8B-C6 \\sim F7A-C6 ~
 F7B-C6 \\sim F11A-C10 \\sim F11B-C10 \\sim F12A-C10 \\sim F12B-C10 \\sim
F10B-C10 \\sim F10A-C10 ~
 F13A-C11 \\sim F13B-C11 \\sim F14A-C11 \\sim F15A-C11 \\sim F14B-C11 \\sim
F15B-C11 \\sim F16A-C15 ~
 F16B-C15 \\sim F18B-C15 \\sim F18A-C15 \\sim F17B-C15 \\sim F17A-C15
 with sigma of 0.01
3. Restrained planarity
 S1B, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B
 with sigma of 0.01
 S1A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A
 with sigma of 0.01
4. Rigid bond restraints
 C17A, C16A, C18A, C19A, C20A, C21A, C22A, C23A, S1A
 with sigma for 1-2 distances of 0.006 and sigma for 1-3 distances of 0.006
5. Uiso/Uaniso restraints and constraints
S1A \\sim C22A \\sim C21A \\sim C20A \\sim C18A \\sim C16A \\sim C19A \\sim
C17A \\sim C23A: within 2A with sigma of 0.006 and sigma for terminal atoms of
0.012
Uanis(F3B) \\sim Ueq, Uanis(F2B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F2B) \\sim Ueq, Uanis(F3B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F6B) \\sim Ueq, Uanis(F4B) \\sim Ueq, Uanis(F5B) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F1B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F4B)
\\sim Ueq, Uanis(F5B) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(F7B) \\sim Ueq,
Uanis(F8B) \\sim Ueq, Uanis(F9B) \\sim Ueq, Uanis(F10B) \\sim Ueq, Uanis(F11B)
\\sim Ueq, Uanis(F12B) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14B) \\sim Ueq,
Uanis(F15A) \\sim Ueq, Uanis(F16B) \\sim Ueq, Uanis(F17A) \\sim Ueq,
Uanis(F18A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F6A)
\\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F8A) \\sim Ueq,
Uanis(F11A) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F12A) \\sim Ueq,
Uanis(F15B) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F13B) \\sim Ueq,
Uanis(F17B) \\sim Ueq, Uanis(F18B) \\sim Ueq, Uanis(F16A) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(S1A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A)
\\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq,
Uanis(C22A) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F5A) = Uanis(F5B)
Uanis(F4B) = Uanis(F4A)
Uanis(F6A) = Uanis(F6B)
Uanis(F9B) = Uanis(F9A)
Uanis(F8A) = Uanis(F8B)
Uanis(F7B) = Uanis(F7A)
Uanis(F11B) = Uanis(F11A)
Uanis(F12A) = Uanis(F12B)
Uanis(F10B) = Uanis(F10A)
Uanis(F14A) = Uanis(F14B)
Uanis(F13B) = Uanis(F13A)
Uanis(F15A) = Uanis(F15B)
Uanis(F17B) = Uanis(F17A)
Uanis(F16B) = Uanis(F16A)
Uanis(F18B) = Uanis(F18A)
Uanis(F2A) = Uanis(F2B)
Uanis(F1A) = Uanis(F1B)
Uanis(F3B) = Uanis(F3A)
Uanis(S1A) = Uanis(S1B)
Uanis(C22A) = Uanis(C22B)
Uanis(C23A) = Uanis(C23B)
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
Uanis(C18A) = Uanis(C18B)
Uanis(C19A) = Uanis(C19B)
Uanis(C20A) = Uanis(C20B)
Uanis(C21A) = Uanis(C21B)
6. Others
 Fixed Sof: F1B(0.5) F2B(0.5) F3B(0.5) F4B(0.5) F5B(0.5) F6B(0.5) F7B(0.5)
 F8B(0.5) F9B(0.5) F10B(0.5) F11B(0.5) F12B(0.5) F13A(0.5) F14B(0.5) F15A(0.5)
 F16B(0.5) F17A(0.5) F18A(0.5) S1A(0.5) C16A(0.5) C17A(0.5) H17(0.5) C18A(0.5)
 H18(0.5) C19A(0.5) H19(0.5) C20A(0.5) H20(0.5) C21A(0.5) C22A(0.5) H22(0.5)
 C23A(0.5) H23(0.5) S1B(0.5) C16B(0.5) C17B(0.5) H17B(0.5) C18B(0.5) H18B(0.5)
 C19B(0.5) H19B(0.5) C20B(0.5) H20B(0.5) C21B(0.5) C22B(0.5) H22B(0.5)
 C23B(0.5) H23B(0.5) F5A(0.5) F4A(0.5) F6A(0.5) F7A(0.5) F9A(0.5) F8A(0.5)
 F11A(0.5) F10A(0.5) F12A(0.5) F15B(0.5) F14A(0.5) F13B(0.5) F17B(0.5)
 F18B(0.5) F16A(0.5) F3A(0.5) F1A(0.5) F2A(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C17A(H17), C18A(H18), C19A(H19), C20A(H20),
 C22A(H22), C23A(H23), C17B(H17B), C18B(H18B), C19B(H19B), C20B(H20B),
 C22B(H22B), C23B(H23B)
7.b Fitted hexagon refined as free rotating group:
 C16A(C17A,C18A,C19A,C20A,C21A), C16B(C17B,C18B,C19B,C20B,C21B)
;
_olex2_submission_special_instructions 'No special instructions were received'