Complexation of triangular silver(I) or copper(I) nitropyrazolates with dibenzothiophenes having potential use in adsorptive desulfurization.
Yang, Lin; Wang, Lihong; Lv, Xingpu; Chen, Jing-Huo; Wang, Yang; Yang, Guang; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2915–2927; doi:10.1039/d0dt04037a

data_7706561
_publ_section_title
;
 Complexation of triangular silver(I) or copper(I) nitropyrazolates with
 dibenzothiophenes having potential use in adsorptive desulfurization.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2915
_journal_page_last               2927
_journal_paper_doi               10.1039/d0dt04037a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C42 H60 Ag6 N18 O12, C8 H6 S'
_chemical_formula_sum            'C50 H66 Ag6 N18 O12 S'
_chemical_formula_weight         1790.48
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-11 deposited with the CCDC.	2021-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.5782(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2517(4)
_cell_length_b                   24.1571(5)
_cell_length_c                   14.3647(3)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      24.94
_cell_measurement_theta_min      2.76
_cell_volume                     6435.1(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41721
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.769
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0696 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.8926.
The \l/2 correction factor is Not present.
;
_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    1.848
_exptl_crystal_description       prism
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         5677
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0402P)^2^+38.5043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4268
_reflns_number_total             5677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04037a2.cif
_cod_data_source_block           Ag3(denpz)3-BT
_cod_depositor_comments
'Adding full bibliography for 7706555--7706561.cif.'
_cod_database_code               7706561
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.703
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1A-C22A = S1A-C29A = S1B-C22B = S1B-C29B
 1.74 with sigma of 0.01
 C27A-C28A = C27B-C28B
 1.43 with sigma of 0.01
 C28A-C29A = C28B-C29B
 1.39 with sigma of 0.01
 S1A-C27A = S1A-C28A = S1B-C27B = S1B-C28B
 2.57 with sigma of 0.01
 C22A-C28A = C27A-C29A = C22B-C28B = C27B-C29B
 2.33 with sigma of 0.01
 C22A-C29A = C22B-C29B
 2.49 with sigma of 0.01
 C1-C2 = C6-C7 = C8-C9 = C13-C14A = C13-C14B = C15-C16 = C20-C21
 1.54 with sigma of 0.01
 C1-C3 = C5-C7 = C8-C10 = C12-C14A = C12-C14B = C15-C17 = C19-C21
 2.51 with sigma of 0.01
 N8A-C11 \\sim N8B-C11
 with sigma of 0.005
 O4A-N8A \\sim O4B-N8B \\sim O3B-N8B \\sim O3A-N8A
 with sigma of 0.005
 O3A-N8A \\sim O3B-N8B \\sim O4A-N8A \\sim O4B-N8B
 with sigma of 0.005
3. Restrained planarity
 S1A, C22A, C23A, C24A, C25A, C26A, C27A, C28A, C29A
 with sigma of 0.01
 S1B, C22B, C23B, C24B, C25B, C26B, C27B, C28B, C29B
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O4B)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O4A) \\sim Ueq,
Uanis(O3B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C27A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1A) \\sim Ueq, Uanis(S1B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C23B) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N8A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O3B) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C14A) \\sim Ueq, Uanis(C14B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(S1A) = Uanis(C23A) = Uanis(S1B) = Uanis(C23B)
Uanis(C22A) = Uanis(C22B)
Uanis(C27A) = Uanis(C27B)
Uanis(C24A) = Uanis(C25A) = Uanis(C26A) = Uanis(C28A) = Uanis(C29A) =
Uanis(C24B) = Uanis(C25B) = Uanis(C26B) = Uanis(C28B) = Uanis(C29B)
Uanis(N8A) = Uanis(N8B)
Uanis(O4A) = Uanis(O4B) = Uanis(O3B) = Uanis(O3A)
Uanis(C14A) = Uanis(C14B)
5. Others
 Fixed Sof: O3A(0.5) O4B(0.5) N8B(0.5) H13A(0.5) H13B(0.5) H13C(0.5) H13D(0.5)
 C14A(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C14B(0.5) H14D(0.5) H14E(0.5)
 H14F(0.5) S1A(0.25) C22A(0.25) C23A(0.25) H23A(0.25) C24A(0.25) H24A(0.25)
 C25A(0.25) H25A(0.25) C26A(0.25) H26A(0.25) C27A(0.25) C28A(0.25) H28A(0.25)
 C29A(0.25) H29A(0.25) S1B(0.25) C22B(0.25) C23B(0.25) H23B(0.25) C24B(0.25)
 H24B(0.25) C25B(0.25) H25B(0.25) C26B(0.25) H26B(0.25) C27B(0.25) C28B(0.25)
 H28B(0.25) C29B(0.25) H29B(0.25) O4A(0.5) N8A(0.5) O3B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C9(H9A,H9B), C13(H13A,H13B), C13(H13C,H13D),
 C16(H16A,H16B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C28A(H28A), C29A(H29A),
 C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C28B(H28B), C29B(H29B)
6.c Fitted hexagon refined as free rotating group:
 C22A(C23A,C24A,C25A,C26A,C27A), C22B(C23B,C24B,C25B,C26B,C27B)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14A(H14A,H14B,H14C),
 C14B(H14D,H14E,H14F), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'