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_7706559
_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         'C21 H30 Ag3 N9 O6, C14 H12 S'
_chemical_formula_sum            'C35 H42 Ag3 N9 O6 S'
_chemical_formula_weight         1040.44
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-08 deposited with the CCDC.	2021-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.078(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2738(6)
_cell_length_b                   22.3282(7)
_cell_length_c                   13.8197(6)
_cell_measurement_reflns_used    9609
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      26.6340
_cell_measurement_theta_min      3.2610
_cell_volume                     4032.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -53.00   44.00   1.0000   27.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -37.0000  -60.0000 97

  2 omega   -6.00   85.00   1.0000   27.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9396   37.0000  120.0000 91

  3 omega   35.00   60.00   1.0000   27.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -99.0000   60.0000 25

  4 omega  -50.00   37.00   1.0000   27.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -57.0000 -150.0000 87

  5 omega   59.00   84.00   1.0000   27.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  178.0000   90.0000 25

  6 omega   -8.00   56.00   1.0000   27.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9396   77.0000 -180.0000 64

  7 omega  -42.00    1.00   1.0000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2521  -77.0000  -90.0000 43
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28415
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.969
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.714
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7123
_refine_ls_number_restraints     407
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1149P)^2^+5.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.2069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5312
_reflns_number_total             7123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04037a2.cif
_cod_data_source_block           ag3(denpz)3-dmdbt
_cod_depositor_comments
'Adding full bibliography for 7706555--7706561.cif.'
_cod_database_code               7706559
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15-C16
 1.5 with sigma of 0.01
 C14-C13
 1.5 with sigma of 0.01
 C15-C16 = C14-C13
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, N7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C11, N8, H29
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C18, N9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N8, O3, O4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N7, O1, O2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N9, O5, O6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C15 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(N8)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C9(H9A,H9B), C13(H13A,H13B), C16(H16A,H16B),
 C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              84993
_olex2_submission_special_instructions 'No special instructions were received'