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_7706555
_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         '2(C21 H30 Ag3 N9 O6)'
_chemical_formula_sum            'C42 H60 Ag6 N18 O12'
_chemical_formula_weight         1656.30
_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                 91.0170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.0348(10)
_cell_length_b                   17.4283(7)
_cell_length_c                   13.2012(5)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.44
_cell_volume                     5759.0(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            73119
_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         2.475
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1067 before and 0.0568 after correction. The Ratio of minimum to maximum transmission is 0.8780. 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    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         10151
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0314P)^2^+14.7620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7222
_reflns_number_total             10151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04037a2.cif
_cod_data_source_block           ag3(denpz)3
_cod_depositor_comments
'Adding full bibliography for 7706555--7706561.cif.'
_cod_database_code               7706555
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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
 C7B-C6
 1.53 with sigma of 0.01
 C9B-C8B
 1.53 with sigma of 0.01
 C35A-C34 = C35B-C34
 1.52 with sigma of 0.005
 C42A-C41 = C42B-C41
 1.52 with sigma of 0.005
 C35A-C34 \\sim C35B-C34
 with sigma of 0.005
 C42A-C41 \\sim C42B-C41
 with sigma of 0.005
 N18B-C39 \\sim N18A-C39
 with sigma of 0.005
 O12A-N18A \\sim O12B-N18B \\sim O11B-N18B \\sim O11A-N18A
 with sigma of 0.005
 C13A-C12 \\sim C13B-C12
 with sigma of 0.005
 C14B-C13B \\sim C14A-C13A
 with sigma of 0.005
 C7B-C6 \\sim C7A-C6
 with sigma of 0.005
 C10-C9A \\sim C10-C9B
 with sigma of 0.005
 C9B-C8B \\sim C9A-C8A
 with sigma of 0.005
3. Rigid bond restraints
 C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, N8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C33 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim N8: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C35B) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C41) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C36) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O11B) \\sim Ueq, Uanis(O12B) \\sim Ueq, Uanis(N18A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C14A) \\sim Ueq, Uanis(C13A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C9B) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C8B)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C37) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C35A) = Uanis(C35B)
Uanis(C42A) = Uanis(C42B)
Uanis(N18B) = Uanis(N18A)
Uanis(O12A) = Uanis(O12B) = Uanis(O11A) = Uanis(O11B)
Uanis(C13A) = Uanis(C13B)
Uanis(C14A) = Uanis(C14B)
Uanis(C7A) = Uanis(C7B)
Uanis(C8A) = Uanis(C8B)
Uanis(C9B) = Uanis(C9A)
5. Others
 Fixed Sof: H6BC(0.5) H6BD(0.5) H6AA(0.5) H6AB(0.5) C7A(0.5) H7AA(0.5)
 H7AB(0.5) H7AC(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C8A(0.5) H8AA(0.5)
 H8AB(0.5) H8AC(0.5) C8B(0.5) H8BA(0.5) H8BB(0.5) H8BC(0.5) C9A(0.5) H9AA(0.5)
 H9AB(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) C13A(0.5) H13C(0.5) H13D(0.5) C13B(0.5)
 H13A(0.5) H13B(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C14B(0.5)
 H14A(0.5) H14B(0.5) H14C(0.5) H34C(0.5) H34D(0.5) H34A(0.5) H34B(0.5)
 C35A(0.5) H35D(0.5) H35E(0.5) H35F(0.5) C35B(0.5) H35A(0.5) H35B(0.5)
 H35C(0.5) H41C(0.5) H41D(0.5) H41A(0.5) H41B(0.5) C42A(0.5) H42D(0.5)
 H42E(0.5) H42F(0.5) C42B(0.5) H42A(0.5) H42B(0.5) H42C(0.5) N18A(0.5)
 N18B(0.5) O11A(0.5) O11B(0.5) O12A(0.5) O12B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6BC,H6BD), C6(H6AA,H6AB), C9A(H9AA,H9AB), C9B(H9BA,H9BB),
 C13A(H13C,H13D), C13B(H13A,H13B), C16(H16A,H16B), C20(H20A,H20B), C23(H23A,
 H23B), C27(H27A,H27B), C30(H30A,H30B), C34(H34C,H34D), C34(H34A,H34B),
 C37(H37A,H37B), C41(H41C,H41D), C41(H41A,H41B)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC), C8A(H8AA,H8AB,
 H8AC), C8B(H8BA,H8BB,H8BC), C14A(H14D,H14E,H14F), C14B(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C35A(H35D,H35E,H35F), C35B(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C42A(H42D,H42E,H42F), C42B(H42A,H42B,H42C)
;
_shelx_res_checksum              1076
_olex2_submission_special_instructions 'No special instructions were received'