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_7706557
_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 Cu3 N9 O6, C14 H12 S'
_chemical_formula_sum            'C35 H42 Cu3 N9 O6 S'
_chemical_formula_weight         907.45
_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                 98.4970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8398(6)
_cell_length_b                   21.8537(10)
_cell_length_c                   14.0702(6)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.21
_cell_volume                     3904.7(3)
_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    'ShelXT (Sheldrick, 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_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0201
_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            61638
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0704 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.8484.
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    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         6899
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0421P)^2^+3.1541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5489
_reflns_number_total             6899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04037a2.cif
_cod_data_source_block           cu3(denpz)3-dmdbt
_cod_depositor_comments
'Adding full bibliography for 7706555--7706561.cif.'
_cod_database_code               7706557
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.724
_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
 N8A-C5 \\sim N8B-C5
 with sigma of 0.001
 C15A-C14 \\sim C15B-C14
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(N8A) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O3A) \\sim Ueq, Uanis(O3B) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(O4A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(C15A) \\sim Ueq, Uanis(C15B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O4A) = Uanis(O4B)
Uanis(O3A) = Uanis(O3B)
Uanis(N8B) = Uanis(N8A)
Uanis(C15A) = Uanis(C15B)
4. Others
 Fixed Sof: H14C(0.5) H14D(0.5) H14A(0.5) H14B(0.5) C15A(0.5) H15D(0.5)
 H15E(0.5) H15F(0.5) C15B(0.5) H15A(0.5) H15B(0.5) H15C(0.5) N8A(0.5) N8B(0.5)
 O3A(0.5) O3B(0.5) O4A(0.5) O4B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C14(H14C,H14D), C14(H14A,H14B), C16(H16A,
 H16B), C18(H18A,H18B), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C31(H31), C32(H32), C33(H33)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15A(H15D,H15E,H15F), C15B(H15A,
 H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              24011
_olex2_submission_special_instructions 'No special instructions were received'