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_7706558
_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, C12 H8 S'
_chemical_formula_sum            'C33 H38 Cu3 N9 O6 S'
_chemical_formula_weight         879.40
_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                 99.202(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8446(18)
_cell_length_b                   21.390(3)
_cell_length_c                   13.7791(19)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      23.86
_cell_measurement_theta_min      2.42
_cell_volume                     3737.0(9)
_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 2018/2 (Sheldrick, 2018)'
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0304
_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       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45165
_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         2.227
_exptl_absorpt_coefficient_mu    1.803
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1233 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.7308.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6597
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+3.5119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4485
_reflns_number_total             6597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04037a2.cif
_cod_data_source_block           cu3(denpz)3-dbt
_cod_depositor_comments
'Adding full bibliography for 7706555--7706561.cif.'
_cod_database_code               7706558
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.491
_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. Rigid bond restraints
 C20, C21
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C15, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C32, C33
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C32 \\sim C33: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C29) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C11(H11A,H11B), C13(H13A,H13B), C18(H18A,H18B),
 C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C23(H23), C29(H29), C30(H30), C31(H31), C32(H32)
4.c Fitted hexagon refined as free rotating group:
 C24(C25,C26,C27,C22,C23), C28(C29,C30,C31,C32,C33)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              342
_olex2_submission_special_instructions 'No special instructions were received'