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_7706560
_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         '0.5(C42 H60 Cu6 N18 O12)'
_chemical_formula_sum            'C21 H30 Cu3 N9 O6'
_chemical_formula_weight         695.16
_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                 90.671(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.6486(15)
_cell_length_b                   17.7157(10)
_cell_length_c                   12.7565(7)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.48
_cell_volume                     5570.0(6)
_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    '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_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0291
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            69497
_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         2.558
_exptl_absorpt_coefficient_mu    2.323
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0846 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.8542. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         9813
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0506P)^2^+17.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7444
_reflns_number_total             9813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04037a2.cif
_cod_data_source_block           cu3(denpz)3
_cod_depositor_comments
'Adding full bibliography for 7706555--7706561.cif.'
_cod_database_code               7706560
_shelx_shelxl_version_number     2017/1
_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
 C26-C27B = C26-C27A
 1.5 with sigma of 0.005
 C27B-C28B = C27A-C28A
 1.52 with sigma of 0.005
 C7B-C6A = C7A-C6B
 1.52 with sigma of 0.005
 C5-C6B = C6A-C5
 1.5 with sigma of 0.005
 C7B-C6B = C7A-C6A
 1.52 with sigma of 0.005
 C23-C22A = C23-C22B
 1.52 with sigma of 0.005
 C31-C30A = C31-C30B
 1.5 with sigma of 0.005
 C29A-C30A = C29B-C30B
 1.52 with sigma of 0.005
 C41-C42A = C41-C42B
 1.52 with sigma of 0.005
 C5-C6A \\sim C5-C6B
 with sigma of 0.005
 C7B-C6A \\sim C7A-C6B
 with sigma of 0.005
 N8B-C11 \\sim N8A-C11
 with sigma of 0.02
 O3B-N8B \\sim O3A-N8A
 with sigma of 0.02
 O4B-N8B \\sim O4A-N8A
 with sigma of 0.02
3. Rigid bond restraints
 N7, O1, O2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
N7 \\sim O1 \\sim O2: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C27A) \\sim Ueq, Uanis(C27B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C6B) \\sim Ueq, Uanis(C6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22B) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42A) \\sim Ueq, Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(O8) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O4B) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N8B) \\sim Ueq, Uanis(N8A) \\sim Ueq, Uanis(O3B) \\sim Ueq, Uanis(O3A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7B) = Uanis(C7A)
Uanis(C28A) = Uanis(C28B)
Uanis(C27A) = Uanis(C27B)
Uanis(C6A) = Uanis(C6B)
Uanis(C22B) = Uanis(C22A)
Uanis(C30A) = Uanis(C30B)
Uanis(C29B) = Uanis(C29A)
Uanis(C42A) = Uanis(C42B)
Uanis(N8B) = Uanis(N8A)
Uanis(O4B) = Uanis(O4A)
Uanis(O3A) = Uanis(O3B)
5. Others
 Fixed Sof: C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5) H6BA(0.5) H6BB(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) N8A(0.5)
 N8B(0.5) O3A(0.5) O3B(0.5) O4A(0.5) O4B(0.5) C22A(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5) H23C(0.7) H23D(0.7)
 H23A(0.3) H23B(0.3) C27A(0.5) H27A(0.5) H27B(0.5) C27B(0.5) H27C(0.5)
 H27D(0.5) C28A(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C28B(0.5) H28D(0.5)
 H28E(0.5) H28F(0.5) C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C29B(0.5)
 H29D(0.5) H29E(0.5) H29F(0.5) C30A(0.5) H30A(0.5) H30B(0.5) C30B(0.5)
 H30C(0.5) H30D(0.5) H41C(0.6) H41D(0.6) H41A(0.4) H41B(0.4) C42A(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5) C42B(0.5) H42D(0.5) H42E(0.5) H42F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C9(H9A,H9B), C13(H13A,H13B),
 C16(H16A,H16B), C20(H20A,H20B), C23(H23C,H23D), C23(H23A,H23B), C27A(H27A,
 H27B), C27B(H27C,H27D), C30A(H30A,H30B), C30B(H30C,H30D), 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), C8(H8A,H8B,H8C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22A(H22A,H22B,
 H22C), C22B(H22D,H22E,H22F), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F),
 C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C42A(H42A,H42B,H42C), C42B(H42D,H42E,H42F)
;
_shelx_res_checksum              14289
_olex2_submission_special_instructions 'No special instructions were received'