Six cobalt(ii), zinc(ii), nickel(ii) and copper(ii) complexes based on bis-benzimidazolyl bidentate ligands with phenolyl ether linkers: synthesis, structural studies and recognition of HSO4−
Zhao, Zhixiang; Yang, Yue; Hu, Linhai; Wang, Jianhua; Yu, Jie; Liu, Qingxiang; CrystEngComm 26 (2024) 5078–5089; doi:10.1039/D4CE00553H

data_7249189
_publ_section_title
;
 Six cobalt(ii), zinc(ii), nickel(ii) and copper(ii) complexes based on
 bis-benzimidazolyl bidentate ligands with phenolyl ether linkers:
 synthesis, structural studies and recognition of HSO4&#x2212;
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5078
_journal_page_last               5089
_journal_paper_doi               10.1039/D4CE00553H
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C29 H24 Cu N4 O6 S, C3 H7 N O'
_chemical_formula_sum            'C32 H31 Cu N5 O7 S'
_chemical_formula_weight         693.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-25 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                68.893(12)
_cell_angle_beta                 79.659(13)
_cell_angle_gamma                72.373(11)
_cell_formula_units_Z            2
_cell_length_a                   10.546(8)
_cell_length_b                   12.516(9)
_cell_length_c                   12.968(9)
_cell_measurement_reflns_used    482
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.78
_cell_measurement_theta_min      2.74
_cell_volume                     1517.1(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_unetI/netI     0.2760
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7651
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.031
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1023 before and 0.0505 after correction. The Ratio of minimum to maximum transmission is 0.6385. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5292
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.2224
_refine_ls_R_factor_gt           0.0969
_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^)+(0.0843P)^2^+9.3702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2484
_reflns_number_total             5292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00553h2.cif
_cod_data_source_block           n110530a
_cod_depositor_comments
'Adding full bibliography for 7249188--7249193.cif.'
_cod_database_code               7249189
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.883
_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
 N5-C31 = N5-C32
 1.48 with sigma of 0.001
 N5-C30
 1.33 with sigma of 0.001
 C30-O7
 1.23 with sigma of 0.01
 C30-C31 = C30-C32
 2.42 with sigma of 0.01
 N5-O7
 2.28 with sigma of 0.01
 N5'-C31' = N5'-C32'
 1.48 with sigma of 0.001
 N5'-C30'
 1.33 with sigma of 0.001
 C30'-O7'
 1.23 with sigma of 0.01
 C30'-C31' = C30'-C32'
 2.42 with sigma of 0.01
 N5'-O7'
 2.28 with sigma of 0.01
3. Restrained planarity
 N5, O7, C30, C31, C32
 with sigma of 0.001
 N5', O7', C30', C31', C32'
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C30') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O7) = Uanis(O7')
Uanis(N5) = Uanis(N5')
Uanis(C30) = Uanis(C30')
Uanis(C31) = Uanis(C31')
Uanis(C32) = Uanis(C32')
5. Others
 Sof(O7')=Sof(N5')=Sof(C30')=Sof(H30')=Sof(C31')=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C32')=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(O7)=Sof(N5)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C15(H15A,H15B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C6(H6), C5(H5), C4(H4), C3(H3), C7(H7), C18(H18), C19(H19),
  C20(H20), C21(H21), C30(H30), C30'(H30')
6.c Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C14,C9), C24(C25,C26,C27,C28,C23), C2(C1,C6,C5,C4,C3),
 C18(C19,C20,C21,C16,C17)
6.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C31'(H31D,H31E,H31F), C32'(H32D,
 H32E,H32F)
;
_shelx_res_checksum              61568
_olex2_submission_special_instructions 'No special instructions were received'