Synthesis and structures of divalent Co, Ni, Zn and Cd complexes of mixed dichalcogen and dipnictogen ligands with corrosion inhibition properties: experimental and computational studies
Yusuf, Tunde L.; Quadri, Taiwo W.; Tolufashe, Gideon F.; Olasunkanmi, Lukman O.; Ebenso, Eno E.; van Zyl, Werner E.; RSC Advances 10 (2020) 41967–41982; doi:10.1039/D0RA07770D

data_7241657
_publ_section_title
;
 Synthesis and structures of divalent Co, Ni, Zn and Cd complexes of mixed
 dichalcogen and dipnictogen ligands with corrosion inhibition properties:
 experimental and computational studies
;
_journal_issue                   69
_journal_name_full               'RSC Advances'
_journal_page_first              41967
_journal_page_last               41982
_journal_paper_doi               10.1039/D0RA07770D
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C31.72 H35.16 N2 O4 P2 S4 Zn'
_chemical_formula_sum            'C31.72 H35.16 N2 O4 P2 S4 Zn'
_chemical_formula_weight         764.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-04 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                87.0380(10)
_cell_angle_beta                 78.8780(10)
_cell_angle_gamma                73.5350(10)
_cell_formula_units_Z            2
_cell_length_a                   10.02980(10)
_cell_length_b                   12.6887(2)
_cell_length_c                   14.1918(2)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.23
_cell_volume                     1699.52(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.9751
_diffrn_measured_fraction_theta_max 0.9751
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0117
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20706
_diffrn_reflns_theta_full        27.4048
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0322 before and 0.0222 after correction.
The Ratio of minimum to maximum transmission is 0.9218.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4929
_exptl_crystal_description       block
_exptl_crystal_F_000             793.2321
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.191
_refine_diff_density_max         0.6838
_refine_diff_density_min         -0.5950
_refine_diff_density_rms         0.0661
_refine_ls_d_res_high            0.7721
_refine_ls_d_res_low             12.1683
_refine_ls_goodness_of_fit_ref   1.0372
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    65
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7546
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0371
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.6576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7002
_reflns_number_total             7546
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ra07770d2.cif
_cod_data_source_block           3
_cod_database_code               7241657
_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
 S4, P1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Others
 Sof(C0aa)=Sof(H0aa)=Sof(H0ab)=Sof(H0ac)=FVAR(1)
 Fixed Sof: C4AA(0.5) H4AA(0.5) C1AA(0.5) H1AA(0.5) C3AA(0.5) H3AA(0.5)
 O10(0.5) C2AA(0.5) H2AA(0.5) O13(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C11(H11a,H11b), C12(H12a,H12b)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C15(H15), C16(H16), C18(H18), C19(H19), C23(H23), C24(H24),
 C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C4AA(H4AA),
 C1AA(H1AA), C3AA(H3AA), C2AA(H2AA)
4.c Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C20(H20a,H20b,H20c), C5AA(H5Aa,H5Ab,H5Ac), C0aa(H0aa,
 H0ab,H0ac)
;
_olex2_submission_special_instructions 'No special instructions were received'