Trinuclear vanadium(iv) and vanadium(v) complexes derived from 2,4,6-triacetylphloroglucinol and study of their peroxidase mimicking activity.
Maurya, Mannar R.; Tomar, Reshu; Avecilla, Fernando; Ribeiro, Nádia; Carvalho, M Fernanda N N; Kuznetsov, Maxim L.; Correia, Isabel; Pessoa, João Costa; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2589–2609; doi:10.1039/c9dt04415a

data_7703333
_publ_section_title
;
 Trinuclear vanadium(iv) and vanadium(v) complexes derived from
 2,4,6-triacetylphloroglucinol and study of their peroxidase mimicking
 activity.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2589
_journal_page_last               2609
_journal_paper_doi               10.1039/c9dt04415a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C27 H30 K2.69 N6 O22.51 V3, C H3 O, 4(H2 O)'
_chemical_formula_sum            'C28 H42 K2.69 N6 O27.48 V3'
_chemical_formula_weight         1160.35
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-15 deposited with the CCDC.	2020-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                99.742(4)
_cell_angle_beta                 106.683(4)
_cell_angle_gamma                106.122(4)
_cell_formula_units_Z            2
_cell_length_a                   12.3971(10)
_cell_length_b                   14.4307(11)
_cell_length_c                   14.4835(11)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.366
_cell_measurement_theta_min      2.315
_cell_volume                     2295.5(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            89780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_min         2.315
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0670 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.8901. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.097
_refine_diff_density_max         2.239
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         9406
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0935P)^2^+9.3347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7495
_reflns_number_total             9406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04415a2.cif
_cod_data_source_block           compound6a
_cod_depositor_comments
'Adding full bibliography for 7703333--7703335.cif.'
_cod_database_code               7703333
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.720
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C1MA-O1M \\sim C1MB-O1M
 with sigma of 0.02
3. Rigid bond restraints
 C1MA, O1M, C1MB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1MA \\sim O1M \\sim C1MB: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Others
 Sof(C1MB)=Sof(H1Md)=Sof(H1Me)=Sof(H1Mf)=1-FVAR(1)
 Sof(C1MA)=Sof(H1Ma)=Sof(H1Mb)=Sof(H1Mc)=FVAR(1)
 Sof(O2WB)=Sof(H2Wc)=Sof(H2Wd)=1-FVAR(2)
 Sof(O2WA)=Sof(H2Wa)=Sof(H2Wb)=FVAR(2)
6.a Riding coordinates:
 O1W(H1Wa,H1Wb), O2WA(H2Wa,H2Wb), O2WB(H2Wc,H2Wd), O4W(H4Wa,H4Wb), O5W(H5Wa,
 H5Wb), O6W(H6Wa,H6Wb), O7W(H7Wa,H7Wb), O8W(H8Wa,H8Wb), O9W(H9Wa,H9Wb),
 O10W(H10a,H10b), O11W(H11a,H11b)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C18(H18), C19(H19), C20(H20), C25(H25),
 C26(H26), C27(H27)
6.c Idealised Me refined as rotating group:
 C1MA(H1Ma,H1Mb,H1Mc), C1MB(H1Md,H1Me,H1Mf), C8(H8a,H8b,H8c), C15(H15a,H15b,
 H15c), C22(H22a,H22b,H22c)
;
_olex2_submission_special_instructions 'No special instructions were received'