New bis[<i>cis</i>-{MoO<sub>2</sub>}] complexes with dihydrazone ligands: synthesis, characterization, theoretical investigation and their peroxidase mimicking activity.
Rana, Lata; Dheeraj, ?; Hundal, Geeta; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00118k

data_7712721
_publ_section_title
;
 New bis[<i>cis</i>-{MoO<sub>2</sub>}] complexes with dihydrazone ligands:
 synthesis, characterization, theoretical investigation and their
 peroxidase mimicking activity.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00118k
_journal_year                    2023
_chemical_formula_moiety         'C28 H30 Mo2 N4 O12 S2'
_chemical_formula_sum            'C28 H30 Mo2 N4 O12 S2'
_chemical_formula_weight         870.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-22 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.844(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2043(3)
_cell_length_b                   7.9921(2)
_cell_length_c                   17.2958(3)
_cell_measurement_reflns_used    15767
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      25.9590
_cell_measurement_theta_min      2.7960
_cell_volume                     1686.81(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30493
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.355
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       square
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 2022 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         5951
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5173
_reflns_number_total             5951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00118k2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7712721
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.835
_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
2. Restrained distances
 Mo02-O12 \\sim Mo02-O12A
 with sigma of 0.02
 S2-O12 \\sim S2A-O12A
 with sigma of 0.02
 O12-C27 \\sim O12A-C27A
 with sigma of 0.04
 S2-C28 \\sim S2A-C28A
 with sigma of 0.02
 S2-C27 \\sim S2A-C27A
 with sigma of 0.02
 O12-C28 \\sim O12A-C28A
 with sigma of 0.04
 C28-C27 \\sim C28A-C27A
 with sigma of 0.04
 Mo02-S2 \\sim Mo02-S2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C27A)
Uanis(C27) = Uanis(C28A)
4. Rigid body (RIGU) restrains
 S2, O12, C28, C27, O12A, S2A, C27A, C28A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O12A)=Sof(S2A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(S2)=Sof(O12)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(H27C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12),
 C17(H17), C19(H19), C20(H20), C21(H21)
6.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C27A(H27D,H27E,H27F),
 C28A(H28D,H28E,H28F)
;
_shelx_res_checksum              21130
_shelx_hkl_checksum              31565
_olex2_submission_special_instructions 'No special instructions were received'