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_7712722
_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         'C40 H54 Mo2 N4 O10 S, 2(C2 H6 O S)'
_chemical_formula_sum            'C44 H66 Mo2 N4 O12 S3'
_chemical_formula_weight         1131.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-12-15
_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                 93.355(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8430(4)
_cell_length_b                   12.0101(2)
_cell_length_c                   47.2649(8)
_cell_measurement_reflns_used    46770
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      27.0190
_cell_measurement_theta_min      2.5880
_cell_volume                     10678.0(3)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            76893
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         2.378
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68840
_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            'metallic yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       needle
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         11331
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+38.1394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8348
_reflns_number_total             11331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00118k2.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               7712722
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C36 \\sim C35-C361 \\sim C35-C37 \\sim C35-C371 \\sim C35-C38 \\sim
C35-C381
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C36) = Uanis(C361) = Uanis(C37) = Uanis(C371) = Uanis(C38) = Uanis(C381)
4. Others
 Sof(C361)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C371)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=Sof(C381)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
5.a Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C361(H36D,H36E,H36F), C371(H37D,H37E,H37F), C381(H38D,
 H38E,H38F), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C24(H24),
 C28(H28), C30(H30)
;
_shelx_res_checksum              51866
_shelx_hkl_checksum              44541
_olex2_submission_special_instructions 'No special instructions were received'