Trinuclear dioxidomolybdenum(vi) complexes derived from benzene-1,3,5-tricarbohydrazide and study of the catalytic activity
Maurya, Mannar R.; Singh, Devesh; Avecilla, Fernando; Sharma, Akhilesh; Gupta, Puneet; New Journal of Chemistry 47 (2023) 6114–6134; doi:10.1039/D2NJ05936C

data_7062308
_publ_section_title
;
 Trinuclear dioxidomolybdenum(vi) complexes derived from
 benzene-1,3,5-tricarbohydrazide and study of the catalytic activity
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6114
_journal_page_last               6134
_journal_paper_doi               10.1039/D2NJ05936C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C55 H62 Mo3 N12 O15 S'
_chemical_formula_sum            'C55 H62 Mo3 N12 O15 S'
_chemical_formula_weight         1451.037
_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             2021-11-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                101.405
_cell_angle_beta                 92.74
_cell_angle_gamma                96.302
_cell_formula_units_Z            2
_cell_length_a                   14.1056
_cell_length_b                   14.2433
_cell_length_c                   16.2004
_cell_measurement_reflns_used    8809
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.507
_cell_measurement_theta_min      2.467
_cell_volume                     3163.196
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.9896
_diffrn_measured_fraction_theta_max 0.9752
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.1039
_diffrn_reflns_Laue_measured_fraction_full 0.9896
_diffrn_reflns_Laue_measured_fraction_max 0.9752
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40573
_diffrn_reflns_point_group_measured_fraction_full 0.9896
_diffrn_reflns_point_group_measured_fraction_max 0.9752
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.46
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.691
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1466.559
_refine_diff_density_max         3.0407
_refine_diff_density_min         -2.0101
_refine_diff_density_rms         0.2673
_refine_ls_d_res_high            0.7449
_refine_ls_d_res_low             13.9846
_refine_ls_goodness_of_fit_ref   1.0506
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    105
_refine_ls_number_parameters     821
_refine_ls_number_reflns         15625
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.0486
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1599P)^2^+13.9719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2902
_refine_ls_wR_factor_ref         0.3236
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                9701
_reflns_number_total             15625
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj05936c2.cif
_cod_data_source_block           compound4a
_cod_depositor_comments
'Adding full bibliography for 7062307--7062310.cif.'
_cod_original_cell_volume        3163.1964
_cod_database_code               7062308
_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, All O(H) groups
2. Restrained distances
 S1A-O1D \\sim S1B-O1D
 with sigma of 0.02
 S1A-C1A \\sim S1B-C1B \\sim S1A-C2A \\sim S1B-C2B
 with sigma of 0.02
3. Rigid bond restraints
 S1A, S1B, C1A, C1B, C2A, C2B, O1D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
S1A \\sim S1B \\sim C1A \\sim C1B \\sim C2A \\sim C2B \\sim O1D: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Others
 Sof(S1B)=Sof(C1B)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=Sof(C2B)=Sof(H2Ba)=Sof(H2Bb)=
 Sof(H2Bc)=1-FVAR(1)
 Sof(S1A)=Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=
 Sof(H2Ac)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b), C24(H24a,H24b), C25(H25a,H25b), C39(H39a,H39b),
 C40(H40a,H40b)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C47(H47), C48(H48), C49(H49),
  C50(H50), C51(H51)
6.c Idealised Me refined as rotating group:
 C1A(H1Aa,H1Ab,H1Ac), C2A(H2Aa,H2Ab,H2Ac), C1B(H1Ba,H1Bb,H1Bc), C2B(H2Ba,H2Bb,
 H2Bc), C1M(H1Ma,H1Mb,H1Mc), C2M(H2Ma,H2Mb,H2Mc), C11(H11a,H11b,H11c), C15(H15a,
 H15b,H15c), C26(H26a,H26b,H26c), C30(H30a,H30b,H30c), C41(H41a,H41b,H41c),
 C45(H45a,H45b,H45c)
;
_olex2_submission_special_instructions 'No special instructions were received'