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_7062309
_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         'C51 H53 Mo3 N13 O15, H2 O'
_chemical_formula_sum            'C51 H55 Mo3 N13 O16'
_chemical_formula_weight         1393.877
_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             2022-10-12
_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                100.540(15)
_cell_angle_beta                 97.066(16)
_cell_angle_gamma                100.449(16)
_cell_formula_units_Z            2
_cell_length_a                   9.410(5)
_cell_length_b                   13.710(6)
_cell_length_c                   27.128(12)
_cell_measurement_reflns_used    189591
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.754
_cell_measurement_theta_min      4.460
_cell_volume                     3339(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9931
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9931
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            141006
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9931
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         2.24
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.623
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1404.314
_refine_diff_density_max         3.0069
_refine_diff_density_min         -1.3509
_refine_diff_density_rms         0.1480
_refine_ls_d_res_high            0.7471
_refine_ls_d_res_low             9.0949
_refine_ls_goodness_of_fit_ref   1.0707
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     770
_refine_ls_number_reflns         16684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0707
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+13.7281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                14113
_reflns_number_total             16684
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj05936c2.cif
_cod_data_source_block           compound3a
_cod_depositor_comments
'Adding full bibliography for 7062307--7062310.cif.'
_cod_database_code               7062309
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O2W(H2Wa,H2Wb)
2.b Rotating group:
 O3W(H3Wa,H3Wb), O1W(H1Wa,H1Wb)
2.c Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C33(H33a,H33b), C47(H47a,H47b)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3D(H3D), C4(H4), C6(H6), N7(H7), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45)
2.e Idealised Me refined as rotating group:
 C1D(H1Da,H1Db,H1Dc), C2D(H2Da,H2Db,H2Dc), C18(H18a,H18b,H18c), C20(H20a,H20b,
 H20c), C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C46(H46a,H46b,H46c), C48(H48a,
 H48b,H48c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'