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_7062310
_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         'C62 H52 Mo3 N12 O15, C3 H7 N O, 0.5(C2 H6 O)'
_chemical_formula_sum            'C66 H62 Mo3 N13 O16.5'
_chemical_formula_weight         1589.099
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2022-09-17
_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                90
_cell_angle_beta                 106.119(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.723(8)
_cell_length_b                   14.233(6)
_cell_length_c                   28.309(11)
_cell_measurement_reflns_used    254934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.169
_cell_measurement_theta_min      4.685
_cell_volume                     7247(5)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.9915
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.9961
_diffrn_reflns_Laue_measured_fraction_max 0.9915
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            140895
_diffrn_reflns_point_group_measured_fraction_full 0.9961
_diffrn_reflns_point_group_measured_fraction_max 0.9915
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.22
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3208.808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.6809
_refine_diff_density_min         -1.8988
_refine_diff_density_rms         0.1396
_refine_ls_d_res_high            0.7462
_refine_ls_d_res_low             9.1849
_refine_ls_goodness_of_fit_ref   1.0643
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    111
_refine_ls_number_parameters     914
_refine_ls_number_reflns         18119
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0642
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0902P)^2^+15.4226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -25
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              -17
_reflns_number_gt                15148
_reflns_number_total             18119
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj05936c2.cif
_cod_data_source_block           compound5a
_cod_depositor_comments
'Adding full bibliography for 7062307--7062310.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7062310
_olex2_refinement_description
;
1. Restrained distances
 O1M-H1M
 0.85 with sigma of 0.01
 Mo1-H1M
 2.863633 with sigma of 0.02
 C1M-H1M
 1.897467 with sigma of 0.02
2. Others
 Fixed Sof: O2M(0.5) H2M(0.5) C3M(0.5) H3Ma(0.5) H3Mb(0.5) C4M(0.5) H4Ma(0.5)
 H4Mb(0.5) H4Mc(0.5)
3.a Rotating group:
 O1W(H1Wa,H1Wb), O2W(H2Wa,H2Wb)
3.b Secondary CH2 refined with riding coordinates:
 C1M(H1Ma,H1Mb), C3M(H3Ma,H3Mb)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3D(H3D), C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59)
3.d Idealised Me refined as rotating group:
 C1D(H1Da,H1Db,H1Dc), C2D(H2Da,H2Db,H2Dc), C2M(H2Ma,H2Mb,H2Mc), C4M(H4Ma,H4Mb,
 H4Mc), C24(H24a,H24b,H24c), C42(H42a,H42b,H42c), C60(H60a,H60b,H60c)
3.e Idealised tetrahedral OH refined as rotating group:
 O2M(H2M)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'