Synthesis and electrochemical properties of molybdenum nitrido complexes supported by redox-active NHC and MIC ligands.
Leitner, Daniel; Neururer, Florian R.; Hohloch, Stephan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 582–594; doi:10.1039/d4dt02405b

data_7717360
_publ_section_title
;
 Synthesis and electrochemical properties of molybdenum nitrido complexes
 supported by redox-active NHC and MIC ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              582
_journal_page_last               594
_journal_paper_doi               10.1039/d4dt02405b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H54 Mo N4 O2 S, 0.5(C6 H14), 0.5[C6H14]'
_chemical_formula_sum            'C46 H68 Mo N4 O2 S'
_chemical_formula_weight         837.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-24
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-23 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                65.177(5)
_cell_angle_beta                 68.890(5)
_cell_angle_gamma                81.949(5)
_cell_formula_units_Z            4
_cell_length_a                   16.754(2)
_cell_length_b                   17.595(2)
_cell_length_c                   18.362(2)
_cell_measurement_reflns_used    3314
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      18.876
_cell_measurement_theta_min      2.185
_cell_volume                     4582.7(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest, Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1975
_diffrn_reflns_av_unetI/netI     0.1563
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75311
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.084
_diffrn_reflns_theta_max         25.084
_diffrn_reflns_theta_min         2.152
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0788 after correction.
The Ratio of minimum to maximum transmission is 0.8331.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         16173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0796P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8411
_reflns_number_total             16173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_463n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_original_cell_volume        4582.7(10)
_cod_database_code               7717360
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.971
_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
2.a Secondary CH2 refined with riding coordinates:
 C103(H10A,H10B), C101(H10F,H10G), C104(H10H,H10I), C102(H10J,H10K)
2.b Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C6(H6), C8(H8), C12A(H12A), C14(H14), C8A(H8A), C6A(H6A),
 C12(H12), C42A(H42A), C42(H42), C44(H44), C44A(H44A)
2.c Idealised Me refined as rotating group:
 C61A(H61A,H61B,H61C), C30A(H30A,H30B,H30C), C32A(H32A,H32B,H32C), C31A(H31A,
 H31B,H31C), C30(H30D,H30E,H30F), C27A(H27A,H27B,H27C), C22(H22D,H22E,H22F),
 C26A(H26A,H26B,H26C), C32(H32D,H32E,H32F), C20(H20D,H20E,H20F), C61(H61D,H61E,
 H61F), C31(H31D,H31E,H31F), C48A(H48A,H48B,H48C), C22A(H22A,H22B,H22C),
 C27(H27D,H27E,H27F), C48(H48D,H48E,H48F), C46A(H46A,H46B,H46C), C28A(H28A,H28B,
 H28C), C24A(H24A,H24B,H24C), C24(H24D,H24E,H24F), C23A(H23A,H23B,H23C),
 C46(H46D,H46E,H46F), C23(H23D,H23E,H23F), C18A(H18A,H18B,H18C), C20A(H20A,H20B,
 H20C), C19A(H19A,H19B,H19C), C26(H26D,H26E,H26F), C18(H18D,H18E,H18F),
 C19(H19D,H19E,H19F), C28(H28D,H28E,H28F), C47(H47D,H47E,H47F), C105(H10C,H10D,
 H10E), C47A(H47A,H47B,H47C), C100(H10L,H10M,H10N)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 102 electrons were 
found in a volume of 729\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.25[C6H14] per formula unit 
which account for 100 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27939
_shelx_fab_checksum              81796
_olex2_submission_special_instructions 'No special instructions were received'