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_7717364
_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         'C35 H52 Mo N4 O2 S, 0.167[C6H14]'
_chemical_formula_sum            'C36 H54.33 Mo N4 O2 S'
_chemical_formula_weight         703.16
_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             2024-04-30
_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                102.384(4)
_cell_angle_beta                 115.020(3)
_cell_angle_gamma                101.929(4)
_cell_formula_units_Z            6
_cell_length_a                   19.0492(14)
_cell_length_b                   19.4669(16)
_cell_length_c                   20.4769(17)
_cell_measurement_reflns_used    2599
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      18.915
_cell_measurement_theta_min      2.411
_cell_volume                     6330.0(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.2740
_diffrn_reflns_av_unetI/netI     0.1805
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            135451
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.089
_diffrn_reflns_theta_max         25.089
_diffrn_reflns_theta_min         1.688
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1104 before and 0.0820 after correction.
The Ratio of minimum to maximum transmission is 0.8787.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             2234
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1250
_refine_ls_number_reflns         22463
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0792P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10622
_reflns_number_total             22463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_467n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_database_code               7717364
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13A-C25A \\sim C13A-C4
 with sigma of 0.02
 C25A-C27A \\sim C4-C3
 with sigma of 0.02
 C25A-C26A \\sim C4-C1C
 with sigma of 0.02
 C25A-C28A \\sim C4-C1D
 with sigma of 0.02
 C13A-C27A \\sim C13A-C3
 with sigma of 0.04
 C13A-C26A \\sim C13A-C1C
 with sigma of 0.04
 C13A-C28A \\sim C13A-C1D
 with sigma of 0.04
 C27A-C26A \\sim C3-C1C
 with sigma of 0.04
 C27A-C28A \\sim C3-C1D
 with sigma of 0.04
 C26A-C28A \\sim C1C-C1D
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C25A \\sim C27A \\sim C26A \\sim C28A \\sim C3 \\sim C4 \\sim C1C \\sim C1D:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
4. Others
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=
 Sof(H1CC)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=1-FVAR(1)
 Sof(C25A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C26A)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C6B(H6B), C12B(H12B), C6(H6), C6A(H6A), C8B(H8B), C8A(H8A),
 C14B(H14B), C14A(H14A), C12(H12), C12A(H12A), C14(H14)
5.b Idealised Me refined as rotating group:
 C22(H22G,H22H,H22I), C24(H24G,H24H,H24I), C61B(H61D,H61E,H61F), C61A(H61A,
 H61B,H61C), C23(H23G,H23H,H23I), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F),
 C22B(H22D,H22E,H22F), C30B(H30D,H30E,H30F), C28B(H28D,H28E,H28F), C18A(H18A,
 H18B,H18C), C31B(H31D,H31E,H31F), C26(H26G,H26H,H26I), C24A(H24A,H24B,H24C),
 C22A(H22A,H22B,H22C), C42(H42G,H42H,H42I), C27(H27G,H27H,H27I), C20B(H20D,H20E,
 H20F), C26B(H26D,H26E,H26F), C19(H19G,H19H,H19I), C31A(H31A,H31B,H31C),
 C23A(H23A,H23B,H23C), C43(H43G,H43H,H43I), C18B(H18D,H18E,H18F), C32B(H32D,
 H32E,H32F), C30(H30G,H30H,H30I), C18(H18G,H18H,H18I), C27B(H27D,H27E,H27F),
 C32A(H32A,H32B,H32C), C41A(H41A,H41B,H41C), C28(H28G,H28H,H28I), C41(H41G,H41H,
 H41I), C19B(H19D,H19E,H19F), C31(H31G,H31H,H31I), C32(H32G,H32H,H32I),
 C20A(H20A,H20B,H20C), C30A(H30A,H30B,H30C), C19A(H19A,H19B,H19C), C42A(H42A,
 H42B,H42C), C43A(H43A,H43B,H43C), C20(H20G,H20H,H20I), C61(H61G,H61H,H61I),
 C42B(H42D,H42E,H42F), C27A(H27A,H27B,H27C), C41B(H41D,H41E,H41F), C43B(H43D,
 H43E,H43F), C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C3(H3A,H3B,H3C),
 C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 51 electrons were 
found in a volume of 1701\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.167[C6H14] per formula unit 
which account for 50 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78629
_shelx_fab_checksum              40002
_olex2_submission_special_instructions 'No special instructions were received'