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_7717367
_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 H43 F9 Mo N4 O3, C4 H8 O, 0.9[C4H10O1]'
_chemical_formula_sum            'C42.6 H60 F9 Mo N4 O4.9'
_chemical_formula_weight         973.48
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.409(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7763(10)
_cell_length_b                   10.5017(6)
_cell_length_c                   28.0439(18)
_cell_measurement_reflns_used    5145
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      22.998
_cell_measurement_theta_min      2.292
_cell_volume                     4909.9(5)
_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  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest, PhotonIII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            67721
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.069
_diffrn_reflns_theta_max         25.069
_diffrn_reflns_theta_min         2.072
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0692 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.8878.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             2023
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8700
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0774P)^2^+0.5937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6362
_reflns_number_total             8700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_155n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_original_formula_sum        'C42.60 H60 F9 Mo N4 O4.90'
_cod_database_code               7717367
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.966
_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. Restrained distances
 F4-C42 \\sim F4A-C42A
 with sigma of 0.02
 F6-C42 \\sim F6A-C42A
 with sigma of 0.02
 F5-C42 \\sim F5A-C42A
 with sigma of 0.02
 C40-C42 \\sim C40-C42A
 with sigma of 0.02
 F4-F6 \\sim F4A-F6A
 with sigma of 0.04
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 F4-C40 \\sim F4A-C40
 with sigma of 0.04
 F6-F5 \\sim F6A-F5A
 with sigma of 0.04
 F6-C40 \\sim F6A-C40
 with sigma of 0.04
 F5-C40 \\sim F5A-C40
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C42A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C42) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C42A)=Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(1)
 Sof(F4)=Sof(F6)=Sof(F5)=Sof(C42)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C103(H10C,H10D), C102(H10E,H10F), C101(H10G,H10H)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C12(H12), C14(H14)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C23(H23A,H23B,H23C), C61(H61A,H61B,
 H61C), C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C22(H22A,
 H22B,H22C), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C18(H18A,H18B,H18C),
 C26(H26A,H26B,H26C), C20(H20A,H20B,H20C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 152 electrons were 
found in a volume of 1420\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.9[C4H10O1] per formula unit 
which account for 151 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31430
_shelx_fab_checksum              56531
_olex2_submission_special_instructions 'No special instructions were received'