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_7717356
_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         'C50 H58 Mo N4 O2 S'
_chemical_formula_sum            'C50 H58 Mo N4 O2 S'
_chemical_formula_weight         875.00
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2023-05-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-06-23 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                81.921(5)
_cell_angle_beta                 85.646(5)
_cell_angle_gamma                86.098(5)
_cell_formula_units_Z            2
_cell_length_a                   9.3240(16)
_cell_length_b                   11.1134(18)
_cell_length_c                   23.386(4)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.19
_cell_volume                     2388.3(7)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      153.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16723
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.169
_diffrn_reflns_theta_max         25.169
_diffrn_reflns_theta_min         2.159
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1162 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.8749.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Flack x determined using 6449 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.036(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         16723
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0929P)^2^+4.8446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                15095
_reflns_number_total             16723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_219n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_original_cell_volume        2388.2(7)
_cod_database_code               7717356
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.826(3)
 0.174(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C18A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C12(H12), C6A(H6A), C42(H42), C42A(H42A), C6(H6), C54A(H54A),
 C8A(H8A), C48A(H48A), C46(H46), C14A(H14A), C52(H52), C46A(H46A), C52A(H52A),
 C8(H8), C54(H54), C14(H14), C58A(H58A), C43A(H43A), C49(H49), C49A(H49A),
 C43(H43), C55A(H55A), C48(H48), C57A(H57A), C56(H56), C51A(H51A), C50A(H50A),
 C58(H58), C55(H55), C45A(H45A), C44(H44), C56A(H56A), C51(H51), C44A(H44A),
 C57(H57), C50(H50), C45(H45)
4.b Idealised Me refined as rotating group:
 C32A(H32A,H32B,H32C), C28A(H28A,H28B,H28C), C31A(H31A,H31B,H31C), C31(H31D,
 H31E,H31F), C27(H27D,H27E,H27F), C22(H22D,H22E,H22F), C30(H30D,H30E,H30F),
 C23(H23D,H23E,H23F), C24A(H24A,H24B,H24C), C26(H26D,H26E,H26F), C23A(H23A,H23B,
 H23C), C24(H24D,H24E,H24F), C22A(H22A,H22B,H22C), C32(H32D,H32E,H32F),
 C27A(H27A,H27B,H27C), C26A(H26A,H26B,H26C), C30A(H30A,H30B,H30C), C28(H28D,
 H28E,H28F), C18(H18D,H18E,H18F), C18A(H18A,H18B,H18C), C61A(H61A,H61B,H61C),
 C19(H19D,H19E,H19F), C20(H20D,H20E,H20F), C20A(H20A,H20B,H20C), C61(H61D,H61E,
 H61F), C19A(H19A,H19B,H19C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66060
_shelx_fab_checksum              46894
_olex2_submission_special_instructions 'No special instructions were received'