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_7717361
_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         'C62 H86 Cl2 Mo2 N6 O4, 0.75(C7 H8)'
_chemical_formula_sum            'C67.25 H92 Cl2 Mo2 N6 O4'
_chemical_formula_weight         1311.24
_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             2024-03-04
_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                90.214(4)
_cell_angle_beta                 97.829(4)
_cell_angle_gamma                94.020(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0665(10)
_cell_length_b                   10.9440(11)
_cell_length_c                   30.514(3)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      25.486
_cell_measurement_theta_min      2.241
_cell_volume                     3321.8(6)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13717
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.536
_diffrn_reflns_theta_min         2.021
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1114 before and 0.0776 after correction.
The Ratio of minimum to maximum transmission is 0.9006.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             1375
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.578
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         13717
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0538P)^2^+29.7411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12646
_reflns_number_total             13717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_426n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_database_code               7717361
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7465(14)
 0.2535(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C61A
 1.5 with sigma of 0.02
 C106-C100
 1.54 with sigma of 0.02
 N2A-C61C
 1.5 with sigma of 0.02
 C100-C101
 1.39 with sigma of 0.01
 C101-C102
 1.39 with sigma of 0.01
 C102-C103
 1.39 with sigma of 0.01
 C103-C104
 1.39 with sigma of 0.01
 C104-C105
 1.39 with sigma of 0.01
 C105-C100
 1.39 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C61A \\sim N2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
C100 \\sim C106: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
C61 \\sim N3: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.7A
C61B \\sim N3A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(C100) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C106) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C61A)=Sof(H61J)=Sof(H61K)=Sof(H61L)=1-FVAR(1)
 Sof(C61)=Sof(H61D)=Sof(H61E)=Sof(H61F)=FVAR(1)
 Sof(C61C)=Sof(H61G)=Sof(H61H)=Sof(H61I)=1-FVAR(2)
 Sof(C61B)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(2)
 Fixed Sof: C100(0.75) C104(0.75) H104(0.75) C101(0.75) H101(0.75) C105(0.75)
 H105(0.75) C102(0.75) H102(0.75) C103(0.75) H103(0.75) C106(0.75) H10A(0.75)
 H10B(0.75) H10C(0.75)
6.a Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C6(H6), C12(H12), C14(H14), C8A(H8A), C12A(H12A), C8(H8),
 C14A(H14A), C104(H104), C101(H101), C105(H105), C102(H102), C103(H103)
6.b Idealised Me refined as rotating group:
 C30A(H30A,H30B,H30C), C24(H24A,H24B,H24C), C22A(H22A,H22B,H22C), C30(H30D,
 H30E,H30F), C28(H28A,H28B,H28C), C26A(H26A,H26B,H26C), C22(H22D,H22E,H22F),
 C19(H19A,H19B,H19C), C18A(H18A,H18B,H18C), C20(H20A,H20B,H20C), C24A(H24D,H24E,
 H24F), C32A(H32A,H32B,H32C), C32(H32D,H32E,H32F), C27A(H27A,H27B,H27C),
 C61B(H61A,H61B,H61C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C27(H27D,H27E,
 H27F), C20A(H20D,H20E,H20F), C31A(H31D,H31E,H31F), C61(H61D,H61E,H61F),
 C23A(H23D,H23E,H23F), C26(H26D,H26E,H26F), C18(H18D,H18E,H18F), C19A(H19D,H19E,
 H19F), C28A(H28D,H28E,H28F), C106(H10A,H10B,H10C), C61C(H61G,H61H,H61I),
 C61A(H61J,H61K,H61L)
;
_shelx_res_checksum              32890
_olex2_submission_special_instructions 'No special instructions were received'