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_7717358
_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         'C44 H55 Mo N3 O3'
_chemical_formula_sum            'C44 H55 Mo N3 O3'
_chemical_formula_weight         769.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-03
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6804)
;
_audit_update_record
;
2024-06-23 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.051(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.202(4)
_cell_length_b                   13.0643(10)
_cell_length_c                   18.5211(17)
_cell_measurement_reflns_used    2631
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      21.72
_cell_measurement_theta_min      2.20
_cell_volume                     8022.3(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1445
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44014
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.392
_diffrn_reflns_theta_min         2.202
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.8742.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8212
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+26.0118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5487
_reflns_number_total             8212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_289n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_original_cell_volume        8022.4(13)
_cod_database_code               7717358
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.913
_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
 C32-C35 \\sim C32-C35A
 with sigma of 0.02
 C32-C33 \\sim C32-C33A
 with sigma of 0.02
 C32-C34 \\sim C32-C34A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33A) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C17(H17), C11(H11), C4(H4), C44(H44), C9(H9), C6(H6),
 C5(H5), C42(H42)
5.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C46(H46A,H46B,H46C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C23(H23A,
 H23B,H23C), C30(H30A,H30B,H30C), C35(H35A,H35B,H35C), C21(H21A,H21B,H21C),
 C31(H31A,H31B,H31C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35A(H35D,H35E,H35F), C34A(H34D,H34E,H34F), C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              82140
_olex2_submission_special_instructions 'No special instructions were received'