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_7717366
_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         'C40 H54 Mo N4 O3, 1.5(C6 H6)'
_chemical_formula_sum            'C49 H63 Mo N4 O3'
_chemical_formula_weight         851.97
_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             2023-01-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2024-06-23 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                95.467(2)
_cell_angle_beta                 107.910(2)
_cell_angle_gamma                109.900(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3406(6)
_cell_length_b                   13.6168(7)
_cell_length_c                   15.6475(9)
_cell_measurement_reflns_used    7950
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      25.517
_cell_measurement_theta_min      2.378
_cell_volume                     2293.1(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.999
_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  0.0968
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            78746
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.452
_diffrn_reflns_theta_min         1.897
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0955 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.9238.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0450P)^2^+1.9141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7786
_reflns_number_total             9426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_149n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_database_code               7717366
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.922
_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.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C44(H44), C12(H12), C14(H14), C42(H42), C104(H104),
 C100(H100), C105(H105), C101(H101), C103(H103), C102(H102), C202(H202),
 C201(H201), C200(H200)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C24(H24A,H24B,H24C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C48(H48A,H48B,H48C), C23(H23A,H23B,H23C), C18(H18A,
 H18B,H18C), C20(H20A,H20B,H20C), C46(H46A,H46B,H46C), C61(H61A,H61B,H61C),
 C47(H47A,H47B,H47C), C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              44539
_olex2_submission_special_instructions 'No special instructions were received'