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_7717365
_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 H52 Mo N4 O3'
_chemical_formula_sum            'C35 H52 Mo N4 O3'
_chemical_formula_weight         672.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-04
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9259(3)
_cell_length_b                   19.4438(7)
_cell_length_c                   31.0776(13)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      2.622
_cell_volume                     3580.8(3)
_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 0.999
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            39210
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         2.195
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1289 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.7632.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+2.6426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3286
_reflns_number_total             3746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_168n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_database_code               7717365
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.906
_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. Shared sites
{C2, N2}
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(N2)
4. Others
 Fixed Sof: C2(0.5) H41B(0.5) H41C(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
 N2(0.5)
5.a Me refined with riding coordinates:
 C41(H41A,H41B,H41C)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8)
5.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C42(H42A,H42B,H42C), C61(H61A,
 H61B,H61C)
;
_shelx_res_checksum              76370
_olex2_submission_special_instructions 'No special instructions were received'