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_7717362
_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         'C70 H88 Cl2 Mo2 N4 O4, 0.6[C4H10O]'
_chemical_formula_sum            'C72.4 H94 Cl2 Mo2 N4 O4.6'
_chemical_formula_weight         1356.69
_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             2024-02-08
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.01.24 svn.r2f8d729c for OlexSys, GUI svn.r6923)
;
_audit_update_record
;
2024-06-23 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                103.777(6)
_cell_angle_beta                 100.008(6)
_cell_angle_gamma                104.777(6)
_cell_formula_units_Z            2
_cell_length_a                   13.0612(17)
_cell_length_b                   16.0524(18)
_cell_length_c                   18.038(2)
_cell_measurement_reflns_used    3312
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      25.044
_cell_measurement_theta_min      2.284
_cell_volume                     3439.1(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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Quest, Photon III'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2026
_diffrn_reflns_av_unetI/netI     0.2139
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45614
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.147
_diffrn_reflns_theta_max         25.147
_diffrn_reflns_theta_min         2.075
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1482 before and 0.0904 after correction.
The Ratio of minimum to maximum transmission is 0.7959.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       needle
_exptl_crystal_F_000             1422
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         12246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0718
_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^)+(0.0257P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6189
_reflns_number_total             12246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_403n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_original_formula_sum        'C72.40 H94 Cl2 Mo2 N4 O4.60'
_cod_database_code               7717362
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.846
_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:
 C11A(H11A), C9A(H9A), C6(H6), C5A(H5A), C17A(H17A), C17(H17), C4(H4),
 C15A(H15A), C9(H9), C6A(H6A), C15(H15), C5(H5), C3A(H3A), C4A(H4A), C11(H11),
 C3(H3)
2.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C29A(H29A,H29B,H29C), C26(H26A,H26B,
 H26C), C25A(H25A,H25B,H25C), C31A(H31A,H31B,H31C), C33A(H33D,H33E,H33F),
 C34(H34A,H34B,H34C), C27A(H27A,H27B,H27C), C30A(H30A,H30B,H30C), C21(H21A,H21B,
 H21C), C25(H25D,H25E,H25F), C23A(H23A,H23B,H23C), C34A(H34D,H34E,H34F),
 C27(H27D,H27E,H27F), C35A(H35D,H35E,H35F), C22A(H22A,H22B,H22C), C22(H22D,H22E,
 H22F), C26A(H26D,H26E,H26F), C23(H23D,H23E,H23F), C21A(H21D,H21E,H21F),
 C31(H31D,H31E,H31F), C29(H29D,H29E,H29F), C30(H30D,H30E,H30F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 55 electrons were 
found in a volume of 483\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.6[C4H10O] per Asymmetric Unit 
which account for 50 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51666
_shelx_fab_checksum              82328
_olex2_submission_special_instructions 'No special instructions were received'