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_7717372
_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 H44 Cl Mo N3 O2'
_chemical_formula_sum            'C35 H44 Cl Mo N3 O2'
_chemical_formula_weight         670.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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            8
_cell_length_a                   13.7921(6)
_cell_length_b                   16.5408(8)
_cell_length_c                   29.0621(13)
_cell_measurement_reflns_used    5020
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.03
_cell_volume                     6630.0(5)
_computing_cell_refinement       'Bruker Apex3 suite, 2019'
_computing_data_collection       'Bruker Apex3 suite, 2019'
_computing_data_reduction        'Bruker Apex3 suite, 2019'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            95100
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.367
_diffrn_reflns_theta_min         2.036
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1729 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.8831.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0173P)^2^+14.3277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5020
_reflns_number_total             6071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_0003n_0m
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_database_code               7717372
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details   'Blessing, 1995'
_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:
 C9(H9), C3(H3), C15(H15), C17(H17), C6(H6), C11(H11), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C31(H31A,H31B,
 H31C), C26(H26A,H26B,H26C), C33(H33A,H33B,H33C), C22(H22A,H22B,H22C), C27(H27A,
 H27B,H27C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C),
 C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'