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_7717359
_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         'C39 H44 F9 Mo N3 O3, C4 H8 O, 0.6[C4H10O]'
_chemical_formula_sum            'C45.4 H58 F9 Mo N3 O4.6'
_chemical_formula_weight         986.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_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                   23.4925(19)
_cell_length_b                   9.8772(9)
_cell_length_c                   20.6824(15)
_cell_measurement_reflns_used    6043
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      24.424
_cell_measurement_theta_min      2.237
_cell_volume                     4799.1(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      153.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.1261
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            100217
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.990
_diffrn_reflns_theta_min         2.237
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0909 before and 0.0498 after correction.
The Ratio of minimum to maximum transmission is 0.8900.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       plate
_exptl_crystal_F_000             2045
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0543
_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^)+(0.1042P)^2^+3.9846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3665
_reflns_number_total             4844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02405b2.cif
_cod_data_source_block           sh_429_ortho
_cod_depositor_comments
'Adding full bibliography for 7717356--7717372.cif.'
_cod_original_formula_sum        'C45.40 H58 F9 Mo N3 O4.60'
_cod_database_code               7717359
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O100-C100 = O100-C103
 1.44 with sigma of 0.02
 C100-C101 = C102-C103
 1.53 with sigma of 0.02
 C101-C102
 1.54 with sigma of 0.02
 O100-C101 = O100-C102 = C100-C102 = C101-C103
 2.38 with sigma of 0.04
 C41-F41 \\sim C41-F42 \\sim C41-F40
 with sigma of 0.02
 F45-C42 \\sim F45A-C42A
 with sigma of 0.02
 C40-C42 \\sim C40-C42A
 with sigma of 0.02
 C42-F44 \\sim C42A-F44A
 with sigma of 0.02
 F41-F42 \\sim F42-F40 \\sim F40-F41
 with sigma of 0.03
 C100-C101 \\sim C101-C102 \\sim C102-C103
 with sigma of 0.02
 O100-C100 \\sim O100-C103
 with sigma of 0.02
 O100-C101 \\sim O100-C102
 with sigma of 0.04
 C101-C103 \\sim C100-C102
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C42A \\sim C42: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
C41 \\sim F41 \\sim F42 \\sim F40: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
O100 \\sim C100 \\sim C101 \\sim C102 \\sim C103: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O100, C100, C101, C102, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C42A)=Sof(F44A)=Sof(F45A)=1-FVAR(1)
 Sof(F45)=Sof(C42)=Sof(F44)=FVAR(1)
 Fixed Sof: O100(0.5) C100(0.5) H10A(0.5) H10B(0.5) C101(0.5) H10C(0.5)
 H10D(0.5) C102(0.5) H10E(0.5) H10F(0.5) C103(0.5) H10G(0.5) H10H(0.5) C41(0.5)
 F41(0.5) F42(0.5) F40(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C4(H4), C3(H3)
6.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 92 electrons were 
found in a volume of 890\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.6[C4H10O] per formula unit 
which account for 101 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69612
_shelx_fab_checksum              24882
_olex2_submission_special_instructions 'No special instructions were received'