A Readily Accessible CH Anion Transfer Reagent for the Preparation of a Molybdenum Methylidyne Complex
Mukkera, Rajesh; Le, Nghia; Woo, Chandler I.; Webster, Charles Edwin; Creutz, Sidney E.; Chemical Science  (2026) –; doi:10.1039/D5SC07469J

data_1576607
_publ_section_title
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 A readily accessible CH anion transfer reagent for the preparation of a
 molybdenum methylidyne complex.
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_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              8780
_journal_page_last               8786
_journal_paper_doi               10.1039/d5sc07469j
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         '2(C16 H40 Mo N4 Si3)'
_chemical_formula_sum            'C32 H80 Mo2 N8 Si6'
_chemical_formula_weight         937.46
_chemical_name_systematic        (TMS-TREN)MoCH
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2025-03-27
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
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_audit_update_record
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2025-09-07 deposited with the CCDC.	2026-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8581(17)
_cell_length_b                   16.8406(17)
_cell_length_c                   34.208(3)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      2.42
_cell_volume                     9711.7(16)
_computing_cell_refinement       'APEX6 v2024.9.0'
_computing_data_collection       'APEX6 v2024.9.0'
_computing_data_reduction        'Saint, APEX6 v2024.9.0.'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            397235
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.529
_diffrn_reflns_theta_min         1.810
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.504
_exptl_crystal_size_mid          0.456
_exptl_crystal_size_min          0.363
_refine_diff_density_max         2.461
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         14811
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0315P)^2^+13.0914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12741
_reflns_number_total             14811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07469j2.cif
_cod_data_source_block           rm_2-113-final
_cod_depositor_comments          'Adding full bibliography for 1576607.cif.'
_cod_original_cell_volume        9711.8(17)
_cod_database_code               1576607
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.721
_olex2_refinement_description
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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. Uiso/Uaniso restraints and constraints
C23B \\sim C24B \\sim C25B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C23B) \\sim Ueq, Uanis(C24B) \\sim Ueq, Uanis(C25B) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.05
Uanis(C22A) = Uanis(C22B)
Uanis(C12A) = Uanis(C12B)
Uanis(C32A) = Uanis(C32B)
3. Rigid body (RIGU) restrains
 C23B, C24B, C25B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Same fragment restrains
{C21A, C22A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C21B, C22B}
{C11A, C12A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11B, C12B}
{C23A, C24A, C25A, Si2A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23B, C24B, C25B, Si2B}
{C31A, C32A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C31B, C32B}
5. Others
 Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C31B)=
 Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C11B)=Sof(H11C)=
 Sof(H11D)=Sof(C12B)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(Si2B)=1-FVAR(2)
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(Si2A)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C22A(H22A,H22B), C31A(H31A,H31B), C32A(H32A,H32B), C11A(H11A,
 H11B), C12A(H12A,H12B), C21B(H21C,H21D), C22B(H22C,H22D), C31B(H31C,H31D),
 C32B(H32C,H32D), C11B(H11C,H11D), C12B(H12C,H12D), C21(H21E,H21F), C22(H22E,
 H22F), C31(H31E,H31F), C32(H32E,H32F), C11(H11E,H11F), C12(H12E,H12F)
6.b Idealised Me refined as rotating group:
 C24(H24G,H24H,H24I), C23(H23G,H23H,H23I), C25(H25G,H25H,H25I), C23A(H23A,H23B,
 H23C), C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C23B(H23D,H23E,H23F),
 C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C33(H33D,H33E,H33F), C33A(H33A,
 H33B,H33C), C34(H34D,H34E,H34F), C34A(H34A,H34B,H34C), C35(H35D,H35E,H35F),
 C35A(H35A,H35B,H35C), C13(H13D,H13E,H13F), C13A(H13A,H13B,H13C), C14(H14D,H14E,
 H14F), C14A(H14A,H14B,H14C), C15(H15D,H15F,H15E), C15A(H15A,H15B,H15C)
6.c :
 C1(H1), C1A(H1A)
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_shelx_res_checksum              85014
_olex2_submission_special_instructions 'No special instructions were received'