Formation of tungsten ethylidene complexes from diethyl complexes through a proton-catalyzed rearrangement of ethylene.
Maji, Milan; Zeng, Landley; Schrock, Richard R.; Conley, Matthew P.; Carta, Veronica; Chemical science 17 (2026) 421–429; doi:10.1039/d5sc07302b

data_1576725
_publ_section_title
;
 Formation of tungsten ethylidene complexes from diethyl complexes through
 a proton-catalyzed rearrangement of ethylene.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              421
_journal_page_last               429
_journal_paper_doi               10.1039/d5sc07302b
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C28 H44 N2 W'
_chemical_formula_sum            'C28 H44 N2 W'
_chemical_formula_weight         592.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-08-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-01-24 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.6806(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3829(9)
_cell_length_b                   18.8032(13)
_cell_length_c                   22.2737(15)
_cell_measurement_reflns_used    9347
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      3.13
_cell_volume                     5369.1(6)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            100571
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.272
_diffrn_reflns_theta_min         3.133
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.075
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1413 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.6650.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_preparation       synthesized
_exptl_crystal_recrystallization_method 'slow cooling of pentane at 30 C'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0089P)^2^+10.3598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9674
_reflns_number_total             9678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07302b1.cif
_cod_data_source_block           cu_mc3lz_0m
_cod_database_code               1576725
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.341
_shelx_estimated_absorpt_t_min   0.164
_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.a Ternary CH refined with riding coordinates:
 C19A(H19A), C14A(H14A), C7A(H7A), C19(H19), C26(H26), C7(H7), C26A(H26A),
 C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C3(H3A,H3B), C1(H1A,H1B), C1A(H1AA,H1AB)
2.c Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C23A(H23A), C10(H10), C22A(H22A), C24(H24), C12A(H12A), C12(H12),
 C10A(H10A), C11(H11), C23(H23), C22(H22), C11A(H11A)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C2A(H2AA,H2AB,H2AC), C21A(H21D,H21E,H21F), C2(H2A,H2B,
 H2C), C9A(H9AA,H9AB,H9AC), C9(H9A,H9B,H9C), C27A(H27D,H27E,H27F), C15A(H15D,
 H15E,H15F), C21(H21A,H21B,H21C), C4(H4A,H4B,H4C), C20A(H20D,H20E,H20F),
 C16A(H16D,H16E,H16F), C16(H16A,H16B,H16C), C8A(H8AA,H8AB,H8AC), C28A(H28D,H28E,
 H28F), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C4A(H4AA,
 H4AB,H4AC), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              3520
_olex2_submission_special_instructions 'No special instructions were received'