Toward vanadium-mediated alkyne metathesis
Hernandez, Shirley; Krivovicheva, Vasilisa; Sousa-Silva, Adenilson; Solans-Monfort, Xavier; Bukhryakov, Konstantin V.; Chemical Science  (2026) –; doi:10.1039/D6SC01683A

data_1576942
_publ_section_title
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 Toward vanadium-mediated alkyne metathesis.
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_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              9132
_journal_page_last               9137
_journal_paper_doi               10.1039/d6sc01683a
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C47 H55 N2 O2 S Si2 V'
_chemical_formula_sum            'C47 H55 N2 O2 S Si2 V'
_chemical_formula_weight         819.11
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-06 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.874(2)
_cell_angle_gamma                90
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_cell_length_b                   30.044(3)
_cell_length_c                   13.4314(14)
_cell_measurement_reflns_used    8721
_cell_measurement_temperature    172(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.55
_cell_volume                     4424.4(8)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      172(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest Photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46652
_diffrn_reflns_point_group_measured_fraction_full 0.995
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_diffrn_reflns_theta_full        25.075
_diffrn_reflns_theta_max         25.075
_diffrn_reflns_theta_min         2.300
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether at --35?'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.270
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+3.8026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5254
_reflns_number_total             7811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc01683a3.cif
_cod_data_source_block           sh_sphome
_cod_depositor_comments
'Adding full bibliography for 1576939--1576943.cif.'
_cod_original_cell_volume        4424.3(8)
_cod_database_code               1576942
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.954
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C18(H18), C21(H21), C20(H20), C13(H13), C41(H41), C43(H43),
 C31(H31), C47(H47), C45(H45), C35(H35), C12(H12), C46(H46), C44(H44), C40(H40),
  C6(H6), C32(H32), C37(H37), C33(H33), C34(H34), C9(H9), C39(H39), C38(H38),
 C7(H7), C8(H8)
1.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C11(H11A,H11B,H11C), C4(H4A,
 H4B,H4C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              26071
_olex2_submission_original_sample_id SH_SPhOMe
_olex2_submission_special_instructions 'No special instructions were received'