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_1576939
_publ_section_title
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 Toward vanadium-mediated alkyne metathesis.
;
_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         'C37 H48 N O Si3 V'
_chemical_formula_sum            'C37 H48 N O Si3 V'
_chemical_formula_weight         657.97
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-10-06 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8811(7)
_cell_length_b                   14.3289(9)
_cell_length_c                   22.4754(14)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    172(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.54
_cell_volume                     3767.2(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40057
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.063
_diffrn_reflns_theta_max         25.063
_diffrn_reflns_theta_min         2.310
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentanes at --35?'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0387P)^2^+2.2256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5442
_reflns_number_total             6662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc01683a3.cif
_cod_data_source_block           sh_661_1
_cod_depositor_comments
'Adding full bibliography for 1576939--1576943.cif.'
_cod_database_code               1576939
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.927
_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 Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C14(H14), C13(H13), C37(H37), C31(H31), C27(H27),
 C21(H21), C36(H36), C30(H30), C25(H25), C22(H22), C23(H23), C29(H29), C35(H35),
  C33(H33), C28(H28), C24(H24), C34(H34)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C),
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              81244
_olex2_submission_original_sample_id SH_661_1
_olex2_submission_special_instructions 'No special instructions were received'