Vanadium-catalysed regioselective hydroboration of epoxides for synthesis of secondary alcohols
Zhang, Guoqi; Neary, Michelle C.; Zeng, Haisu; Zheng, Shengping; Tang, Quan; Ates, Selin; Dalton Transactions  (2023) –; doi:10.1039/D3DT01865B

data_7713667
_publ_section_title
;
 Vanadium-catalysed regioselective hydroboration of epoxides for synthesis
 of secondary alcohols
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01865B
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H23 Cl3 N3 O2 V, C4 H8 O'
_chemical_formula_sum            'C21 H31 Cl3 N3 O3 V'
_chemical_formula_weight         530.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-06-01 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4989(5)
_cell_length_b                   12.5715(5)
_cell_length_c                   15.7661(6)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      2.30
_cell_volume                     2477.33(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            80912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         34.302
_diffrn_reflns_theta_min         2.584
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.7093
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         10059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0399P)^2^+0.8434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                8527
_reflns_number_total             10059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01865b2.cif
_cod_data_source_block           gz1504
_cod_database_code               7713667
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.763
_shelx_estimated_absorpt_t_max   0.902
_shelx_res_checksum              26607