A facile approach to C-functionalized β-ketoimine compounds via terminal alkylation of a tetralithiated intermediate
Zhou, Shuai; Xu, Xiaojuan; Zhu, Xu; Zheng, Yu; Chen, Sufang; Xue, Mingqiang; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB00640E

data_7158701
_publ_section_title
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 A facile approach to C-functionalized \b-ketoimine compounds via terminal
 alkylation of a tetralithiated intermediate
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_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB00640E
_journal_year                    2022
_chemical_formula_moiety         '0.5(C48 H68 Li4 N4 O8)'
_chemical_formula_sum            'C24 H34 Li2 N2 O4'
_chemical_formula_weight         428.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-01-09
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2022-05-05 deposited with the CCDC.	2022-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                99.394(3)
_cell_angle_beta                 94.887(3)
_cell_angle_gamma                93.080(3)
_cell_formula_units_Z            4
_cell_length_a                   10.4007(11)
_cell_length_b                   13.6605(15)
_cell_length_c                   17.5771(19)
_cell_measurement_reflns_used    4541
_cell_measurement_temperature    128.01
_cell_measurement_theta_max      22.70
_cell_measurement_theta_min      2.20
_cell_volume                     2449.1(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      128.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.3262
_diffrn_reflns_av_unetI/netI     0.1719
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44384
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.756
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.100
_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         8661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1825
_refine_ls_R_factor_gt           0.0969
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1664P)^2^+0.0439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2569
_refine_ls_wR_factor_ref         0.3327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4240
_reflns_number_total             8661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob00640e2.cif
_cod_data_source_block           mo_b200801b_0m
_cod_database_code               7158701
_publcif_datablock.id            {70fcef60-a7d2-4c1e-9d0b-b301dfad0704}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.977
_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:
 C39(H39a,H39b), C43(H43a,H43b), C37(H37a,H37b), C40(H40a,H40b), C38(H38a,
 H38b), C12(H12a,H12b), C36(H36a,H36b), C15(H15a,H15b), C42(H42a,H42b),
 C16(H16a,H16b), C13(H13a,H13b), C14(H14a,H14b), C41(H41a,H41b), C19(H19a,H19b),
  C17(H17a,H17b), C18(H18a,H18b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C9(H9), C4(H4), C46(H46), C28(H28), C26(H26), C33(H33),
 C6(H6), C25(H25), C30(H30), C22(H22)
2.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C11(H11a,H11b,H11c), C48(H48a,H48b,H48c), C35(H35a,H35b,
 H35c), C31(H31a,H31b,H31c), C44(H44a,H44b,H44c), C20(H20a,H20b,H20c), C24(H24a,
 H24b,H24c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37119
_shelx_fab_checksum              8125
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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