CuCl<sub>2</sub>·2H<sub>2</sub>O/TBHP mediated synthesis of β-enaminones <i>via</i> coupling reaction of vinyl azides with aldehydes.
Zhang, Yaohong; Luo, Mengqiang; Zhang, Yichan; Cheng, Kai; Li, Yong; Qi, Chenze; Shen, Runpu; Wang, Hai; Organic & biomolecular chemistry 20 (2022) 1952–1957; doi:10.1039/d1ob02479e

data_7158510
_publ_section_title
;
 CuCl<sub>2</sub>&#x00B7;2H<sub>2</sub>O/TBHP mediated synthesis of
 \b-enaminones <i>via</i> coupling reaction of vinyl azides with
 aldehydes.
;
_journal_issue                   9
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1952
_journal_page_last               1957
_journal_paper_doi               10.1039/d1ob02479e
_journal_volume                  20
_journal_year                    2022
_chemical_formula_sum            'C24 H21 N O2'
_chemical_formula_weight         355.42
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2022-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                97.864(2)
_cell_angle_beta                 108.797(2)
_cell_angle_gamma                103.162(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8259(3)
_cell_length_b                   9.8256(2)
_cell_length_c                   10.8672(3)
_cell_measurement_reflns_used    11380
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      74.1990
_cell_measurement_theta_min      4.3940
_cell_volume                     941.65(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20561
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         4.41
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.37791
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            coloreless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.383
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2185
_refine_ls_wR_factor_ref         0.2913
_reflns_number_gt                2887
_reflns_number_total             3333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1ob02479e2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7158510.cif.
;
_cod_original_cell_volume        941.65(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7158510