Synthesis of unsymmetrical ketones via dual catalysed cross-coupling of α,β-unsaturated carboxylic acids with aryldiazonium salts
Chand, Shiv; Sharma, Anup Kumar; Pandey, Anand Kumar; Singh, Krishna Nand; Chemical Communications  (2023) –; doi:10.1039/D3CC04898E

data_7132376
_publ_section_title
;
 Synthesis of unsymmetrical ketones via dual catalysed cross-coupling of
 \a,\b-unsaturated carboxylic acids with aryldiazonium salts
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04898E
_journal_year                    2023
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_audit_update_record
;
2023-05-12 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.136(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.9049(5)
_cell_length_b                   23.030(3)
_cell_length_c                   11.4621(12)
_cell_measurement_temperature    296(2)
_cell_volume                     1030.1(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.927
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
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_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       3
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_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.306
_diffrn_reflns_theta_min         3.839
_exptl_absorpt_coefficient_mu    1.157
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_F_000             462
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0045(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0652P)^2^+2.3690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1270
_reflns_number_total             1756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04898e2.cif
_cod_data_source_block           data1_a
_cod_depositor_comments
;

2025-01-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C H N O'
_cod_original_formula_weight         43.03
_cod_original_formula_units_Z            21
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7132376
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              41184
_shelx_hkl_checksum              9415