Regioselective Synthesis of Chromones via Cyclocarbonylative Sonogashira Coupling Catalyzed by Highly Active Bridged-Bis(N-Heterocyclic Carbene)Palladium(II) Complexes.
Mansour, Waseem; Fettouhi, Mohammed; El Ali, Bassam; ACS omega 5 (2020) 32515–32529; doi:10.1021/acsomega.0c04706

data_4518294
_publ_section_title
;
 Regioselective Synthesis of Chromones via Cyclocarbonylative Sonogashira
 Coupling Catalyzed by Highly Active Bridged-Bis(N-Heterocyclic
 Carbene)Palladium(II) Complexes.
;
_journal_issue                   50
_journal_name_full               'ACS omega'
_journal_page_first              32515
_journal_page_last               32529
_journal_paper_doi               10.1021/acsomega.0c04706
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C31 H28 Br2 N4 Pd, C H2 Cl2, H2O'
_chemical_formula_sum            'C32 H32 Br2 Cl2 N4 O Pd'
_chemical_formula_weight         825.73
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yb'
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_cell_angle_beta                 92.033(2)
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_cell_measurement_theta_max      25.186
_cell_measurement_theta_min      2.419
_cell_volume                     3374.0(5)
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_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 2017)'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
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_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS D8 Quest diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_k_min       -31
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_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.367
_diffrn_reflns_theta_min         2.564
_diffrn_source                   'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.108
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS. Ver. 2014/5. (Krause et al., 2015)'
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.120
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     399
_refine_ls_number_reflns         8604
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0903P)^2^+17.1993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.2298
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_reflns_number_gt                5336
_reflns_number_total             8604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c04706_si_002.cif
_cod_data_source_block           W500
_cod_depositor_comments
'Adding full bibliography for 4518294--4518295.cif.'
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4518294
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.436
_shelx_estimated_absorpt_t_max   0.746
_shelx_res_checksum              84616
_shelx_hkl_checksum              82745