Synthesis of dihydroisoquinolinone-4-methylboronic esters via domino Heck/borylation using a structurally characterized palladacycle as a catalyst
Morla, Jhansi Rani; Nareddula, Dastagiri Reddy; RSC Advances 12 (2022) 6762–6771; doi:10.1039/D2RA00389A

data_7244528
_publ_section_title
;
 Synthesis of dihydroisoquinolinone-4-methylboronic esters via domino
 Heck/borylation using a structurally characterized palladacycle as a
 catalyst
;
_journal_issue                   11
_journal_name_full               'RSC Advances'
_journal_page_first              6762
_journal_page_last               6771
_journal_paper_doi               10.1039/D2RA00389A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C37 H29 Cl N5 O P Pd, 2(C3 H6 O)'
_chemical_formula_sum            'C43 H41 Cl N5 O3 P Pd'
_chemical_formula_weight         848.63
_chemical_name_systematic        Palladacycle
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-05-31T12:03:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2021-06-02 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.477(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5617(4)
_cell_length_b                   39.7290(15)
_cell_length_c                   10.2744(4)
_cell_measurement_reflns_used    9303
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.0274
_cell_measurement_theta_min      3.9173
_cell_volume                     3899.4(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0060303
_diffrn_orient_matrix_UB_12      -0.0147065
_diffrn_orient_matrix_UB_13      0.0384031
_diffrn_orient_matrix_UB_21      -0.0189738
_diffrn_orient_matrix_UB_22      -0.0093839
_diffrn_orient_matrix_UB_23      -0.0567314
_diffrn_orient_matrix_UB_31      0.0715106
_diffrn_orient_matrix_UB_32      -0.0037366
_diffrn_orient_matrix_UB_33      -0.0087908
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29580
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.104
_diffrn_reflns_theta_min         3.929
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.92838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN and acetone'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.243
_refine_diff_density_min         -3.942
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.1159
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+110.0319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2373
_reflns_Friedel_coverage         0
_reflns_number_gt                7615
_reflns_number_total             9220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra00389a2.cif
_cod_data_source_block           Palladacycle
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7244528
_shelx_shelxl_version_number     2018/3