Design and synthesis of versatile ligand precursors based on phosphonium ylides for palladalactam formation and catalytic investigation.
Kao, Cheng-Po; Lee, Jhen-Yi; Tang, Min-Cheng; Lee, Hon Man; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10475–10485; doi:10.1039/d4dt00862f

data_7716250
_publ_section_title
;
 Design and synthesis of versatile ligand precursors based on phosphonium
 ylides for palladalactam formation and catalytic investigation.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10475
_journal_page_last               10485
_journal_paper_doi               10.1039/d4dt00862f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H21 Cl N O P Pd'
_chemical_formula_sum            'C26 H21 Cl N O P Pd'
_chemical_formula_weight         536.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-03-15 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.783(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2817(11)
_cell_length_b                   9.8382(8)
_cell_length_c                   17.6371(12)
_cell_measurement_reflns_used    9323
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.0840
_cell_measurement_theta_min      3.4710
_cell_volume                     2396.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     18.00  76.00   0.50    3.44    --   57.89-125.00  60.00  116
  2  \w     48.00  92.00   0.50    3.44    --   57.89  15.00-120.00   88
  3  \w     21.00  59.00   0.50    3.44    --   57.89-125.00 -30.00   76
  4  \w   -105.00 -76.00   0.50    3.44    --  -60.97 -15.00  60.00   58
  5  \w    -73.00 -44.00   0.50    3.44    --  -60.97 -15.00  60.00   58
  6  \w    -68.00 -31.00   0.50    3.44    --  -73.68 125.00  60.00   74
  7  \w    -95.00 -44.00   0.50    3.44    --  -73.68 125.00 120.00  102
  8  \w   -115.00 -84.00   0.50    3.44    --  -73.68 -15.00-180.00   62
  9  \w    -83.00 -31.00   0.50    3.44    --  -73.68 125.00-150.00  104
 10  \w   -112.00 -63.00   0.50    3.44    --  -74.02 -15.00 -60.00   98
 11  \w     53.00 118.00   0.50    3.44    --   74.39  15.00-120.00  130
 12  \w     82.00 119.00   0.50    3.44    --   74.39  15.00 -30.00   74
 13  \w    -98.00 -71.00   0.50    3.44    --  -78.57 119.00-121.70   54
 14  \w    -98.00 -73.00   0.50    3.44    --  -78.57 119.00-149.39   50
 15  \w    -71.00 -45.00   0.50    3.44    --  -78.57 115.00-105.66   52
 16  \w    -68.00 -37.00   0.50    3.44    --  -78.57 117.00 153.62   62
 17  \w     43.00  95.00   0.50    3.44    --   78.57-114.00-108.27  104
 18  \w     41.00  98.00   0.50    3.44    --   78.57-120.00 173.82  114
 19  \w     72.00  97.00   0.50    3.44    --   78.57-117.00-154.69   50
 20  \w     72.00  97.00   0.50    3.44    --   78.57-116.00-126.08   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0400618000
_diffrn_orient_matrix_UB_12      0.1339289000
_diffrn_orient_matrix_UB_13      0.0244967000
_diffrn_orient_matrix_UB_21      0.0824419000
_diffrn_orient_matrix_UB_22      0.0789224000
_diffrn_orient_matrix_UB_23      -0.0219891000
_diffrn_orient_matrix_UB_31      -0.0637379000
_diffrn_orient_matrix_UB_32      0.0179945000
_diffrn_orient_matrix_UB_33      -0.0841014000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14396
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.752
_diffrn_reflns_theta_min         3.568
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.33a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00040(6)
_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   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+3.1608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4110
_reflns_number_total             4538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00862f2.cif
_cod_data_source_block           220283lt_auto
_cod_depositor_comments
'Adding full bibliography for 7716247--7716254.cif.'
_cod_database_code               7716250
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Pd P Cl'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31875
_shelx_hkl_checksum              60005
_shelx_fab_checksum              75269
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.163
_oxdiff_exptl_absorpt_empirical_full_min 0.596