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_7716252
_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 H39 Cl N O P Pd'
_chemical_formula_sum            'C26 H39 Cl N O P Pd'
_chemical_formula_weight         554.40
_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     iterative
_audit_creation_date             2022-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-15 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5669(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.87687(19)
_cell_length_b                   19.9674(4)
_cell_length_c                   14.8230(3)
_cell_measurement_reflns_used    13593
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.9410
_cell_measurement_theta_min      3.0730
_cell_volume                     2841.75(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -109.00 -37.00   0.50    0.16    --  -59.30 -15.00-150.00  144
  2  \w   -113.00 -55.00   0.50    0.16    --  -71.94 -15.00-180.00  116
  3  \w   -126.00 -45.00   0.50    0.16    --  -76.01 -15.00 -60.00  162
  4  \w    -81.00 -28.00   0.50    0.16    --  -76.01 111.00  60.00  106
  5  \w     29.00  57.00   0.50    0.16    --   76.52-111.00 -60.00   56
  6  \w     19.00  50.00   0.50    0.16    --   56.10 -95.00-180.00   62
  7  \w     37.00  62.00   0.50    0.16    --   84.37-111.00-120.00   50
  8  \w     48.00  83.00   0.50    0.16    --   76.52 -95.00 -90.00   70
  9  \w     43.00  68.00   0.50    0.16    --   84.37-111.00 -60.00   50
 10  \w     13.00  38.00   0.50    0.16    --   56.10 -95.00 -60.00   50
 11  \w     47.00  91.00   0.50    0.16    --   84.37 -95.00 -60.00   88
 12  \w     49.00  89.00   0.50    0.16    --   84.37 -95.00-180.00   80
 13  \w     37.00  80.00   0.50    0.16    --   76.52 -95.00   0.00   86
 14  \w     43.00  68.00   0.50    0.16    --   84.37 -90.00 -57.00   50
 15  \w     40.00  68.00   0.50    0.16    --   84.37-111.00  30.00   56
 16  \w     48.00  84.00   0.50    0.16    --   84.37 -95.00  30.00   72
 17  \w     34.00  59.00   0.50    0.16    --   76.52 -95.00  90.00   50
 18  \w     48.00  80.00   0.50    0.16    --   76.52 -95.00 120.00   64
 19  \w     37.00 101.00   0.50    0.16    --   56.10  15.00 120.00  128
 20  \w     49.00 132.00   0.50    0.16    --   84.37  15.00 -90.00  166
 21  \w     51.00  86.00   0.50    0.16    --   84.37  15.00-180.00   70
 22  \w     92.00 134.00   0.50    0.16    --   84.37  15.00-180.00   84
;
_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      0.0449166000
_diffrn_orient_matrix_UB_12      -0.0700912000
_diffrn_orient_matrix_UB_13      -0.0249277000
_diffrn_orient_matrix_UB_21      -0.1196102000
_diffrn_orient_matrix_UB_22      -0.0003682000
_diffrn_orient_matrix_UB_23      -0.0879849000
_diffrn_orient_matrix_UB_31      0.0970548000
_diffrn_orient_matrix_UB_32      0.0322541000
_diffrn_orient_matrix_UB_33      -0.0553972000
_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  0.0322
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20020
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.061
_diffrn_reflns_theta_max         67.061
_diffrn_reflns_theta_min         3.783
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.00076(19)
_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   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4619
_reflns_number_total             5079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00862f2.cif
_cod_data_source_block           220443lt_auto
_cod_depositor_comments
'Adding full bibliography for 7716247--7716254.cif.'
_cod_original_cell_volume        2841.74(10)
_cod_database_code               7716252
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.648
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8), C12(H12), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 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              30705
_shelx_hkl_checksum              70941
_shelx_fab_checksum              99808
_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 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.830