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_7716251
_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         'C34 H32 Cl N2 O4 P Pd'
_chemical_formula_sum            'C34 H32 Cl N2 O4 P Pd'
_chemical_formula_weight         705.43
_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             2022-04-19
_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                 98.1770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4769(2)
_cell_length_b                   10.10810(10)
_cell_length_c                   17.5375(3)
_cell_measurement_reflns_used    9665
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.4370
_cell_measurement_theta_min      3.3050
_cell_volume                     3066.65(7)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.953
_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     69.00 103.00   0.50   10.00    --   56.31  15.00 120.00   68
  2  \w     14.00  39.00   0.50   10.00    --   56.31 -95.00-150.00   50
  3  \w     37.00  63.00   0.50   10.00    --   56.31  15.00-120.00   52
  4  \w     79.00 107.00   0.50   10.00    --   56.31  15.00-120.00   56
  5  \w    -43.00 -15.00   0.50   10.00    --  -59.30 125.00-180.00   56
  6  \w    -74.00 -48.00   0.50   10.00    --  -76.01 -15.00  60.00   52
  7  \w   -121.00 -51.00   0.50   10.00    --  -76.01 -15.00 -90.00  140
  8  \w    -92.00 -34.00   0.50   10.00    --  -76.01 111.00-120.00  116
  9  \w   -114.00 -55.00   0.50   10.00    --  -76.01 -15.00 -30.00  118
 10  \w   -120.00 -93.00   0.50   10.00    --  -76.01 -15.00  60.00   54
 11  \w     35.00  76.00   0.50   10.00    --   76.52 -95.00  30.00   82
 12  \w     38.00  79.00   0.50   10.00    --   76.52 -95.00  90.00   82
 13  \w     62.00  89.00   0.50   10.00    --   84.37 -95.00   0.00   54
 14  \w     51.00  91.00   0.50   10.00    --   84.37 -95.00 120.00   80
 15  \w     48.00 134.00   0.50   10.00    --   84.37  15.00 -30.00  172
 16  \w     56.00 135.00   0.50   10.00    --   84.37  15.00-120.00  158
 17  \w     59.00  85.00   0.50   10.00    --   84.37 -95.00-120.00   52
 18  \w     37.00  92.00   0.50   10.00    --   84.37-111.00 -30.00  110
;
_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      0.0699941000
_diffrn_orient_matrix_UB_12      -0.0528864000
_diffrn_orient_matrix_UB_13      -0.0350485000
_diffrn_orient_matrix_UB_21      0.0456075000
_diffrn_orient_matrix_UB_22      -0.0150057000
_diffrn_orient_matrix_UB_23      0.0814194000
_diffrn_orient_matrix_UB_31      -0.0308866000
_diffrn_orient_matrix_UB_32      -0.1420960000
_diffrn_orient_matrix_UB_33      0.0044811000
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18536
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.086
_diffrn_reflns_theta_min         3.340
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89852
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.551
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.849
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.849
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0320
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5271
_reflns_number_total             6031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00862f2.cif
_cod_data_source_block           2203106lt_auto
_cod_depositor_comments
'Adding full bibliography for 7716247--7716254.cif.'
_cod_database_code               7716251
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.356
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25),
  C26(H26), C29(H29), C30(H30), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              3458
_shelx_hkl_checksum              49173
_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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.791