Synthesis, characterization, and reactivity of [Pd(phosphine)(py)Cl2] (PEPPSI) and [Pd(phosphine)Cl2]2 com-plexes
Nolan, Steven P.; Voloshkin, Vladislav; Belis, Marek; Cazin, Catherine; Peng, Min; Liu, Yaxu; Van Hecke, Kristof; Dalton Transactions  (2023) –; doi:10.1039/D3DT00293D

data_7712313
_publ_section_title
;
 Synthesis, characterization, and reactivity of [Pd(phosphine)(py)Cl2]
 (PEPPSI) and [Pd(phosphine)Cl2]2 com-plexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00293D
_journal_year                    2023
_chemical_formula_moiety         'C31 H39 Cl3 N O2 P Pd'
_chemical_formula_sum            'C31 H39 Cl3 N O2 P Pd'
_chemical_formula_weight         701.35
_chemical_name_systematic        VL203
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.74090(10)
_cell_length_b                   16.5403(2)
_cell_length_c                   21.5878(3)
_cell_measurement_reflns_used    13582
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.4940
_cell_measurement_theta_min      3.3360
_cell_volume                     3121.10(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -87.00  -6.00   1.00    1.00    --  -41.68 125.00-180.00   81
  2  \w    -87.00  -6.00   1.00    1.00    --  -41.68 125.00   0.00   81
  3  \w     27.00  98.00   1.00    1.00    --   41.68-125.00-150.00   71
  4  \w     80.00 178.00   1.00    2.00    --  106.01  45.00   0.00   98
  5  \w     30.00 139.00   1.00    2.00    --  106.01 -77.00   0.00  109
  6  \w    103.00 178.00   1.00    2.00    --  106.01  77.00  90.00   75
  7  \w     80.00 178.00   1.00    2.00    --  106.01  45.00-120.00   98
  8  \w    103.00 178.00   1.00    2.00    --  106.01  77.00-150.00   75
  9  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-150.00  101
 10  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 -30.00  101
 11  \w   -114.00 -13.00   1.00    1.00    --  -41.68 -61.00 104.00  101
 12  \w     77.00 178.00   1.00    2.00    --  106.01  61.00 -60.00  101
 13  \w     78.00 178.00   1.00    2.00    --  106.01  30.00-180.00  100
 14  \w     80.00 178.00   1.00    2.00    --  106.01  45.00  60.00   98
 15  \w     33.00  58.00   1.00    2.00    --  106.01-125.00-120.00   25
 16  \w     33.00 112.00   1.00    2.00    --  106.01-125.00 -60.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0743748000
_diffrn_orient_matrix_UB_12      -0.0522542000
_diffrn_orient_matrix_UB_13      0.0508308000
_diffrn_orient_matrix_UB_21      0.1315145000
_diffrn_orient_matrix_UB_22      -0.0616412000
_diffrn_orient_matrix_UB_23      -0.0056084000
_diffrn_orient_matrix_UB_31      0.0907829000
_diffrn_orient_matrix_UB_32      0.0463562000
_diffrn_orient_matrix_UB_33      0.0497401000
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27105
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.850
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.868
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Pentane diffusion in DCM'
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2423 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         6239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0271P)^2^+0.4220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                5895
_reflns_number_total             6239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00293d2.cif
_cod_data_source_block           vl203
_cod_database_code               7712313
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H39 Cl3 N O2 P Pd'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C22(H22A,H22B), C25(H25A,H25B), C24(H24A,H24B), C23(H23A,
 H23B), C19(H19A,H19B), C20(H20A,H20B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C31(H31), C30(H30), C6(H6), C29(H29), C27(H27),
 C11(H11), C9(H9), C10(H10)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              64627
_shelx_hkl_checksum              36010
_olex2_date_sample_data_collection 2020-11-09
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id VL203
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.748