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_7712312
_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         'C60 H86 Cl4 O4 P2 Pd2'
_chemical_formula_sum            'C60 H86 Cl4 O4 P2 Pd2'
_chemical_formula_weight         1287.83
_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             2020-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.314(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8194(3)
_cell_length_b                   16.4376(4)
_cell_length_c                   18.6502(5)
_cell_measurement_reflns_used    5703
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.4530
_cell_measurement_theta_min      3.5520
_cell_volume                     2997.34(14)
_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  (Sheldrick, 2015)'
_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 0.984
_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   -116.00 -17.00   1.00    4.50    --  -41.68 -38.00 -60.00   99
  2  \w    -87.00  -6.00   1.00    4.50    --  -41.68 125.00  90.00   81
  3  \w   -116.00 -17.00   1.00    4.50    --  -41.68 -38.00  30.00   99
  4  \w     30.00 134.00   1.00   14.00    --  106.01 -30.00  60.00  104
  5  \w     33.00 132.00   1.00   14.00    --  106.01 -45.00-180.00   99
  6  \w     34.00 135.00   1.00   14.00    --  106.01 -61.00  90.00  101
  7  \w     30.00 139.00   1.00   14.00    --  106.01 -77.00 -30.00  109
  8  \w    103.00 178.00   1.00   14.00    --  106.01  77.00 -90.00   75
  9  \w     97.00 178.00   1.00   14.00    --  106.01 125.00 150.00   81
 10  \w   -115.00 -14.00   1.00    4.50    --  -41.68 -57.00-180.00  101
 11  \w    -87.00  -6.00   1.00    4.50    --  -41.68 125.00 -60.00   81
 12  \w     53.00 178.00   1.00   14.00    --  106.01  15.00-120.00  125
 13  \w     78.00 178.00   1.00   14.00    --  106.01  30.00   0.00  100
 14  \w     33.00 112.00   1.00   14.00    --  106.01-125.00 -60.00   79
 15  \w     53.00 178.00   1.00   14.00    --  106.01  15.00 120.00  125
 16  \w   -115.00 -14.00   1.00    4.50    --  -41.68 -57.00-120.00  101
;
_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      0.0862368000
_diffrn_orient_matrix_UB_12      -0.0763535000
_diffrn_orient_matrix_UB_13      0.0198546000
_diffrn_orient_matrix_UB_21      -0.0819448000
_diffrn_orient_matrix_UB_22      -0.0478010000
_diffrn_orient_matrix_UB_23      -0.0606597000
_diffrn_orient_matrix_UB_31      0.1032255000
_diffrn_orient_matrix_UB_32      0.0260529000
_diffrn_orient_matrix_UB_33      -0.0529799000
_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  0.0893
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.981
_diffrn_reflns_theta_min         3.591
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.326
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.612
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_preparation       synthesis
_exptl_crystal_recrystallization_method 'CDCl3/Hexane slow vapour diffudion'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4502
_reflns_number_total             6074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00293d2.cif
_cod_data_source_block           lyx_090_a
_cod_database_code               7712312
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H86 Cl4 O4 P2 Pd2'
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.387
_reflns_odcompleteness_completeness 99.98
_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. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
3. Others
 Sof(H3B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=
 Sof(H2BC)=1-FVAR(1)
 Sof(H3A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
 Sof(H2AC)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C19(H19), C3(H3A), C3(H3B), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C29(H29A,H29B), C26(H26A,H26B), C20(H20A,H20B), C28(H28A,
 H28B), C27(H27A,H27B), C23(H23A,H23B), C21(H21A,H21B), C24(H24A,H24B),
 C22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C11(H11), C7(H7), C12(H12), C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,
 H2AC), C1B(H1BA,H1BB,H1BC), C2B(H2BA,H2BB,H2BC)
;
_shelx_res_checksum              30407
_shelx_hkl_checksum              6955
_olex2_date_sample_data_collection 2020-11-29
_olex2_exptl_crystal_mounting_method 'mouted on a litholoop'
_olex2_submission_original_sample_id CAZ_LXY090A
_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 2.437
_oxdiff_exptl_absorpt_empirical_full_min 0.515