Understanding existing and designing novel synthetic routes to Pd-PEPPSI-NHC and Pd-PEPPSI-PR<sub>3</sub> pre-catalysts.
Guillet, Sébastien G; Voloshkin, Vladislav A.; Saab, Marina; Beliš, Marek; Van Hecke, Kristof; Nahra, Fady; Nolan, Steven P.; Chemical communications (Cambridge, England) 56 (2020) 5953–5956; doi:10.1039/d0cc02262d

data_7126418
_publ_section_title
;
 Understanding existing and designing novel synthetic routes to
 Pd-PEPPSI-NHC and Pd-PEPPSI-PR<sub>3</sub> pre-catalysts.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5953
_journal_page_last               5956
_journal_paper_doi               10.1039/d0cc02262d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C27 H37 N2, 0.5(Cl6 Pd2), C H Cl3'
_chemical_formula_sum            'C28 H38 Cl6 N2 Pd'
_chemical_formula_weight         721.70
_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             2018-05-19
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2020-01-20 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.478(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8037(4)
_cell_length_b                   17.1488(5)
_cell_length_c                   15.3764(4)
_cell_measurement_reflns_used    8757
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.5940
_cell_measurement_theta_min      3.8850
_cell_volume                     3268.95(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -66.00  33.00   1.00    5.00    --  -41.68  38.00   0.00   99
  2  \w    -83.00  38.00   1.00    5.00    --  -41.68  19.00 120.00  121
  3  \w     23.00  98.00   1.00    5.00    --   41.68-125.00-180.00   75
  4  \w     81.00 178.00   1.00   25.00    --  109.13  30.00  30.00   97
  5  \w     36.00 117.00   1.00   25.00    --  109.13-125.00  60.00   81
  6  \w     94.00 178.00   1.00   25.00    --  109.13 125.00-150.00   84
  7  \w     36.00 135.00   1.00   25.00    --  109.13 -45.00-150.00   99
  8  \w     36.00 135.00   1.00   25.00    --  109.13 -45.00   0.00   99
  9  \w   -118.00  -9.00   1.00    5.00    --  -41.68 -77.00   0.00  109
 10  \w   -118.00  -9.00   1.00    5.00    --  -41.68 -77.00 120.00  109
 11  \w     77.00 178.00   1.00   25.00    --  109.13  77.00 -60.00  101
 12  \w     26.00 110.00   1.00   25.00    --  109.13 -94.00-150.00   84
 13  \w     83.00 178.00   1.00   25.00    --  109.13  45.00-120.00   95
 14  \w     56.00 178.00   1.00   25.00    --  109.13  15.00-180.00  122
 15  \w    -70.00  31.00   1.00    5.00    --  -41.68  57.00-120.00  101
 16  \w   -118.00  -9.00   1.00    5.00    --  -41.68 -77.00-120.00  109
 17  \w     80.00 160.00   1.00   25.00    --  109.13  61.00  60.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0491017000
_diffrn_orient_matrix_UB_12      -0.0017767000
_diffrn_orient_matrix_UB_13      -0.0818071000
_diffrn_orient_matrix_UB_21      0.1064008000
_diffrn_orient_matrix_UB_22      -0.0318456000
_diffrn_orient_matrix_UB_23      0.0597585000
_diffrn_orient_matrix_UB_31      -0.0415464000
_diffrn_orient_matrix_UB_32      -0.0839282000
_diffrn_orient_matrix_UB_33      -0.0211117000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31549
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.401
_diffrn_reflns_theta_min         3.932
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.242
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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 brownish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.967
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6643
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0900P)^2^+1.7065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             6643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02262d2.cif
_cod_data_source_block           fn036
_cod_depositor_comments
'Adding full bibliography for 7126418--7126420.cif.'
_cod_database_code               7126418
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H38 Cl6 N2 Pd'
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C28(H28), C10(H10), C13(H13), C22(H22), C25(H25)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              91972
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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 1.481
_oxdiff_exptl_absorpt_empirical_full_min 0.553