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_7126419
_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         'C23 H20 Cl2 N P Pd'
_chemical_formula_sum            'C23 H20 Cl2 N P Pd'
_chemical_formula_weight         518.67
_chemical_name_systematic        VL134
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-03
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-17 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8655(2)
_cell_length_b                   10.7674(2)
_cell_length_c                   22.2732(4)
_cell_measurement_reflns_used    11330
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.3480
_cell_measurement_theta_min      2.9620
_cell_volume                     2122.94(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 0.999
_diffrn_measured_fraction_theta_max 0.891
_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    -52.00  69.00   1.00   25.00    --  -11.11  19.00 120.00  121
  2  \w    -91.00  30.00   1.00   25.00    --  -11.11 -19.00 -60.00  121
  3  \w    -15.00  10.00   1.00   25.00    --   10.17 -99.00-120.00   25
  4  \w    -15.00  30.00   1.00   25.00    --  -11.11 -99.00 120.00   45
  5  \w    -36.00  63.00   1.00   25.00    --  -11.11  38.00 -30.00   99
;
_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      -0.0722114000
_diffrn_orient_matrix_UB_12      -0.0269197000
_diffrn_orient_matrix_UB_13      -0.0061574000
_diffrn_orient_matrix_UB_21      -0.0048111000
_diffrn_orient_matrix_UB_22      0.0294296000
_diffrn_orient_matrix_UB_23      -0.0285356000
_diffrn_orient_matrix_UB_31      0.0343471000
_diffrn_orient_matrix_UB_32      -0.0524395000
_diffrn_orient_matrix_UB_33      -0.0128549000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.605
_diffrn_reflns_theta_min         2.633
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.681
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       needle
_exptl_crystal_F_000             1040
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Pentane diffusion in DCM'
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0210P)^2^+1.0579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4424
_reflns_number_total             5321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02262d2.cif
_cod_data_source_block           vl134
_cod_depositor_comments
'Adding full bibliography for 7126418--7126420.cif.'
_cod_database_code               7126419
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H20 Cl2 N P Pd'
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.790
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C6(H6), C14(H14), C20(H20), C4(H4), C3(H3), C19(H19),
 C22(H22), C23(H23), C18(H18), C8(H8), C11(H11), C9(H9), C5(H5), C10(H10),
 C15(H15), C16(H16), C21(H21), C17(H17)
;
_shelx_res_checksum              54625
_olex2_date_sample_data_collection 2020-03-03
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id VL134
_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 1.798
_oxdiff_exptl_absorpt_empirical_full_min 0.435