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_7126420
_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_absolute_configuration ad
_chemical_formula_moiety         'C20 H29 Cl2 N3 Pd, 0.5(C H Cl3)'
_chemical_formula_sum            'C20.5 H29.5 Cl3.5 N3 Pd'
_chemical_formula_weight         548.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           27
_space_group_name_Hall           'P 2 -2c'
_space_group_name_H-M_alt        'P c c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-20 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.68060(10)
_cell_length_b                   15.68200(10)
_cell_length_c                   11.63120(10)
_cell_measurement_reflns_used    36850
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.8540
_cell_measurement_theta_min      2.7840
_cell_volume                     4866.55(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.998
_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    -66.00  33.00   1.00    1.00    --  -41.68  38.00  60.00   99
  3  \w     27.00  98.00   1.00    1.00    --   41.68-125.00-150.00   71
  4  \w    103.00 178.00   1.00    5.00    --  106.01  77.00  60.00   75
  5  \w     80.00 178.00   1.00    5.00    --  106.01  45.00-150.00   98
  6  \w     77.00 178.00   1.00    5.00    --  106.01  61.00 -60.00  101
  7  \w     30.00 139.00   1.00    5.00    --  106.01 -77.00  60.00  109
  8  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00  60.00  101
  9  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 -60.00  101
 10  \w    103.00 178.00   1.00    5.00    --  106.01  77.00 120.00   75
 11  \w     23.00 107.00   1.00    5.00    --  106.01 -94.00 -90.00   84
 12  \w     77.00 178.00   1.00    5.00    --  106.01  61.00-120.00  101
 13  \w     77.00 178.00   1.00    5.00    --  106.01  61.00   0.00  101
 14  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-180.00  101
 15  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 120.00  101
 16  \w     78.00 178.00   1.00    5.00    --  106.01  30.00  90.00  100
 17  \w     33.00 112.00   1.00    5.00    --  106.01-125.00  60.00   79
 18  \w     33.00 112.00   1.00    5.00    --  106.01-125.00-120.00   79
 19  \w     77.00 178.00   1.00    5.00    --  106.01  61.00 150.00  101
 20  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-120.00  101
 21  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00   0.00  101
 22  \w     77.00 178.00   1.00    5.00    --  106.01  61.00  90.00  101
 23  \w     77.00 178.00   1.00    5.00    --  106.01  61.00  30.00  101
 24  \w     77.00 178.00   1.00    5.00    --  106.01  61.00 120.00  101
 25  \w     77.00 178.00   1.00    5.00    --  106.01  61.00 -90.00  101
 26  \w    -87.00  -6.00   1.00    1.00    --  -41.68 125.00  60.00   81
 27  \w      6.00  83.00   1.00    1.00    --   41.68 -99.00 -90.00   77
 28  \w     77.00 118.00   1.00    5.00    --  106.01  61.00 -30.00   41
;
_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      -0.0057848000
_diffrn_orient_matrix_UB_12      0.0953006000
_diffrn_orient_matrix_UB_13      -0.0293892000
_diffrn_orient_matrix_UB_21      0.0406470000
_diffrn_orient_matrix_UB_22      -0.0086710000
_diffrn_orient_matrix_UB_23      -0.0933604000
_diffrn_orient_matrix_UB_31      -0.0405886000
_diffrn_orient_matrix_UB_32      -0.0223099000
_diffrn_orient_matrix_UB_33      -0.0892197000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            75469
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.877
_diffrn_reflns_theta_min         3.269
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.768
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       needle
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 4324 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9822
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                9483
_reflns_number_total             9822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02262d2.cif
_cod_data_source_block           sg134-1
_cod_depositor_comments
;
Adding full bibliography for 7126418--7126420.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C41 H59 Cl7 N6 Pd2'
_cod_original_formula_weight         1096.89
_cod_original_formula_moiety         '2(C20 H29 Cl2 N3 Pd), C H Cl3'
_cod_original_formula_units_Z            4
_cod_database_code               7126420
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H30 Cl2 N3 Pd'
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.336
_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
2.a Ternary CH refined with riding coordinates:
 C4(H4), C10(H10), C30(H30), C24(H24), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C28(H28A,H28B), C27(H27A,H27B), C9(H9A,H9B), C29(H29A,H29B),
 C15(H15A,H15B), C13(H13A,H13B), C25(H25A,H25B), C5(H5A,H5B), C11(H11A,H11B),
 C26(H26A,H26B), C14(H14A,H14B), C6(H6A,H6B), C7(H7A,H7B), C31(H31A,H31B),
 C35(H35A,H35B), C8(H8A,H8B), C34(H34A,H34B), C32(H32A,H32B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C22(H22), C39(H39), C36(H36), C40(H40), C37(H37), C16(H16), C23(H23),
 C3(H3), C17(H17), C18(H18), C20(H20), C19(H19), C38(H38)
;
_shelx_res_checksum              13368
_olex2_date_sample_data_collection 2019-12-18
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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 1.604
_oxdiff_exptl_absorpt_empirical_full_min 0.761