Synthesis and catalytic activity of palladium complexes bearing <i>N</i>-heterocyclic carbenes (NHCs) and 1,4,7-triaza-9-phosphatricyclo[5.3.2.1]tridecane (CAP) ligands.
Scattolin, Thomas; Voloshkin, Vladislav A.; Martynova, Ekaterina; Vanden Broeck, Sofie M. P.; Beliš, Marek; Cazin, Catherine S. J.; Nolan, Steven P.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9491–9499; doi:10.1039/d1dt01716k

data_7707679
_publ_section_title
;
 Synthesis and catalytic activity of palladium complexes bearing
 <i>N</i>-heterocyclic carbenes (NHCs) and
 1,4,7-triaza-9-phosphatricyclo[5.3.2.1]tridecane (CAP) ligands.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9491
_journal_page_last               9499
_journal_paper_doi               10.1039/d1dt01716k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C36 H56 Cl2 N5 P Pd, 2(C H Cl3)'
_chemical_formula_sum            'C38 H58 Cl8 N5 P Pd'
_chemical_formula_weight         1005.86
_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             2020-12-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.8980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.83540(10)
_cell_length_b                   22.31660(10)
_cell_length_c                   16.5717(2)
_cell_measurement_reflns_used    19713
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7580
_cell_measurement_theta_min      3.4330
_cell_volume                     4463.45(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 0.986
_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   -115.00 -14.00   1.00    2.25    --  -41.68 -57.00 -90.00  101
  2  \w    -21.00  74.00   1.00    2.25    --   41.68 -77.00 120.00   95
  3  \w     27.00  98.00   1.00    2.25    --   41.68-125.00 -60.00   71
  4  \w     33.00 132.00   1.00   13.40    --  106.01 -45.00 -60.00   99
  5  \w    103.00 178.00   1.00   13.40    --  106.01  77.00  30.00   75
  6  \w     34.00 135.00   1.00   13.40    --  106.01 -61.00-150.00  101
  7  \w     33.00 112.00   1.00   13.40    --  106.01-125.00  30.00   79
  8  \w     78.00 178.00   1.00   13.40    --  106.01  30.00-180.00  100
  9  \w     30.00 139.00   1.00   13.40    --  106.01 -77.00  90.00  109
 10  \w   -115.00 -14.00   1.00    2.25    --  -41.68 -57.00  60.00  101
 11  \w   -116.00 -17.00   1.00    2.25    --  -41.68 -38.00 150.00   99
 12  \w     53.00 178.00   1.00   13.40    --  106.01  15.00 -30.00  125
 13  \w     77.00 178.00   1.00   13.40    --  106.01  61.00-150.00  101
 14  \w     77.00 178.00   1.00   13.40    --  106.01  61.00 -30.00  101
 15  \w     53.00 178.00   1.00   13.40    --  106.01  15.00  90.00  125
 16  \w   -115.00 -56.00   1.00    2.25    --  -41.68 -57.00   0.00   59
;
_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      -0.0112293000
_diffrn_orient_matrix_UB_12      0.0576398000
_diffrn_orient_matrix_UB_13      -0.0534715000
_diffrn_orient_matrix_UB_21      -0.0761933000
_diffrn_orient_matrix_UB_22      -0.0331759000
_diffrn_orient_matrix_UB_23      -0.0798119000
_diffrn_orient_matrix_UB_31      -0.1017719000
_diffrn_orient_matrix_UB_32      0.0185178000
_diffrn_orient_matrix_UB_33      0.0234197000
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.925
_diffrn_reflns_theta_min         3.459
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.363
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.679
_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    1.497
_exptl_crystal_description       needle
_exptl_crystal_F_000             2072
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Pentane diffusion in CHCl3'
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+2.2142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8064
_reflns_number_total             8915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01716k2.cif
_cod_data_source_block           ts132
_cod_depositor_comments
'Adding full bibliography for 7707679--7707680.cif.'
_cod_database_code               7707679
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H57 Cl2 N5 P Pd'
_reflns_odcompleteness_completeness 99.99
_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:
 C13(H13), C10(H10), C25(H25), C22(H22), C37(H37), C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C2(H2A,H2B), C3(H3A,H3B), C28(H28A,H28B), C29(H29A,H29B),
 C33(H33A,H33B), C34(H34A,H34B), C32(H32A,H32B), C35(H35A,H35B), C31(H31A,H31B),
  C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C7(H7), C20(H20), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C27(H27A,H27B,
 H27C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              62414
_olex2_date_sample_data_collection 2020-12-12
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id TS132
_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 1.486
_oxdiff_exptl_absorpt_empirical_full_min 0.816