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_7707680
_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         'C14 H23 Cl2 N4 P Pd'
_chemical_formula_sum            'C14 H23 Cl2 N4 P Pd'
_chemical_formula_weight         455.63
_chemical_name_systematic        VL400
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4158(3)
_cell_length_b                   12.2045(2)
_cell_length_c                   18.2376(4)
_cell_measurement_reflns_used    11388
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.6150
_cell_measurement_theta_min      4.8330
_cell_volume                     3431.26(12)
_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   -130.00  46.00   1.00    1.00    --  -41.68   0.00 -90.00  176
  2  \w    -87.00  -6.00   1.00    1.00    --  -41.68 125.00 -90.00   81
  3  \w     23.00 107.00   1.00    2.60    --  106.01 -94.00  60.00   84
  4  \w    103.00 178.00   1.00    2.60    --  106.01  77.00 -60.00   75
  5  \w     33.00 112.00   1.00    2.60    --  106.01-125.00   0.00   79
  6  \w    103.00 178.00   1.00    2.60    --  106.01  77.00-120.00   75
  7  \w     34.00 135.00   1.00    2.60    --  106.01 -61.00 120.00  101
  8  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-180.00  101
  9  \w     14.00 115.00   1.00    1.00    --   41.68  57.00 120.00  101
 10  \w     78.00 178.00   1.00    2.60    --  106.01  30.00-180.00  100
 11  \w     78.00 176.00   1.00    2.60    --  106.01  30.00 -90.00   98
 12  \w     53.00 178.00   1.00    2.60    --  106.01  15.00  90.00  125
;
_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      0.0764226000
_diffrn_orient_matrix_UB_12      0.0613776000
_diffrn_orient_matrix_UB_13      0.0355150000
_diffrn_orient_matrix_UB_21      -0.0565799000
_diffrn_orient_matrix_UB_22      0.1038426000
_diffrn_orient_matrix_UB_23      0.0064035000
_diffrn_orient_matrix_UB_31      -0.0307789000
_diffrn_orient_matrix_UB_32      -0.0371889000
_diffrn_orient_matrix_UB_33      0.0763656000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23954
_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         74.054
_diffrn_reflns_theta_min         4.850
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.480
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.585
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1840
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Pentane diffusion in DCM'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.6372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3120
_reflns_number_total             3440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01716k2.cif
_cod_data_source_block           vl400
_cod_depositor_comments
'Adding full bibliography for 7707679--7707680.cif.'
_cod_database_code               7707680
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C14 H23 Cl2 N4 P Pd'
_reflns_odcompleteness_completeness 99.97
_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 Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C7(H7A,H7B), C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B),
 C9(H9A,H9B), C6(H6A,H6B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C10(H10), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              65746
_olex2_date_sample_data_collection 2021-03-15
_olex2_exptl_crystal_mounting_method 'Little loop'
_olex2_submission_original_sample_id VL400
_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 2.376
_oxdiff_exptl_absorpt_empirical_full_min 0.721