Towards structurally versatile mesoionic N-heterocyclic olefin ligands and their coordination to palladium, gold, and boron hydride.
Ževart, Tisa; Pinter, Balazs; Lozinšek, Matic; Urankar, Damijana; Jansen-van Vuuren, Ross D; Košmrlj, Janez; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8915–8925; doi:10.1039/d4dt00195h

data_7715577
_publ_section_title
;
 Towards structurally versatile mesoionic N-heterocyclic olefin ligands
 and their coordination to palladium, gold, and boron hydride.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8915
_journal_page_last               8925
_journal_paper_doi               10.1039/d4dt00195h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C50 H54 Cl2 N6 P2 Pd, 2(B F4), C D Cl3'
_chemical_formula_sum            'C51 H54 B2 Cl5 D F8 N6 P2 Pd'
_chemical_formula_weight         1272.22
_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     iterative
_audit_creation_date             2023-09-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-27 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4136(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7815(3)
_cell_length_b                   12.9118(2)
_cell_length_c                   23.7001(4)
_cell_measurement_reflns_used    17835
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.5600
_cell_measurement_theta_min      2.7420
_cell_volume                     5633.69(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger2 R CdTe 1M'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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  -5.00   0.50    3.00    --  -47.56  71.00  65.00  122
  2  \w    -82.00 -29.00   0.50    3.00    --  -47.56 -71.00 -64.00  106
  3  \w     77.00 105.00   0.50    3.00    --   47.56  71.00  65.00   56
  4  \w     42.00  69.00   0.50    3.00    --   47.56  71.00  65.00   54
  5  \w   -101.00 -74.00   0.50    6.00    --  -82.50 -71.00 -64.00   54
  6  \w    -81.00 -50.00   0.50    6.00    --  -82.50  71.00  65.00   62
  7  \w     86.00 161.00   0.50    6.00    --  104.00  71.00  65.00  150
  8  \w     52.00  86.00   0.50    6.00    --  104.00 -71.00 -64.00   68
  9  \w   -101.00 -48.00   0.50    3.00    --  -47.56 -57.00-120.00  106
 10  \w   -110.00 -47.00   0.50    3.00    --  -47.56 -57.00  90.00  126
 11  \w    -10.00  53.00   0.50    3.00    --   47.56 -71.00 -64.00  126
 12  \w    -48.00 -17.00   0.50    6.00    --  -82.50  45.00 -90.00   62
 13  \w    -49.00 -19.00   0.50    6.00    --  -82.50  45.00-120.00   60
 14  \w     43.00  70.00   0.50    6.00    --  104.00 -61.00   0.00   54
 15  \w     91.00 155.00   0.50    6.00    --  104.00  77.00 -30.00  128
 16  \w     44.00  69.00   0.50    6.00    --  104.00 -61.00-150.00   50
 17  \w     43.00  70.00   0.50    6.00    --  104.00 -61.00 -90.00   54
 18  \w    101.00 153.00   0.50    6.00    --  104.00  77.00  30.00  104
 19  \w    100.00 157.00   0.50    6.00    --  104.00  61.00   0.00  114
 20  \w     49.00  94.00   0.50    6.00    --  104.00 -77.00-180.00   90
 21  \w     44.00  69.00   0.50    6.00    --  104.00 -61.00-120.00   50
 22  \w     66.00  97.00   0.50    6.00    --  104.00 -77.00 -30.00   62
 23  \w     54.00  94.00   0.50    6.00    --  104.00 -77.00-150.00   80
 24  \w     43.00  70.00   0.50    6.00    --  104.00 -61.00  90.00   54
 25  \w     48.00  89.00   0.50    6.00    --  104.00 -77.00  90.00   82
 26  \w     43.00  71.00   0.50    6.00    --  104.00 -61.00-180.00   56
 27  \w     53.00  90.00   0.50    6.00    --  104.00 -77.00  30.00   74
 28  \w    139.00 167.00   0.50    6.00    --  104.00  45.00  90.00   56
 29  \w     51.00  92.00   0.50    6.00    --  104.00 -77.00 150.00   82
 30  \w    105.00 149.00   0.50    6.00    --  104.00  45.00 -30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy-S, Dualflex, Eiger2 R CdTe 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0247065000
_diffrn_orient_matrix_UB_12      -0.0953240000
_diffrn_orient_matrix_UB_13      -0.0302288000
_diffrn_orient_matrix_UB_21      -0.0735721000
_diffrn_orient_matrix_UB_22      -0.0013481000
_diffrn_orient_matrix_UB_23      -0.0424432000
_diffrn_orient_matrix_UB_31      0.0312441000
_diffrn_orient_matrix_UB_32      0.0717146000
_diffrn_orient_matrix_UB_33      -0.0410369000
_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  0.0572
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.099
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.956
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform-d'
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.071
_refine_diff_density_max         6.456
_refine_diff_density_min         -2.683
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         11392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0987
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1791P)^2^+36.7797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2641
_refine_ls_wR_factor_ref         0.2717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10029
_reflns_number_total             11392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00195h2.cif
_cod_data_source_block           tzd247_1
_cod_depositor_comments
'Adding full bibliography for 7715576--7715577.cif.'
_cod_original_cell_volume        5633.69(15)
_cod_database_code               7715577
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C51 H55 B2 Cl5 F8 N6 P2 Pd'
_chemical_oxdiff_usercomment     '100 K, TZ'
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.481
_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:
 C51(D51)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C28(H28A,H28B), C29(H29A,H29B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C33(H33), C34(H34),
  C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              87490
_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 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.588