Achieving (quasi)-monocoordination in metal complexes with an exceptionally bulky carbene ligand.
Zapf, Ludwig; Rivard, Eric; Chemical science 17 (2026) 6500–6506; doi:10.1039/d5sc09514j

data_1577009
_publ_section_title
;
 Achieving (quasi)-monocoordination in metal complexes with an
 exceptionally bulky carbene ligand.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              6500
_journal_page_last               6506
_journal_paper_doi               10.1039/d5sc09514j
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C54 H43 Cl N2 Pd'
_chemical_formula_sum            'C54 H43 Cl N2 Pd'
_chemical_formula_weight         861.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-07-22
_audit_update_record
;
2025-11-25 deposited with the CCDC.	2026-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.017(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.1901(4)
_cell_length_b                   21.5445(11)
_cell_length_c                   35.5333(18)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.21
_cell_volume                     7790.2(6)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40B (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
;
 Sparks R.A., Computational Crystallography p1-18 (Clarendon Press, 1982)
;
_diffrn_orient_matrix_UB_11      -0.0063387
_diffrn_orient_matrix_UB_12      -0.0461588
_diffrn_orient_matrix_UB_13      0.0022375
_diffrn_orient_matrix_UB_21      0.0029171
_diffrn_orient_matrix_UB_22      0.0037657
_diffrn_orient_matrix_UB_23      0.0280814
_diffrn_orient_matrix_UB_31      -0.0980224
_diffrn_orient_matrix_UB_32      0.0030970
_diffrn_orient_matrix_UB_33      -0.0007962
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            222127
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.976
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.9895
_exptl_absorpt_correction_T_min  0.8276
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_preparation
;
 Crystals were grown at 20 \%C from saturated solution in penzene/pentane. 
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
_exptl_crystal_size_max          0.473
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Refined as an inversion twin'
_refine_ls_abs_structure_Flack   0.433(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1772
_refine_ls_number_reflns         31797
_refine_ls_number_restraints     1183
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+2.7209P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                29206
_reflns_number_total             31797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc09514j3.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1577009
_shelx_shelxl_version_number     2019/1
_exptl_absorpt_special_details
;
 Incident beam scaling, empirical absorption correction using spherical 
 harmonics, and outlier rejection was employed as implemented in SADABS
;
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              16403
_shelx_fab_checksum              73235