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_1577006
_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_absolute_configuration unk
_chemical_formula_moiety         'C45 H34 N2 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C47 H38 Cl4 N2 Pd'
_chemical_formula_weight         878.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                 100.817(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.998(4)
_cell_length_b                   25.266(6)
_cell_length_c                   9.438(2)
_cell_measurement_reflns_used    6555
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.44
_cell_volume                     3981.3(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      -0.0135321
_diffrn_orient_matrix_UB_12      0.0370456
_diffrn_orient_matrix_UB_13      0.0240221
_diffrn_orient_matrix_UB_21      0.0229836
_diffrn_orient_matrix_UB_22      0.0134632
_diffrn_orient_matrix_UB_23      -0.0831939
_diffrn_orient_matrix_UB_31      -0.0536284
_diffrn_orient_matrix_UB_32      -0.0035778
_diffrn_orient_matrix_UB_33      -0.0643253
_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  0.0763
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            36500
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_min         2.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       needle
_exptl_crystal_F_000             1792
_exptl_crystal_preparation
;
 Crystals were grown at -35 \%C from saturated solution in CH2Cl2. 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          0.294
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 2464 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, 
 Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0024P)^2^+7.4169P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    0.838
_reflns_Friedel_fraction_max     0.826
_reflns_number_gt                6375
_reflns_number_total             7409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc09514j3.cif
_cod_data_source_block           8-2CH2Cl2
_cod_original_cell_volume        3981.4(17)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1577006
_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. 
 Additional spherical absorption correction with mu*r value set to 0.2 was 
 applied.
;
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              88032