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_1577008
_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         'C45 H34 N2, 0.5(C6 H14)'
_chemical_formula_sum            'C48 H41 N2'
_chemical_formula_weight         645.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 93.968(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.261(6)
_cell_length_b                   9.757(4)
_cell_length_c                   40.853(14)
_cell_measurement_reflns_used    5988
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.89
_cell_measurement_theta_min      5.14
_cell_volume                     7261(5)
_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    'SHELXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_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      0.0069145
_diffrn_orient_matrix_UB_12      0.0146778
_diffrn_orient_matrix_UB_13      0.0577979
_diffrn_orient_matrix_UB_21      0.0234583
_diffrn_orient_matrix_UB_22      0.0042563
_diffrn_orient_matrix_UB_23      0.0039320
_diffrn_orient_matrix_UB_31      -0.0019865
_diffrn_orient_matrix_UB_32      0.1013494
_diffrn_orient_matrix_UB_33      -0.0085356
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            89046
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         72.527
_diffrn_reflns_theta_min         4.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.7149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. 
 Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_preparation
;
 Crystals were grown at -35 \%C from saturated solution in Benzene/hexane. 
 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          0.209
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0008P)^2^+8.1051P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6042
_reflns_number_total             7098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc09514j3.cif
_cod_data_source_block           3-C6H14-05
_cod_original_cell_volume        7261(4)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               1577008
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              81712