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_1577012
_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 H35 N2, C F3 O3 S'
_chemical_formula_sum            'C46 H35 F3 N2 O3 S'
_chemical_formula_weight         752.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 104.901(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1976(11)
_cell_length_b                   17.9673(14)
_cell_length_c                   19.1187(19)
_cell_measurement_reflns_used    9685
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.20
_cell_volume                     3717.2(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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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      0.0822633
_diffrn_orient_matrix_UB_12      -0.0087566
_diffrn_orient_matrix_UB_13      0.0347555
_diffrn_orient_matrix_UB_21      -0.0372106
_diffrn_orient_matrix_UB_22      0.0093240
_diffrn_orient_matrix_UB_23      0.0414641
_diffrn_orient_matrix_UB_31      -0.0197040
_diffrn_orient_matrix_UB_32      -0.0541669
_diffrn_orient_matrix_UB_33      0.0015188
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            94628
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.426
_diffrn_reflns_theta_max         26.426
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_preparation
;
 Crystals were grown at 20 \%C from saturated solution in CH2Cl2 / 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          1.000
_exptl_crystal_size_mid          0.551
_exptl_crystal_size_min          0.423
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7568
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0006P)^2^+2.6287P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6546
_reflns_number_total             7568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc09514j3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1577012
_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   0.866
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              7736