Rhodium(I) complexes with proton-responsive anionic tethered N-heterocyclic carbene ligands: synthesis and application in alkyne dimerization.
Karataş, Mert Olgun; Hinojosa, Diego R.; Passarelli, Vincenzo; Oro, Luis A.; Pérez-Torrente, Jesús J; Castarlenas, Ricardo; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15306–15319; doi:10.1039/d5dt01516b

data_7719477
_publ_section_title
;
 Rhodium(I) complexes with proton-responsive anionic tethered
 N-heterocyclic carbene ligands: synthesis and application in alkyne
 dimerization.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15306
_journal_page_last               15319
_journal_paper_doi               10.1039/d5dt01516b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H34 N3 O Rh, 1.5 (C H2 Cl2)'
_chemical_formula_sum            'C29.5 H37 Cl3 N3 O Rh'
_chemical_formula_weight         658.88
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-06-13 deposited with the CCDC.	2025-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.195(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8550(15)
_cell_length_b                   10.5806(16)
_cell_length_c                   28.689(4)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.242
_cell_measurement_theta_min      2.269
_cell_volume                     2974.0(8)
_computing_cell_refinement       'SAINT+ in APEX3 (Bruker AXS,2017)'
_computing_data_collection       'SMART in APEX3 (Bruker AXS,2017)'
_computing_data_reduction        'SAINT+ in APEX3 (Bruker AXS,2017)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            34483
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.361
_diffrn_reflns_theta_min         2.053
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.8132
_exptl_absorpt_correction_T_min  0.7353
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       prism
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         7311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0232P)^2^+10.7723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6071
_reflns_number_total             7311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01516b2.cif
_cod_data_source_block           cmpd_2_VPX272_DRH106b
_cod_depositor_comments
'Adding full bibliography for 7719477--7719479.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C29.50 H37 Cl3 N3 O Rh'
_cod_database_code               7719477
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
; 
 Multi-scan correction included in APEX3 package (Bruker AXS, 2017)
;
_shelx_res_checksum              51696
_shelx_hkl_checksum              56777
_shelx_fab_checksum              22884