Probing the donor strength of yldiide ligands: synthesis, structure and reactivity of rhodium complexes with a PC<sub>ylide</sub>N pincer ligand.
Lapointe, Sébastien; Duari, Prakash; Gessner, Viktoria H.; Chemical science 14 (2023) 3816–3825; doi:10.1039/d2sc06759e

data_1568650
_publ_section_title
;
 Probing the donor strength of yldiide ligands: synthesis, structure and
 reactivity of rhodium complexes with a PC<sub>ylide</sub>N pincer ligand.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              3816
_journal_page_last               3825
_journal_paper_doi               10.1039/d2sc06759e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C54 H65 N2 P4 Rh'
_chemical_formula_weight         968.87
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-19 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.0650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2238(2)
_cell_length_b                   33.5168(4)
_cell_length_c                   12.31380(10)
_cell_measurement_reflns_used    75882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.1350
_cell_measurement_theta_min      2.4150
_cell_volume                     4871.61(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_molecular_graphics    'SHELXLE-2019 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            117672
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.174
_diffrn_reflns_theta_min         2.419
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.268
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.376
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 13451 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         32348
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0354P)^2^+2.3439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.833
_reflns_number_gt                30369
_reflns_number_total             32348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06759e2.cif
_cod_data_source_block           SL-306
_cod_depositor_comments
'Adding full bibliography for 1568644--1568653.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1568650
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              43326
_shelx_hkl_checksum              88980