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_1568644
_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            'C51 H57 N2 P3'
_chemical_formula_weight         790.89
_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   mixed
_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                 106.2070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.72400(10)
_cell_length_b                   22.58670(10)
_cell_length_c                   10.30020(10)
_cell_measurement_reflns_used    34006
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.5010
_cell_measurement_theta_min      3.8370
_cell_volume                     2172.36(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.989
_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_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43386
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.700
_diffrn_reflns_theta_min         3.914
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.128
_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            yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 4020 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         8909
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0541P)^2^+0.5780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                8768
_reflns_number_total             8909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06759e2.cif
_cod_data_source_block           SL-025
_cod_depositor_comments
'Adding full bibliography for 1568644--1568653.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1568644
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              58519
_shelx_hkl_checksum              30152