Ligand properties of boryl ligands in bis-boryl rhodium(iii) complexes: a case study
Drescher, Wiebke; Kleeberg, Christian; Dalton Transactions  (2022) –; doi:10.1039/D1DT04276A

data_7709655
_publ_section_title
;
 Ligand properties of boryl ligands in bis-boryl rhodium(iii) complexes: a
 case study
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04276A
_journal_year                    2022
_chemical_formula_moiety         'C23 H46 B2 N O4 P3 Rh, C32 H12 B F24'
_chemical_formula_sum            'C55 H58 B3 F24 N O4 P3 Rh'
_chemical_formula_weight         1481.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-20 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.739(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0677(3)
_cell_length_b                   13.9610(2)
_cell_length_c                   25.9822(4)
_cell_measurement_reflns_used    100719
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.6140
_cell_measurement_theta_min      2.5560
_cell_volume                     6459.38(18)
_computing_cell_refinement
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2018)
;
_computing_data_collection
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2018)
;
_computing_data_reduction
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2018)
;
_computing_molecular_graphics
;
 K. Brandenburg, 2017, Diamond 4.4.1, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;
_computing_structure_refinement
;
 SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3--8)
;
_computing_structure_solution
;
 SHELXT (Ver. 2018/2) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_diffrn_ambient_environment      N~2~
_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 0.920
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            281801
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.227
_diffrn_reflns_theta_min         2.556
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2992
_exptl_crystal_recrystallization_method
;
 From a solution in PhMe at ambient temperature.
;
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.729
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         24676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0538P)^2^+4.7953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19168
_reflns_number_total             24676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04276a2.cif
_cod_data_source_block           wo85wo
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7709655
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              14328