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_7709656
_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         'C21 H43 B2 Cl O4 P3 Rh, 0.5 (C4 H8 O)'
_chemical_formula_sum            'C23 H47 B2 Cl O4.5 P3 Rh'
_chemical_formula_weight         648.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.7954(11)
_cell_length_b                   13.2910(4)
_cell_length_c                   13.5036(4)
_cell_measurement_reflns_used    27982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8810
_cell_measurement_theta_min      2.9960
_cell_volume                     6245.0(3)
_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. 2014/5) (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_area_resol_mean 16.1419
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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  0.1009
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            183646
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.355
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method
;
 Slow evaporation of THF at room temperature.
;
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8329
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0302P)^2^+11.5265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6243
_reflns_number_total             8329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04276a2.cif
_cod_data_source_block           wo53wo2
_cod_original_formula_sum        'C23 H47 B2 Cl O4.50 P3 Rh'
_cod_database_code               7709656
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              10069