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_7709651
_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         'C18 H42 B2 Cl O4 P2 Rh'
_chemical_formula_sum            'C18 H42 B2 Cl O4 P2 Rh'
_chemical_formula_weight         544.43
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_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                120
_cell_formula_units_Z            18
_cell_length_a                   34.9213(18)
_cell_length_b                   34.9213(18)
_cell_length_c                   11.6219(8)
_cell_measurement_reflns_used    9313
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.92
_cell_measurement_theta_min      2.53
_cell_volume                     12274.1(12)
_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
;
 Olex2 (Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)
;
_computing_structure_refinement
;
 SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, A71, 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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23803
_diffrn_reflns_point_group_measured_fraction_full 0.858
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.222
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
 Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

 Empirical correction (ABSPACK) includes:
   - Absorption correction using spherical harmonics
   - Frame scaling
   - Detector area scaling
   - B-factor correction
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       needle
_exptl_crystal_F_000             5112
_exptl_crystal_recrystallization_method
;
 From a solution in n-pentane at -40 deg C.
;
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
_refine_diff_density_max         2.059
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4133
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1383P)^2^+24.7747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1767
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    0.714
_reflns_Friedel_fraction_max     0.714
_reflns_number_gt                3799
_reflns_number_total             4133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04276a2.cif
_cod_data_source_block           wo110wo
_cod_original_cell_volume        12274.1(15)
_cod_database_code               7709651
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              85529