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_7709650
_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_absolute_configuration unk
_chemical_formula_moiety         'C12 H36 Cl P4 Rh, C12 H8 B O4, C4 H8 O'
_chemical_formula_sum            'C28 H52 B Cl O5 P4 Rh'
_chemical_formula_weight         741.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                   33.9797(7)
_cell_length_b                   15.7885(4)
_cell_length_c                   13.0676(3)
_cell_measurement_reflns_used    63735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.9440
_cell_measurement_theta_min      4.2810
_cell_volume                     7010.6(3)
_computing_cell_refinement
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
;
_computing_data_collection
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
;
_computing_data_reduction
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
;
_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_type            HyPix
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.974
_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_source         'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            166289
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.517
_diffrn_reflns_theta_min         3.086
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.638
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.655
_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 pale yellow'
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       fragement
_exptl_crystal_F_000             3096
_exptl_crystal_recrystallization_method
;
 From a solution in THF-d8 at ambient temperature over a course of eight days.
;
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack (1983), 6664 Friedel pairs'
_refine_ls_abs_structure_Flack   0.482(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         14341
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0680
_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^)+(0.1283P)^2^+17.5441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                12946
_reflns_number_total             14341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04276a2.cif
_cod_data_source_block           wo103wo
_cod_database_code               7709650
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              680