Unexpected B/Al Transelementation within a Rh Pincer Complex.
Lai, Qingheng; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Journal of the American Chemical Society 142 (2020) 20920–20923; doi:10.1021/jacs.0c09344

data_4135382
_publ_section_title
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 Unexpected B/Al Transelementation within a Rh Pincer Complex.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20920
_journal_page_last               20923
_journal_paper_doi               10.1021/jacs.0c09344
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C27 H39 Al N3 O2 P2 Rh'
_chemical_formula_sum            'C27 H39 Al N3 O2 P2 Rh'
_chemical_formula_weight         629.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0983(4)
_cell_length_b                   19.1026(5)
_cell_length_c                   10.0922(2)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      2.283
_cell_volume                     2910.76(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46246
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.232
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1352 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.9040.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0155P)^2^+2.1732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3163
_reflns_number_total             3422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09344_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4135382--4135384.cif.'
_cod_database_code               4135382
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Fixed U12: Rh1(0) Al1(0) O1(0) N2(0) O2(0) C2(0) C9(0) C1(0)
 Fixed U23: Rh1(0) Al1(0) O1(0) N2(0) O2(0) C2(0) C9(0) C1(0)
 Fixed Uiso: H5(0.023) H13(0.022) H4(0.021) H6(0.022) H14A(0.042) H14B(0.042)
 H14C(0.042) H11(0.023) H7(0.024) H15A(0.048) H15B(0.048) H15C(0.048) H8(0.028)
 H12A(0.041) H12B(0.041) H12C(0.041) H9(0.027) H10A(0.037) H10B(0.037)
 H10C(0.037)
 Fixed X: H5(0.532017) H13(0.556773) H4(0.560583) H6(0.58684) H14A(0.461584)
 H14B(0.43449) H14C(0.488352) H11(0.77489) H7(0.789296) H15A(0.597581)
 H15B(0.5485) H15C(0.650835) H8(0.914566) H12A(0.682125) H12B(0.761195)
 H12C(0.668425) H9(0.977245) H10A(0.837388) H10B(0.862703) H10C(0.787344)
 Fixed Y: Rh1(0.75) Al1(0.75) O1(0.75) N2(0.75) O2(0.75) H5(0.54383)
 H13(0.55466) H4(0.515226) H6(0.664855) C2(0.75) H14A(0.637706) H14B(0.624745)
 H14C(0.693678) H11(0.579494) H7(0.853398) H15A(0.65809) H15B(0.585188)
 H15C(0.586066) H8(0.85579) H12A(0.479094) H12B(0.461372) H12C(0.489081)
 C9(0.75) H9(0.75) H10A(0.619396) H10B(0.539343) H10C(0.5582) C1(0.75)
 Fixed Z: H5(0.813555) H13(0.307669) H4(0.570881) H6(0.852899) H14A(0.401125)
 H14B(0.249797) H14C(0.290143) H11(0.284261) H7(0.748441) H15A(0.112279)
 H15B(0.085593) H15C(0.126864) H8(0.881351) H12A(0.441783) H12B(0.341649)
 H12C(0.285682) H9(0.952689) H10A(0.485478) H10B(0.458081) H10C(0.563725)
;
_shelx_res_checksum              2181
_shelx_hkl_checksum              27040
_olex2_submission_special_instructions 'No special instructions were received'