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_4135384
_publ_section_title
;
 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         'C44 H68 Al2 N4 O4 P4 Rh2, C7 H8'
_chemical_formula_sum            'C51 H76 Al2 N4 O4 P4 Rh2'
_chemical_formula_weight         1192.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.389(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2780(5)
_cell_length_b                   9.6009(3)
_cell_length_c                   19.5396(6)
_cell_measurement_reflns_used    9539
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.671
_cell_volume                     2861.11(16)
_computing_cell_refinement
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_data_reduction
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            215669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.646
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.4246
_exptl_absorpt_correction_T_min  0.3703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1368 before and 0.0663 after correction. The Ratio of minimum to maximum transmission is 0.8721. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6562
_refine_ls_number_restraints     373
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+2.1915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5790
_reflns_number_total             6562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09344_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4135382--4135384.cif.'
_cod_database_code               4135384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.893
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7T-C1T = C7S-C1S
 1.52 with sigma of 0.01
 C1S-C6S \\sim C6S-C5S \\sim C5S-C4S \\sim C4S-C3S \\sim C3S-C2S \\sim C2S-C1S
 with sigma of 0.02
 C1S-C3S \\sim C1S-C5S \\sim C2S-C4S \\sim C6S-C2S \\sim C5S-C3S \\sim C6S-C4S
 with sigma of 0.04
 C7S-C2S \\sim C7S-C6S
 with sigma of 0.04
 C1T-C2T \\sim C2T-C3T \\sim C3T-C4T \\sim C4T-C5T \\sim C5T-C6T \\sim C6T-C1T
 with sigma of 0.02
 C1T-C5T \\sim C1T-C3T \\sim C6T-C4T \\sim C2T-C6T \\sim C3T-C5T \\sim C2T-C4T
 with sigma of 0.04
 C7T-C6T \\sim C7T-C2T
 with sigma of 0.04
 C7T-C1T \\sim C7S-C1S
 with sigma of 0.005
3. Restrained planarity
 C1S, C2S, C3S, C4S, C5S, C6S, C7S
 with sigma of 0.1
 C1T, C2T, C3T, C4T, C5T, C6T, C7T
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S \\sim C7S: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1T \\sim C2T \\sim C3T \\sim C4T \\sim C5T \\sim C6T \\sim C7T: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1T \\sim C2T \\sim C3T \\sim C4T \\sim C5T \\sim C6T \\sim C7T \\sim C1S \\sim
C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S \\sim C7S: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C1T) = Uanis(C3S)
5. Rigid body (RIGU) restrains
 C1T, C2T, C3T, C4T, C5T, C6T, C7T, C1S, C2S, C3S, C4S, C5S, C6S, C7S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Others
 Fixed Sof: C1T(0.25) C2T(0.25) H2T(0.25) C3T(0.25) H3T(0.25) C4T(0.25)
 H4T(0.25) C5T(0.25) H5T(0.25) C6T(0.25) H6T(0.25) C7T(0.25) H7TA(0.25)
 H7TB(0.25) H7TC(0.25) C1S(0.25) C2S(0.25) H2S(0.25) C3S(0.25) H3S(0.25)
 C4S(0.25) H4S(0.25) C5S(0.25) H5S(0.25) C6S(0.25) H6S(0.25) C7S(0.25)
 H7SA(0.25) H7SB(0.25) H7SC(0.25)
7.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C17(H17), C20(H20)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C2T(H2T), C3T(H3T), C4T(H4T),
 C5T(H5T), C6T(H6T), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
7.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C7T(H7TA,H7TB,H7TC), C7S(H7SA,H7SB,H7SC)
;
_shelx_res_checksum              20331
_shelx_hkl_checksum              19794
_olex2_submission_special_instructions 'No special instructions were received'