Unsaturated chiral-only-at-metal rhodium(III) complexes bearing SiN-type ligands.
Prieto-Pascual, Unai; Bustos, Itxaso; Salcedo-Abraira, Pablo; Vitorica-Yrezabal, Iñigo J; Landa, Aitor; Freixa, Zoraida; Huertos, Miguel A.; Chemical communications (Cambridge, England) 60 (2024) 11299–11302; doi:10.1039/d4cc03665d

data_7133825
_publ_section_title
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 Unsaturated chiral-only-at-metal rhodium(III) complexes bearing SiN-type
 ligands.
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_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11299
_journal_page_last               11302
_journal_paper_doi               10.1039/d4cc03665d
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H36 B N2 O6 Rh Si2, C H2 Cl2'
_chemical_formula_sum            'C39 H38 B Cl2 N2 O6 Rh Si2'
_chemical_formula_weight         871.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-09-02
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
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_audit_update_record
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2024-09-02 deposited with the CCDC.	2024-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.5875(7)
_cell_length_b                   22.565(2)
_cell_length_c                   40.397(3)
_cell_measurement_reflns_used    3477
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      24.061
_cell_measurement_theta_min      2.755
_cell_volume                     7828.0(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2058
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16076
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.459
_diffrn_reflns_theta_min         2.017
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1288 before and 0.0933 after correction.
The Ratio of minimum to maximum transmission is 0.6886.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       needle
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Flack x determined using 2265 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         16076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1984
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                7800
_reflns_number_total             16076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03665d2.cif
_cod_data_source_block           d-rh(sin)[r-b(s-man)2]
_cod_original_cell_volume        7828.0(12)
_cod_database_code               7133825
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.821
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.0008(15)
 -0.0008(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C29A(H29A), C37A(H37A), C29B(H29B), C37B(H37B)
3.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
3.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C12A(H12A),
 C13A(H13A), C14A(H14A), C16A(H16A), C17A(H17A), C18A(H18A), C23A(H23A),
 C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C31A(H31A), C32A(H32A),
 C33A(H33A), C34A(H34A), C35A(H35A), C1B(H1B), C2B(H2B), C3B(H3B), C5B(H5B),
 C6B(H6B), C7B(H7B), C12B(H12B), C13B(H13B), C14B(H14B), C16B(H16B), C17B(H17B),
  C18B(H18B), C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B),
 C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B)
3.d Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C), C21A(H21A,H21B,H21C), C22A(H22A,
 H22B,H22C), C10B(H10D,H10E,H10F), C11B(H11D,H11E,H11F), C21B(H21D,H21E,H21F),
 C22B(H22D,H22E,H22F)
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_shelx_res_checksum              50778
_shelx_hkl_checksum              91599
_olex2_submission_special_instructions 'No special instructions were received'