Rhodium complexes with planar-chiral cyclopentadienyl ligands: synthesis from tert-butylacetylene and catalytic performance in C-H activation of arylhydroxamates
Kolos, Andrey; Nelyubina, Yulia V.; Podyacheva, Evgeniya; Perekalin, Dmitry S.; Dalton Transactions  (2023) –; doi:10.1039/D3DT03279E

data_7714360
_publ_section_title
;
 Rhodium complexes with planar-chiral cyclopentadienyl ligands: synthesis
 from tert-butylacetylene and catalytic performance in C-H activation of
 arylhydroxamates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03279E
_journal_year                    2023
_chemical_formula_moiety         'C28 H44 F3 O Rh'
_chemical_formula_sum            'C28 H44 F3 O Rh'
_chemical_formula_weight         556.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-14 deposited with the CCDC.	2023-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.4463(3)
_cell_length_b                   22.9213(4)
_cell_length_c                   25.6566(4)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.51
_cell_volume                     10847.9(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            100324
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.934
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1224 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.8924.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       prism
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+35.4286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8182
_reflns_number_total             9544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03279e2.cif
_cod_data_source_block           Cp3tBu-OCH2CF3-Rhcod
_cod_database_code               7714360
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(Rh1') = Uanis(Rh1)
Uanis(Rh2') = Uanis(Rh2)
3. Others
 Sof(Rh1)=1-FVAR(1)
 Sof(Rh1')=FVAR(1)
 Sof(Rh2')=1-FVAR(2)
 Sof(Rh2)=FVAR(2)
4.a Riding coordinates:
 C21'(H21'), C22'(H22'), C25'(H25'), C26'(H26'), C21(H21), C25(H25), C22(H22),
 C26(H26)
4.b Ternary CH refined with riding coordinates:
 C6'(H6'), C6(H6)
4.c Secondary CH2 refined with riding coordinates:
 C7'(H7'A,H7'B), C23'(H23C,H23D), C24'(H24C,H24D), C27'(H27C,H27D), C28'(H28C,
 H28D), C23(H23A,H23B), C27(H27A,H27B), C7(H7A,H7B), C24(H24A,H24B), C28(H28A,
 H28B)
4.d Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C4'(H4'), C2(H2), C4(H4)
4.e Idealised Me refined as rotating group:
 C10'(H10D,H10E,H10F), C11'(H11D,H11E,H11F), C12'(H12D,H12E,H12F), C14'(H14D,
 H14E,H14F), C15'(H15D,H15E,H15F), C16'(H16D,H16E,H16F), C18'(H18D,H18E,H18F),
 C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F), C19(H19A,H19B,H19C), C15(H15A,H15B,
 H15C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,
 H18B,H18C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              48348
_olex2_submission_special_instructions 'No special instructions were received'