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_7714359
_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         '2(C21 H31 Cl2 F6 O Rh), C H2 Cl2'
_chemical_formula_sum            'C43 H64 Cl6 F12 O2 Rh2'
_chemical_formula_weight         1259.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                 99.9180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0112(4)
_cell_length_b                   21.2381(5)
_cell_length_c                   14.5656(4)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.27
_cell_volume                     5183.7(2)
_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 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            63687
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.548
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1145 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.7319.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       prism
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         12503
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+6.7308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10698
_reflns_number_total             12503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03279e2.cif
_cod_data_source_block           Cp3tBu-HFIP-RhCl2
_cod_database_code               7714359
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.749
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2S-C1S \\sim Cl3-C1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3) = Uanis(Cl2S)
4. Others
 Sof(H1SC)=Sof(H1SD)=Sof(Cl3)=1-FVAR(1)
 Sof(H1SA)=Sof(H1SB)=Sof(Cl2S)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C6'(H6'), C7'(H7'), C6(H6)
5.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1S(H1SC,H1SD)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C2'(H2'), C4(H4), C4'(H4')
5.d Idealised Me refined as rotating group:
 C11'(H11D,H11E,H11F), C12'(H12D,H12E,H12F), C11(H11A,H11B,H11C), C13'(H13D,
 H13E,H13F), C15'(H15D,H15E,H15F), C16'(H16D,H16E,H16F), C17'(H17D,H17E,H17F),
 C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17B,H17C,H17A), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C21'(H21D,H21E,H21F), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              14680
_olex2_submission_special_instructions 'No special instructions were received'