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_7714355
_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         'C36 H62 Br4 O2 Rh2, 2(C H Cl3)'
_chemical_formula_sum            'C38 H64 Br4 Cl6 O2 Rh2'
_chemical_formula_weight         1291.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                82.315(2)
_cell_angle_beta                 73.935(2)
_cell_angle_gamma                67.629(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2647(3)
_cell_length_b                   10.4313(3)
_cell_length_c                   12.9342(4)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.21
_cell_volume                     1230.05(7)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24487
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.112
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.275
_exptl_absorpt_correction_T_max  0.1561
_exptl_absorpt_correction_T_min  0.1103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1046 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.7066.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.748
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4814
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0413P)^2^+5.5701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4276
_reflns_number_total             4814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03279e2.cif
_cod_data_source_block           Cp3tBu-OH-RhBr2
_cod_database_code               7714355
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.566
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C10-C7 \\sim C10'-C7
 with sigma of 0.02
 C9'-C7 \\sim C9-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1) = Uanis(O1')
Uanis(C9') = Uanis(C9)
Uanis(C10') = Uanis(C10)
Uanis(Br2) = Uanis(Br2')
4. Others
 Sof(H6B)=Sof(O1)=Sof(H1)=1-FVAR(1)
 Sof(H6A)=Sof(O1')=Sof(H1')=FVAR(1)
 Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=Sof(C10')=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 FVAR(2)
 Sof(Br2)=1-FVAR(3)
 Sof(Br2')=FVAR(3)
5.a Riding coordinates:
 O1'(H1'), O1(H1)
5.b Ternary CH refined with riding coordinates:
 C6(H6B), C6(H6A), C1S(H1S)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C9'(H9'A,H9'B,H9'C), C10'(H10D,H10E,H10F)
;
_shelx_res_checksum              24379
_olex2_submission_special_instructions 'No special instructions were received'