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_7714361
_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_absolute_configuration rmad
_chemical_formula_moiety         'C38 H66 Cl4 O2 Rh2'
_chemical_formula_sum            'C38 H66 Cl4 O2 Rh2'
_chemical_formula_weight         902.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3786(10)
_cell_length_b                   14.1588(6)
_cell_length_c                   23.2064(9)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.15
_cell_volume                     8338.8(6)
_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      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII DUO CCDC'
_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  0.1140
_diffrn_reflns_av_unetI/netI     0.1166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67086
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.829
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1465 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.7975.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       needle
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.967
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         18157
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0228P)^2^+9.5623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14558
_reflns_number_total             18157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03279e2.cif
_cod_data_source_block           Cp3tBu3OMeRhCl2
_cod_database_code               7714361
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.704
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(4)
 0.46(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C02G(H02G), C6A(H6A), C25(H25), C6(H6)
4.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C4A(H4A), C21A(H21A), C23A(H23A), C23(H23), C21(H21), C2(H2), C4(H4)
4.c Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C11A(H11D,
 H11E,H11F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F),
 C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C25A(H25A,
 H25B,H25C), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F),
 C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C35A(H35A,
 H35B,H35C), C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C), C17(H17A,H17B,H17C),
 C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C19(H19A,H19B,
 H19C), C14(H14A,H14B,H14C), C00X(H00A,H00B,H00C), C29(H29A,H29B,H29C),
 C00Y(H00D,H00E,H00F), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C01K(H01A,H01B,
 H01C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C7(H7A,H7B,H7C), C28(H28A,
 H28B,H28C), C9(H9A,H9B,H9C), C32(H32A,H32B,H32C), C10(H10A,H10B,H10C),
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              47066
_olex2_submission_special_instructions 'No special instructions were received'