Planar-chiral arene ruthenium complexes: synthesis, separation of enantiomers, and application for catalytic C-H activation.
Boym, Mikhail A.; Pototskiy, Roman A.; Podyacheva, Evgeniya S.; Chusov, Denis A.; Nelyubina, Yulia V.; Perekalin, Dmitry S.; Chemical communications (Cambridge, England) 60 (2024) 4491–4494; doi:10.1039/d4cc00181h

data_7132893
_publ_section_title
;
 Planar-chiral arene ruthenium complexes: synthesis, separation of
 enantiomers, and application for catalytic C-H activation.
;
_journal_issue                   33
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4491
_journal_page_last               4494
_journal_paper_doi               10.1039/d4cc00181h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C34 H39 Cl2 O P Ru, C H2 Cl2'
_chemical_formula_sum            'C35 H41 Cl4 O P Ru'
_chemical_formula_weight         751.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.3460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0658(2)
_cell_length_b                   15.2520(4)
_cell_length_c                   11.7038(3)
_cell_measurement_reflns_used    5647
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.29
_cell_volume                     1684.71(7)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Quest D8 '
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22525
_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         29.000
_diffrn_reflns_theta_min         1.856
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0617 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.8693.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8409
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0186P)^2^+0.0320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7187
_reflns_number_total             8409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00181h3.cif
_cod_data_source_block           6a
_cod_depositor_comments
'Adding full bibliography for 7132893--7132895.cif.'
_cod_database_code               7132893
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.783
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98(4)
 0.02(4)
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. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C32') \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C29') = Uanis(C29)
Uanis(C30') = Uanis(C30)
Uanis(C32') = Uanis(C32)
Uanis(C34') = Uanis(C34)
Uanis(C31) = Uanis(C31')
Uanis(C33) = Uanis(C33')
4. Others
 Sof(H27A)=Sof(C29')=Sof(C30')=Sof(H30')=Sof(C31')=Sof(H31')=Sof(C32')=
 Sof(H32')=Sof(C33')=Sof(H33')=Sof(C34')=Sof(H34')=1-FVAR(1)
 Sof(H27)=Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=
 Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C27(H27), C27(H27A)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C1S(H1SA,H1SB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C30'(H30'), C31'(H31'), C32'(H32'), C33'(H33'), C34'(H34')
5.d Fitted hexagon refined as free rotating group:
 C29(C30,C31,C32,C33,C34), C29'(C30',C31',C32',C33',C34')
5.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              78277
_shelx_hkl_checksum              53187
_olex2_submission_special_instructions 'No special instructions were received'