Bimetallic Ru-Ir/Rh complexes for catalytic allyl alcohol reduction to propylene.
Kawaji, Kanade; Tsujiwaki, Mina; Kiso, Ayaka; Kitajo, Yukina; Kitamura, Manami; Nishimura, Minako; Horikawa, Junya; Ikushuma, Haruto; Takemoto, Shin; Matsuzaka, Hiroyuki; Chemical communications (Cambridge, England) 60 (2024) 9424–9427; doi:10.1039/d4cc01711k

data_7133460
_publ_section_title
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 Bimetallic Ru-Ir/Rh complexes for catalytic allyl alcohol reduction to
 propylene.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9424
_journal_page_last               9427
_journal_paper_doi               10.1039/d4cc01711k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C47 H36 N4 P2 Rh Ru, 2(C F3 O3 S), C H4 O'
_chemical_formula_sum            'C50 H45 F6 N4 O7 P2 Rh Ru S2'
_chemical_formula_weight         1257.94
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-16 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                99.607(7)
_cell_angle_beta                 95.647(7)
_cell_angle_gamma                92.404(7)
_cell_formula_units_Z            2
_cell_length_a                   12.8700(6)
_cell_length_b                   13.8567(6)
_cell_length_c                   14.2225(7)
_cell_measurement_reflns_used    20169
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.04
_cell_volume                     2484.3(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23068
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         3.044
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       plate
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.857
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         11096
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0315P)^2^+7.6929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9404
_reflns_number_total             11096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01711k2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7133459--7133461.cif.'
_cod_database_code               7133460
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.672
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 Rh-C3 \\sim Rh-C
 with sigma of 0.02
 C2-C3 \\sim C2-C
 with sigma of 0.02
 C1-C3 \\sim C1-C
 with sigma of 0.02
 C50-F5 \\sim C50-F6
 with sigma of 0.02
 C50-F7 \\sim C50-F8
 with sigma of 0.02
 F7-F6 \\sim F8-F6
 with sigma of 0.02
 S2-O4 \\sim S2-O5
 with sigma of 0.02
 S2-O6 \\sim S2-O7
 with sigma of 0.02
 S2-O8 \\sim S3-O8
 with sigma of 0.02
 S2-O6 \\sim S3-O6
 with sigma of 0.02
 S2-C50 \\sim S3-C50
 with sigma of 0.02
 S2-O4 \\sim S3-O4
 with sigma of 0.02
 S2-O5 \\sim S3-O5
 with sigma of 0.02
 S2-O7 \\sim S3-O7
 with sigma of 0.02
 S2-O8 \\sim S2-O9
 with sigma of 0.02
 O8-S3 \\sim O9-S3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C)
Uanis(F5) = Uanis(F6)
Uanis(O9) = Uanis(O8)
Uanis(F7) = Uanis(F8)
Uanis(F6) = Uanis(F5)
Uanis(S3) = Uanis(S2)
Uanis(O7) = Uanis(O6)
Uanis(O4) = Uanis(O5)
4. Others
 Sof(O5)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Sof(O7)=1-FVAR(2)
 Sof(O6)=FVAR(2)
 Sof(S3)=1-FVAR(3)
 Sof(S2)=FVAR(3)
 Sof(O9)=1-FVAR(4)
 Sof(O8)=FVAR(4)
 Fixed Sof: F7(0.49856) C3(0.4785) C(0.5215) F5(0.53682) F6(0.46318) F8(0.50144)
5.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C15(H15), C33(H33), C36(H36), C39(H39), C28(H28), C17(H17),
 C23(H23), C14(H14), C27(H27), C46(H46), C11(H11), C43(H43), C13(H13), C34(H34),
  C35(H35), C21(H21), C26(H26), C24(H24), C41(H41), C9(H9), C6(H6), C7(H7),
 C44(H44), C31(H31), C25(H25), C5(H5), C45(H45), C29(H29), C12(H12), C18(H18),
 C40(H40), C8(H8), C30(H30), C20(H20), C19(H19)
5.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C)
5.c Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_shelx_res_checksum              96662
_shelx_hkl_checksum              70178
_olex2_submission_special_instructions 'No special instructions were received'