Backbone-functionalised ruthenium diphosphine complexes for catalytic upgrading of ethanol and methanol to iso-butanol.
Sama, Folasade J.; Doyle, Rachel A.; Kariuki, Benson M.; Pridmore, Natalie E.; Sparkes, Hazel A.; Wingad, Richard L.; Wass, Duncan F.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8005–8010; doi:10.1039/d4dt00561a

data_7715693
_publ_section_title
;
 Backbone-functionalised ruthenium diphosphine complexes for catalytic
 upgrading of ethanol and methanol to iso-butanol.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8005
_journal_page_last               8010
_journal_paper_doi               10.1039/d4dt00561a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C66 H62 Cl2 N2 P4 Ru, 0.84(C6 H5 F), 0.6(C5 H12)'
_chemical_formula_sum            'C74.03 H73.39 Cl2 F0.84 N2 P4 Ru'
_chemical_formula_weight         1302.90
_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             2018-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                86.830(2)
_cell_angle_beta                 82.892(2)
_cell_angle_gamma                66.874(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3517(3)
_cell_length_b                   11.7890(3)
_cell_length_c                   14.7461(4)
_cell_measurement_reflns_used    3403
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.86
_cell_measurement_theta_min      2.24
_cell_volume                     1642.19(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker Apex suite'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0666
_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       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27125
_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         26.367
_diffrn_reflns_theta_min         1.878
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0789 before and 0.0597 after correction. The Ratio of minimum to maximum transmission is 0.7944. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             677
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6706
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0602P)^2^+0.9517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5125
_reflns_number_total             6706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00561a2.cif
_cod_data_source_block           4_SFJ50
_cod_depositor_comments
'Adding full bibliography for 7715692--7715693.cif.'
_cod_database_code               7715693
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C35B-C34B = C35A-C34A = C36A-C35A = C36B-C35B = C37A-C36A = C37B-C36B = C38B-
 C37B = C38A-C37A
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C34A \\sim
C38A \\sim C36A \\sim C37A \\sim C35A \\sim C37B \\sim C38B \\sim C36B \\sim
C35B \\sim C34B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006
Uanis(C35B) = Uanis(C35A)
Uanis(C34B) = Uanis(C34A)
4. Others
 1*[Sof(C34A)+Sof(H34A)+Sof(H34B)+Sof(H34C)+Sof(C38A)+Sof(H38A)+Sof(H38B)+
 Sof(H38C)+Sof(C36A)+Sof(H36A)+Sof(H36B)+Sof(C37A)+Sof(H37A)+Sof(H37B)+
 Sof(C35A)+Sof(H35A)+Sof(H35B)]+1*[Sof(C37B)+Sof(H37C)+Sof(H37D)+Sof(C38B)+
 Sof(H38D)+Sof(H38E)+Sof(H38F)+Sof(C36B)+Sof(H36C)+Sof(H36D)+Sof(C35B)+
 Sof(H35C)+Sof(H35D)+Sof(C34B)+Sof(H34D)+Sof(H34E)+Sof(H34F)]=0.3 with esd of 0
 Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C38A)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=
 Sof(C35A)=Sof(H35A)=Sof(H35B)=FVAR(1)
 Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(H38D)=Sof(H38E)=Sof(H38F)=
 Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C34B)=
 Sof(H34D)=Sof(H34E)=Sof(H34F)=FVAR(2)
 Fixed Sof: F1(0.41936) C34(0.41936) C35(0.41936) H35(0.41936) C36(0.41936)
 H36(0.41936) C37(0.41936) H37(0.41936) C38(0.41936) H38(0.41936) C39(0.41936)
 H39(0.41936)
5.a Ternary CH refined with riding coordinates:
 C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C36A(H36A,H36B), C37A(H37A,H37B), C35A(H35A,
 H35B), C37B(H37C,H37D), C36B(H36C,H36D), C35B(H35C,H35D)
5.c Me refined with riding coordinates:
 C38A(H38A,H38B,H38C), C38B(H38D,H38E,H38F), C34B(H34D,H34E,H34F)
5.d Aromatic/amide H refined with riding coordinates:
 C27(H27), C12(H12), C29(H29), C23(H23), C8(H8), C11(H11), C31(H31), C5(H5),
 C30(H30), C2(H2), C33(H33), C3(H3), C24(H24), C4(H4), C6(H6), C32(H32),
 C26(H26), C25(H25), C17(H17), C10(H10), C9(H9), C20(H20), C18(H18), C19(H19),
 C21(H21), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
5.e Fitted hexagon refined as free rotating group:
 C34(C35,C36,C37,C38,C39)
5.f Idealised Me refined as rotating group:
 C34A(H34A,H34B,H34C)
;
_shelx_res_checksum              9660
_olex2_submission_special_instructions 'No special instructions were received'