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_7715692
_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         'C70 H90 Cl2 N2 O6 P4 Ru Si2'
_chemical_formula_sum            'C70 H90 Cl2 N2 O6 P4 Ru Si2'
_chemical_formula_weight         1407.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5001(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1386(3)
_cell_length_b                   10.9694(3)
_cell_length_c                   23.2017(6)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.29
_cell_volume                     3340.71(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            73176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.114
_diffrn_reflns_theta_min         1.551
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0761 before and 0.0455 after correction. The Ratio of minimum to maximum transmission is 0.8483. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.419
_exptl_crystal_size_min          0.204
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9837
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0260P)^2^+2.7658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8409
_reflns_number_total             9837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00561a2.cif
_cod_data_source_block           3_sfj51
_cod_depositor_comments
'Adding full bibliography for 7715692--7715693.cif.'
_cod_database_code               7715692
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Restrained distances
 C10-C11 \\sim C10-C11A
 with sigma of 0.005
 O3-C11 \\sim O3-C11A
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C11A)
3. Others
 Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
;
_shelx_res_checksum              96349
_olex2_submission_special_instructions 'No special instructions were received'