Molecular hydrogen and water activation by transition metal frustrated Lewis pairs containing ruthenium or osmium components: catalytic hydrogenation assays
Lamata, Pilar; Beard, Sophie; Grasa, Alejandro; Viguri, Fernando; Ricardo, Rodriguez Martinez; López, José A.; Lahoz, Fernando J.; García-Orduña, Pilar; Carmona, Daniel; Dalton Transactions  (2023) –; doi:10.1039/D3DT02339G

data_7713786
_publ_section_title
;
 Molecular hydrogen and water activation by transition metal frustrated
 Lewis pairs containing ruthenium or osmium components: catalytic
 hydrogenation assays
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02339G
_journal_year                    2023
_chemical_formula_moiety
'C32 H36 N2 Os P S, 2(F6 Sb),5(H2 O), C6 H14, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C38.5 H62 Cl F12 N5 O Os P S Sb2'
_chemical_formula_weight         1371.11
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                86.7350(10)
_cell_angle_beta                 80.2470(10)
_cell_angle_gamma                81.2590(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1759(6)
_cell_length_b                   15.2630(8)
_cell_length_c                   15.4343(8)
_cell_measurement_reflns_used    8221
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.476
_cell_measurement_theta_min      2.288
_cell_volume                     2333.9(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_data_collection       'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       'narrow \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26736
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.644
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.087
_exptl_absorpt_correction_T_max  0.7278
_exptl_absorpt_correction_T_min  0.5885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_description       plate
_exptl_crystal_F_000             1340
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/n-hexane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.720
_refine_diff_density_min         -2.038
_refine_diff_density_rms         0.163
_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     473
_refine_ls_number_reflns         10801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0279P)^2^+11.6736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8824
_reflns_number_total             10801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02339g4.cif
_cod_data_source_block           cmpnd_4
_cod_original_formula_sum        'C38.50 H62 Cl F12 N5 O Os P S Sb2'
_cod_database_code               7713786
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.763
_shelx_estimated_absorpt_t_min   0.579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(F10B)=Sof(F9B)=Sof(F12B)=Sof(F11B)=1-FVAR(1)
 Sof(F10A)=Sof(F9A)=Sof(F12A)=Sof(F11A)=FVAR(1)
3.a Free rotating group:
 O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C8(H8)
3.c Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B)
3.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27),
  C28(H28), C30(H30), C31(H31)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24854
_shelx_fab_checksum              87529
_olex2_submission_special_instructions 'No special instructions were received'