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_7713789
_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_absolute_configuration rmad
_chemical_formula_moiety         'C35 H41 N4 O2 Ru, F6 Sb, C4 H8 O'
_chemical_formula_sum            'C39 H49 F6 N4 O3 Ru Sb'
_chemical_formula_weight         958.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-06-10
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6436(8)
_cell_length_b                   15.5640(11)
_cell_length_c                   21.8392(15)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.279
_cell_volume                     3957.7(5)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52333
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.302
_diffrn_reflns_theta_min         1.865
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1194 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.7822.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: deuterated THF'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 2982 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.039(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0345P)^2^+6.0508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                7702
_reflns_number_total             9779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02339g4.cif
_cod_data_source_block           cmpnd_20
_cod_database_code               7713789
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.876
_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
2.a Ternary CH refined with riding coordinates:
 C16(H16), C32(H32), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C52(H52A,H52B)
2.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C29(H29), C11(H11), N4(H4), C14(H14), C13(H13), C12(H12), C27(H27),
 C26(H26), N3(H3), C23(H23), C19(H19), C22(H22), C2(H2), C6(H6), C5(H5),
 C3(H3A), C20(H20)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C31(H31A,H31B,H31C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C24(H24A,H24B,H24C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              41037
_olex2_submission_special_instructions 'No special instructions were received'