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_7713782
_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 H37 Cl N2 Os P S, F6 Sb'
_chemical_formula_sum            'C32 H37 Cl F6 N2 Os P S Sb'
_chemical_formula_weight         974.06
_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
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                97.1740(10)
_cell_angle_beta                 103.529(2)
_cell_angle_gamma                99.2620(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3781(9)
_cell_length_b                   10.4833(9)
_cell_length_c                   16.9677(15)
_cell_measurement_reflns_used    2936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.345
_cell_measurement_theta_min      2.170
_cell_volume                     1745.8(3)
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_device_type  'Bruker APEX DUO CCD system'
_diffrn_measurement_method       'narrow \w frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17326
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.247
_diffrn_reflns_theta_min         1.997
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.649
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction was carried out with SORTAV program.
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/n-hexane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.918
_refine_diff_density_min         -1.775
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8271
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0186P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6087
_reflns_number_total             8271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02339g4.cif
_cod_data_source_block           cmpnd_2
_cod_database_code               7713782
_shelxl_version_number           2014-3
_shelx_res_checksum              5746