Dehydrogenation of Formic Acid Promoted by a Trihydride-Hydroxo-Osmium(IV) Complex: Kinetics and Mechanism
Esteruelas, Miguel A.; García-Yebra, Cristina; Martín, Jaime; Oñate, Enrique; ACS Catalysis 8 (2018) 11314–; doi:10.1021/acscatal.8b02370

data_4515817
_publ_section_title
;
 Dehydrogenation of Formic Acid Promoted by a
 Trihydride-Hydroxo-Osmium(IV) Complex: Kinetics and Mechanism
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              11314
_journal_paper_doi               10.1021/acscatal.8b02370
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C28 H44 O3 Os P2'
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_space_group_name_Hall           '-P 2ybc'
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_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.174(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.878(2)
_cell_length_b                   10.9673(15)
_cell_length_c                   16.462(2)
_cell_measurement_reflns_used    6076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2866.7(6)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
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_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
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_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX DUO system'
_diffrn_measurement_method       '\w rotations with narrow 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  0.0540
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.499
_diffrn_reflns_theta_max         25.499
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_diffrn_standards_decay_%        0
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_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            colourless
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_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
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_refine_ls_number_parameters     323
_refine_ls_number_reflns         5335
_refine_ls_number_restraints     13
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_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0363
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+5.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3419
_reflns_number_total             5335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02370_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2866.5(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4515817
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.478
_shelx_estimated_absorpt_t_max   0.678
_shelx_res_checksum              4871
_shelx_hkl_checksum              25841