Dehydrogenation of formic acid by Ir–bisMETAMORPhos complexes: experimental and computational insight into the role of a cooperative ligand
Oldenhof, Sander; Lutz, Martin; de Bruin, Bas; Ivar van der Vlugt, Jarl; Reek, Joost N. H.; Chem. Sci. 6 (2015) 1027–; doi:10.1039/C4SC02555E

data_1518097
_publ_section_title
;
 Dehydrogenation of formic acid by Ir--bisMETAMORPhos complexes:
 experimental and computational insight into the role of a cooperative
 ligand
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1027
_journal_paper_doi               10.1039/C4SC02555E
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety
'C57 H71 Ir N2 O6 P2 S2, C H2 Cl2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C60 H78 Cl2 Ir N2 O6.5 P2 S2'
_chemical_formula_weight         1320.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                113.198(2)
_cell_angle_beta                 95.475(2)
_cell_angle_gamma                105.211(1)
_cell_formula_units_Z            2
_cell_length_a                   11.6106(3)
_cell_length_b                   17.2668(6)
_cell_length_c                   18.6161(4)
_cell_measurement_reflns_used    44333
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      1.87
_cell_volume                     3226.00(17)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, Twinabs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.718
_diffrn_reflns_theta_min         1.865
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.314
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2012/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       needle
_exptl_crystal_F_000             1354
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.458
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         14853
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0534P)^2^+2.4464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14073
_reflns_number_total             14853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc02555e2.cif
_cod_data_source_block           l0612a
_cod_depositor_comments          'Adding full bibliography for 1518097.cif.'
_cod_original_cell_volume        3226.02(16)
_cod_original_formula_sum        'C60 H78 Cl2 Ir N2 O6.50 P2 S2'
_cod_database_code               1518097
_shelxl_version_number           2013-4
_shelx_res_checksum              25091