Ammonia borane and hydrazine bis(borane) dehydrogenation mediated by an unsymmetrical (PNN) ruthenium pincer hydride: metal‒ligand cooperation for hydrogen production
Luconi, Lapo; Demirci, Umit B.; Peruzzini, Maurizio; Giambastiani, Giuliano; Rossin, Andrea; Sustainable Energy & Fuels 3 (2019) 2583–; doi:10.1039/C9SE00241C

data_1555299
_publ_section_title
;
 Ammonia borane and hydrazine bis(borane) dehydrogenation mediated by an
 unsymmetrical (PNN) ruthenium pincer hydride: metal--ligand cooperation
 for hydrogen production
;
_journal_issue                   10
_journal_name_full               'Sustainable Energy &amp; Fuels'
_journal_page_first              2583
_journal_paper_doi               10.1039/C9SE00241C
_journal_volume                  3
_journal_year                    2019
_chemical_formula_moiety         'C22 H33 N4 O P Ru'
_chemical_formula_sum            'C22 H33 N4 O P Ru'
_chemical_formula_weight         501.56
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_date             2019-03-05T10:51:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-04-01 deposited with the CCDC.	2019-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                79.305(2)
_cell_angle_beta                 86.313(2)
_cell_angle_gamma                81.975(2)
_cell_formula_units_Z            4
_cell_length_a                   8.4345(3)
_cell_length_b                   14.1852(3)
_cell_length_c                   20.2401(5)
_cell_measurement_reflns_used    12371
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.5450
_cell_measurement_theta_min      4.4240
_cell_measurement_wavelength     1.54184
_cell_volume                     2354.42(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-2014 (Burla et al., 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1241
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0383709
_diffrn_orient_matrix_UB_12      0.0681567
_diffrn_orient_matrix_UB_13      0.0515835
_diffrn_orient_matrix_UB_21      0.1799636
_diffrn_orient_matrix_UB_22      -0.0075647
_diffrn_orient_matrix_UB_23      0.0124947
_diffrn_orient_matrix_UB_31      0.0147634
_diffrn_orient_matrix_UB_32      0.0878835
_diffrn_orient_matrix_UB_33      -0.0565016
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23906
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.811
_diffrn_reflns_theta_min         4.21
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.092
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.81088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040.0
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.085
_reflns_Friedel_coverage         0
_reflns_number_gt                7226
_reflns_number_total             8774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9se00241c2.cif
_cod_data_source_block           2_MeCN
_cod_database_code               1555299
_oxdiff_exptl_absorpt_empirical_full_min 0.596
_oxdiff_exptl_absorpt_empirical_full_max 3.287
_shelx_shelxl_version_number     2018/3