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_1555298
_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_absolute_configuration unk
_chemical_formula_moiety         'C38  H45  N3 O P2 Ru, C7 H8'
_chemical_formula_sum            'C45 H53 N3 O P2 Ru'
_chemical_formula_weight         814.91
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-05T14:48:25-00:00
_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                90
_cell_angle_beta                 108.396(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.512(5)
_cell_length_b                   12.577(6)
_cell_length_c                   16.003(6)
_cell_measurement_reflns_used    5753
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.3740
_cell_measurement_theta_min      4.5670
_cell_measurement_wavelength     1.54184
_cell_volume                     2007.6(15)
_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 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.97
_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      -0.0339725
_diffrn_orient_matrix_UB_12      0.1104334
_diffrn_orient_matrix_UB_13      0.0290355
_diffrn_orient_matrix_UB_21      0.0844823
_diffrn_orient_matrix_UB_22      -0.0249975
_diffrn_orient_matrix_UB_23      0.0956558
_diffrn_orient_matrix_UB_31      0.1246986
_diffrn_orient_matrix_UB_32      0.0469139
_diffrn_orient_matrix_UB_33      -0.0172057
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.08
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.97
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11249
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.8
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         72.361
_diffrn_reflns_theta_min         4.47
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.2
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.36642
_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            orange
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.115
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6341
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+3.3650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.574
_reflns_Friedel_fraction_full    0.66
_reflns_Friedel_fraction_max     0.613
_reflns_number_gt                5539
_reflns_number_total             6341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9se00241c2.cif
_cod_data_source_block           2_PPh3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1555298
_shelx_shelxl_version_number     2018/3