Nitrogen-Based Ligands Accelerate Ammonia Borane Dehydrogenation with the Shvo Catalyst
Zhang, Xingyue; Lu, Zhiyao; Foellmer, Lena K.; Williams, Travis J.; Organometallics 34 (2015) 3732–; doi:10.1021/acs.organomet.5b00409

data_4086132
_publ_section_title
;
 Nitrogen-Based Ligands Accelerate Ammonia Borane Dehydrogenation with the
 Shvo Catalyst
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3732
_journal_paper_doi               10.1021/acs.organomet.5b00409
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         C39H36N2O5Ru2
_chemical_formula_sum            'C39 H36 N2 O5 Ru2'
_chemical_formula_weight         814.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3629(17)
_cell_length_b                   17.807(3)
_cell_length_c                   20.791(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.5398
_cell_measurement_theta_min      2.2713
_cell_volume                     3466.4(10)
_computing_cell_refinement       'APEX2 v2013.6-2 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTL XS 2013/1 (Bruker AXS)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59658
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2012/1'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.850
_refine_ls_abs_structure_details
;
Flack x determined using 3664 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.018(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.5760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                9004
_reflns_number_total             10566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00409_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4086132--4086133.cif.'
_cod_database_code               4086132
_shelx_res_checksum              55464
_shelx_hkl_checksum              99747