Catalytic Acceptorless Dehydrogenation of Amines with Ru(PR2NR′2) and Ru(dppp) Complexes
Stubbs, James M.; Hazlehurst, Richard J.; Boyle, Paul D.; Blacquiere, Johanna M.; Organometallics 36 (2017) 1692–; doi:10.1021/acs.organomet.6b00870

data_4089184
_publ_section_title
;
 Catalytic Acceptorless Dehydrogenation of Amines with Ru(PR2NR&#x2032;2)
 and Ru(dppp) Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1692
_journal_paper_doi               10.1021/acs.organomet.6b00870
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C39 H46 F6 N3 P3 Ru'
_chemical_formula_weight         864.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.179(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.564(3)
_cell_length_b                   23.741(9)
_cell_length_c                   15.120(6)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    110
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.58
_cell_volume                     3792(2)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1162
_diffrn_reflns_av_unetI/netI     0.1089
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55233
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.621
_diffrn_reflns_theta_min         1.715
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.435
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0841P)^2^+5.2475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4999
_reflns_number_total             7828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00870_si_002.cif
_cod_data_source_block           b15352
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089184
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              84511
_shelx_hkl_checksum              94512