Mechanistic Study on the Ruthenium-Catalyzed Direct Amination of Alcohols
Pingen, Dennis; Lutz, Martin; Vogt, Dieter; Organometallics 33 (2014) 1623–; doi:10.1021/om4011998

data_4082833
_publ_section_title
;
 Mechanistic Study on the Ruthenium-Catalyzed Direct Amination of Alcohols
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1623
_journal_paper_doi               10.1021/om4011998
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C57 H47 Cl2 O P3 Ru,  0.6(C7 H8)'
_chemical_formula_sum            'C61.2 H51.8 Cl2 O P3 Ru'
_chemical_formula_weight         1068.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.649(2)
_cell_angle_beta                 102.056(1)
_cell_angle_gamma                90.409(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3253(3)
_cell_length_b                   12.3579(5)
_cell_length_c                   20.3347(5)
_cell_measurement_reflns_used    43855
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.73
_cell_volume                     2659.71(15)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2008/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59328
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         12201
_refine_ls_number_restraints     964
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+3.2875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                10094
_reflns_number_total             12201
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om4011998_si_002.cif
_cod_data_source_block           l0376a
_cod_depositor_comments          'Adding full bibliography for 4082833.cif.'
_cod_original_cell_volume        2659.69(15)
_cod_original_formula_sum        'C61.20 H51.80 Cl2 O P3 Ru'
_cod_database_code               4082833