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_4082832
_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         'C58 H48 Cl O2 P3 Ru, C6 H6'
_chemical_formula_sum            'C64 H54 Cl O2 P3 Ru'
_chemical_formula_weight         1084.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.760(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.0327(7)
_cell_length_b                   11.5362(3)
_cell_length_c                   16.0877(7)
_cell_measurement_reflns_used    46042
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.58
_cell_volume                     2591.14(18)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52253
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         11899
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.5239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                11279
_reflns_number_total             11899
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om4011998_si_002.cif
_cod_data_source_block           l0360a
_cod_depositor_comments          'Adding full bibliography for 4082832.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4082832