A Base and Solvent-Free Ruthenium-Catalyzed Alkylation of Amines
Celaje, Jeff Joseph A.; Zhang, Xingyue; Zhang, Forrest; Kam, Lisa; Herron, Jessica R.; Williams, Travis J.; ACS Catalysis 7 (2017) 1136–; doi:10.1021/acscatal.6b03088

data_4513999
_publ_section_title
;
 A Base and Solvent-Free Ruthenium-Catalyzed Alkylation of Amines
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              1136
_journal_paper_doi               10.1021/acscatal.6b03088
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C25 H39 Cl F3 Ir N O3 P S'
_chemical_formula_weight         749.25
_chemical_name_common            Iridiumcpstarnpligand
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 94.132(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1455(8)
_cell_length_b                   16.5588(16)
_cell_length_c                   20.962(2)
_cell_measurement_reflns_used    9400
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.6284
_cell_measurement_theta_min      2.4600
_cell_volume                     2820.0(5)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL XT 2013/6 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0647
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            68655
_diffrn_reflns_theta_full        30.66
_diffrn_reflns_theta_max         30.66
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    5.007
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS)'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.111
_refine_diff_density_max         2.425
_refine_diff_density_min         -1.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         8609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+14.0820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                7161
_reflns_number_total             8609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b03088_si_003.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 4513999.cif.'
_cod_database_code               4513999
_shelx_res_checksum              5987
_shelx_hkl_checksum              13624