Catalyst Evolution in Ruthenium-Catalyzed Coupling of Amines and Alcohols
Cherepakhin, Valeriy; Williams, Travis J.; ACS Catalysis  (2019) 56–; doi:10.1021/acscatal.9b03679

data_4517150
_publ_section_title
;
 Catalyst Evolution in Ruthenium-Catalyzed Coupling of Amines and Alcohols
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              56
_journal_paper_doi               10.1021/acscatal.9b03679
_journal_year                    2019
_chemical_formula_moiety         'C43 H71 Cl2 N3 O P3 Ru3, C F3 O3 S'
_chemical_formula_sum            'C44 H71 Cl2 F3 N3 O4 P3 Ru3 S'
_chemical_formula_weight         1262.11
_chemical_name_common            Ru3
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 97.812(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.400(5)
_cell_length_b                   20.266(8)
_cell_length_c                   19.218(8)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      16.0978
_cell_measurement_theta_min      1.4774
_cell_volume                     5170(4)
_computing_cell_refinement       'APEX3 v2018.1-0 (Bruker AXS, 2018)'
_computing_data_collection
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2013)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material  'SHELXTL XL 2017/1 (Bruker AXS, 2017)'
_computing_structure_refinement  'SHELXTL XL 2017/1 (Bruker AXS, 2017)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1778
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83773
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.47
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.554
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.896
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         8811
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0115P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                5674
_reflns_number_total             8811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b03679_si_002.cif
_cod_data_source_block           Ru3
_cod_original_cell_volume        5170.(4)
_cod_database_code               4517150
_shelx_res_checksum              47264
_shelx_hkl_checksum              79207