Sn,P-coordinated Ru cation: A robust catalyst for aerobic oxidations of benzylamine and benzyl alcohol
Jambor, Roman; Aman, Michal; Dostál, Libor; R°užička, Aleš; Tydlitat, Jiri; Beckmann, Jens; Turek, Jan; Chemical Communications  (2021) –; doi:10.1039/D1CC06173A

data_7129234
_publ_section_title
;
 Sn,P-coordinated Ru cation: A robust catalyst for aerobic oxidations of
 benzylamine and benzyl alcohol
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06173A
_journal_year                    2021
_chemical_formula_sum            'C44 H50 Cl N2 P Ru Sn'
_chemical_formula_weight         893.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-10-30 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.4751(11)
_cell_length_b                   11.7571(4)
_cell_length_c                   10.4836(3)
_cell_measurement_reflns_used    52302
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     4002.8(2)
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            52302
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.775
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.968
_diffrn_reflns_theta_min         2.558
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 2877 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10755
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+2.9958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.607
_reflns_Friedel_fraction_full    0.863
_reflns_Friedel_fraction_max     0.615
_reflns_number_gt                8611
_reflns_number_total             10755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06173a2.cif
_cod_data_source_block           rj190118Ru1
_cod_database_code               7129234
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.883
;
_shelx_res_checksum              70778
_shelx_hkl_checksum              69784