Abnormal NHC ruthenium catalysts: mechanistic investigations of their preparation and steric influence on catalytic performance
Böth, Alexander D.; Sauer, Michael J.; Baratta, Walter; Kühn, Fritz E.; Catalysis Science & Technology 12 (2022) 5597–5603; doi:10.1039/D2CY01036D

data_1567424
_publ_section_title
;
 Abnormal NHC ruthenium catalysts: mechanistic investigations of their
 preparation and steric influence on catalytic performance
;
_journal_issue                   18
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5597
_journal_page_last               5603
_journal_paper_doi               10.1039/D2CY01036D
_journal_volume                  12
_journal_year                    2022
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C60 H69 N4 O2 P2 Ru, 6(C H2 Cl2), Br'
_chemical_formula_sum            'C66 H81 Br Cl12 N4 O2 P2 Ru'
_chemical_formula_weight         1630.66
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-03-29 deposited with the CCDC.	2022-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                77.650(3)
_cell_angle_beta                 88.094(3)
_cell_angle_gamma                75.630(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3315(7)
_cell_length_b                   12.2669(8)
_cell_length_c                   14.2038(10)
_cell_measurement_reflns_used    9062
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.3880
_cell_measurement_theta_min      2.2164
_cell_volume                     1867.9(2)
_computing_cell_refinement       'SAINT (Bruker, 2017)'
_computing_data_collection       'APEX III Control Software (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL (Sheldrick, 2017), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            77741
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             834
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane, Diethylether, Benzene'
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.286
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.373(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         13197
_refine_ls_number_restraints     690
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0618P)^2^+2.1130P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                12932
_reflns_number_total             13197
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d2cy01036d2.cif
_cod_data_source_block           boeal4_0m
_cod_depositor_comments          'Adding full bibliography for 1567424.cif.'
_cod_database_code               1567424
_shelx_res_checksum              55313