Tandem transfer hydrogenation‒epoxidation of ketone substrates catalysed by alkene-tethered Ru(ii)‒NHC complexes
Malan, Frederick P.; Singleton, Eric; van Rooyen, Petrus H.; Landman, Marilé; New Journal of Chemistry 43 (2019) 8472–; doi:10.1039/C9NJ01220F

data_7058349
_publ_section_title
;
 Tandem transfer hydrogenation--epoxidation of ketone substrates catalysed
 by alkene-tethered Ru(ii)--NHC complexes
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8472
_journal_paper_doi               10.1039/C9NJ01220F
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C150 H148 As4 Cl4 F24 N8 P4 Ru4'
_chemical_formula_weight         3488.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-03-06 deposited with the CCDC.    2019-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   9.910(2)
_cell_length_b                   24.910(5)
_cell_length_c                   15.236(3)
_cell_measurement_reflns_used    9429
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.32
_cell_volume                     3566.6(14)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            133027
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_min         2.316
_exptl_absorpt_coefficient_mu    1.542
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1093 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.8671.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.458(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         14652
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0157P)^2^+9.7438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                13667
_reflns_number_total             14652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01220f2.cif
_cod_data_source_block           mo_FMR12_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7058342--7058349.cif.
;
_cod_database_code               7058349
_shelx_estimated_absorpt_t_min   0.617
_shelx_estimated_absorpt_t_max   0.826
_shelxl_version_number           2013-3
_shelx_res_checksum              93663