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_7058342
_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            'C15.5 H16 I1.5 N P0.5 Ru0.5'
_chemical_formula_weight         472.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                91.365(6)
_cell_angle_beta                 94.352(6)
_cell_angle_gamma                114.451(5)
_cell_formula_units_Z            4
_cell_length_a                   9.4358(17)
_cell_length_b                   9.7889(19)
_cell_length_c                   18.948(4)
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.29
_cell_volume                     1585.7(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.879
_diffrn_reflns_theta_min         2.160
_exptl_absorpt_coefficient_mu    3.488
_exptl_absorpt_correction_T_max  0.4908
_exptl_absorpt_correction_T_min  0.4039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1280 before and 0.0455 after correction.
The Ratio of minimum to maximum transmission is 0.8229.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.310
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0123P)^2^+2.2591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5866
_reflns_number_total             6706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01220f2.cif
_cod_data_source_block           mo_FMTest3_0m_a
_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_original_cell_volume        1585.6(5)
_cod_original_formula_sum        'C15.50 H16 I1.50 N P0.50 Ru0.50'
_cod_database_code               7058342
_shelx_estimated_absorpt_t_min   0.549
_shelx_estimated_absorpt_t_max   0.690
_shelxl_version_number           2013-3
_shelx_res_checksum              48682