Synthesis and catalytic performance of ruthenium complexes ligated with rigid o-(diphenylphosphino)aniline for chemoselective hydrogenation of dimethyl oxalate
Fang, Xiaolong; Zhang, Chunyan; Chen, Jin; Zhu, Hongping; Yuan, Youzhu; RSC Adv.  (2016) –; doi:10.1039/C6RA00320F

data_7225115
_publ_section_title
;
 Synthesis and catalytic performance of ruthenium complexes ligated with
 rigid o-(diphenylphosphino)aniline for chemoselective hydrogenation of
 dimethyl oxalate
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA00320F
_journal_year                    2016
_chemical_formula_sum            'C100.5 H91 Cl3 N5 O0 P5 Ru2'
_chemical_formula_weight         1832.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-20 deposited with the CCDC.
2016-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.598(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4725(7)
_cell_length_b                   44.037(3)
_cell_length_c                   16.4716(9)
_cell_measurement_reflns_used    1490
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.8560
_cell_measurement_theta_min      3.3740
_cell_volume                     9017.9(9)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhanced (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_sigmaI/netI    0.2063
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30813
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.9459
_exptl_absorpt_correction_T_min  0.8495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            'golden yellow'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3772
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment
'refined in a riding mode to the carrier atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         15820
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1804
_refine_ls_R_factor_gt           0.0968
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1929
_reflns_number_gt                8771
_reflns_number_total             15820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra00320f2.cif
_cod_data_source_block           fxl-130823
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/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.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        9018.0(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C100.50 H91 Cl3 N5 O0 P5 Ru2'
_cod_database_code               7225115