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_7225110
_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            'C74 H64 Cl10 N2 P4 Ru2'
_chemical_formula_weight         1661.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 105.027(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.1421(11)
_cell_length_b                   15.5660(5)
_cell_length_c                   16.7390(9)
_cell_measurement_reflns_used    3420
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      61.9970
_cell_measurement_theta_min      3.2590
_cell_volume                     7081.9(5)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11208
_diffrn_reflns_theta_full        62.07
_diffrn_reflns_theta_max         62.07
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    8.131
_exptl_absorpt_correction_T_max  0.6866
_exptl_absorpt_correction_T_min  0.2931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         5517
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+15.0043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                4571
_reflns_number_total             5517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra00320f2.cif
_cod_data_source_block           fxl-140506
_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_sg_symbol_H-M      C2/c
_cod_database_code               7225110