Construction of Pincer-Type symmetrical Ruthenium(II) complexes bearing a Pyridyl-2,6-Pyrazolyl Arms: Catalytic Behavior in Transfer Hydrogenation of Ketones
Zhu, Zhu; Zhang, Jie; Fu, Haiyan; Yuan, Maolin; Zheng, Xueli; Chen, Hua; li, ruixiang; RSC Adv.  (2014) –; doi:10.1039/C4RA07524B

data_7218378
_publ_section_title
;
 Construction of Pincer-Type symmetrical Ruthenium(II) complexes bearing a
 Pyridyl-2,6-Pyrazolyl Arms: Catalytic Behavior in Transfer Hydrogenation
 of Ketones
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA07524B
_journal_year                    2014
_chemical_formula_moiety         'C33 H32 Cl2 N5 P Ru'
_chemical_formula_sum            'C33 H32 Cl2 N5 P Ru'
_chemical_formula_weight         701.57
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-09-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4349(4)
_cell_length_b                   14.1604(4)
_cell_length_c                   21.7232(8)
_cell_measurement_reflns_used    4160
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      28.4740
_cell_measurement_theta_min      3.2990
_cell_volume                     3825.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL-2012, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.7292
_diffrn_measurement_details
;
  1 omega  -19.00   22.60   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611  -99.0000 -180.0000 52

  2 omega   18.00   84.40   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580   57.0000 -120.0000 83

  3 omega    2.00   51.60   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580   57.0000  -30.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0515633000
_diffrn_orient_matrix_UB_12      -0.0038936000
_diffrn_orient_matrix_UB_13      0.0137060000
_diffrn_orient_matrix_UB_21      0.0242401000
_diffrn_orient_matrix_UB_22      0.0130613000
_diffrn_orient_matrix_UB_23      -0.0283091000
_diffrn_orient_matrix_UB_31      -0.0024073000
_diffrn_orient_matrix_UB_32      0.0482086000
_diffrn_orient_matrix_UB_33      0.0087776000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 1993 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0700P)^2^+0.1987P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.561
_reflns_Friedel_fraction_full    0.727
_reflns_Friedel_fraction_max     0.703
_reflns_number_gt                5983
_reflns_number_total             6784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra07524b2.cif
_cod_data_source_block           130912_s2_zz
_cod_database_code               7218378
_chemical_oxdiff_formula         c12h12n4p3cl3Ru1
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C12(H12), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29),
  C30(H30), C31(H31), C32(H32), C33(H33)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.836
_shelx_res_checksum              93652
_shelxl_version_number           2013-2