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_7218377
_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         'C43 H36 Cl2 N5 P Ru, C H2 Cl2'
_chemical_formula_sum            'C44 H38 Cl4 N5 P Ru'
_chemical_formula_weight         910.63
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                73.605(3)
_cell_angle_beta                 81.162(3)
_cell_angle_gamma                84.055(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2141(3)
_cell_length_b                   11.6147(4)
_cell_length_c                   17.2905(6)
_cell_measurement_reflns_used    5983
_cell_measurement_temperature    142.95(10)
_cell_measurement_theta_max      28.5440
_cell_measurement_theta_min      3.4470
_cell_volume                     1940.54(12)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      142.95(10)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.8482
_diffrn_measurement_details
;
  1 omega  -23.00   16.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611  -99.0000   60.0000 39

  2 omega  -24.00   25.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611  -99.0000 -150.0000 49

  3 omega  -93.00  -36.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611 -178.0000   60.0000 57

  4 omega  -24.00   20.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0799  -99.0000  -90.0000 44

  5 omega    7.00   91.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0799   38.0000   60.0000 84

  6 omega  -50.00   34.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0799  -57.0000  -60.0000 84

  7 omega   46.00   88.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0799   57.0000   90.0000 42

  8 omega  -39.00  -14.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611   57.0000   60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0361838000
_diffrn_orient_matrix_UB_12      -0.0486210000
_diffrn_orient_matrix_UB_13      0.0255765000
_diffrn_orient_matrix_UB_21      0.0286972000
_diffrn_orient_matrix_UB_22      -0.0368872000
_diffrn_orient_matrix_UB_23      -0.0254062000
_diffrn_orient_matrix_UB_31      0.0531612000
_diffrn_orient_matrix_UB_32      -0.0185486000
_diffrn_orient_matrix_UB_33      0.0236748000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15862
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88770
_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    1.558
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.967
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0679P)^2^+1.4507P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6263
_reflns_number_total             7931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra07524b2.cif
_cod_data_source_block           130924_s3_zz
_cod_original_cell_volume        1940.55(11)
_cod_database_code               7218377
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C12H12N3P2Cl2Ru1
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.815
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C10(H10), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              16579