Half-Sandwich Ruthenium Complexes with Schiff-Base Ligands: Syntheses, Characterization, and Catalytic Activities for the Reduction of Nitroarenes
Jia, Wei-Guo; Zhang, Hui; Zhang, Tai; Xie, Dong; Ling, Shuo; Sheng, En-Hong; Organometallics 35 (2016) 503–; doi:10.1021/acs.organomet.5b00933

data_4088210
_publ_section_title
;
 Half-Sandwich Ruthenium Complexes with Schiff-Base Ligands: Syntheses,
 Characterization, and Catalytic Activities for the Reduction of
 Nitroarenes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              503
_journal_paper_doi               10.1021/acs.organomet.5b00933
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C22 H22 Cl2 N2 O Ru'
_chemical_formula_sum            'C22 H22 Cl2 N2 O Ru'
_chemical_formula_weight         502.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8993(7)
_cell_length_b                   15.3472(8)
_cell_length_c                   20.0927(11)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      1.98
_cell_volume                     4286.1(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_min         1.977
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 3676 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         9733
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.4564P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                8397
_reflns_number_total             9733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00933_si_002.cif
_cod_data_source_block           ygz
_cod_database_code               4088210
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.818
_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 Ternary CH refined with riding coordinates:
 C20(H20), C42(H42)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C31(H31), C18(H18), C16(H16), C15(H15), C9(H9), C10(H10), C11(H11),
 C12(H12), C7(H7), C5(H5), C3(H3), C2(H2), C41(H41), C40(H40), C38(H38),
 C37(H37), C25(H25), C24(H24), C27(H27), C29(H29), C34(H34), C33(H33), C32(H32)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C35(H35A,H35B,
 H35C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C)
;
_olex2_submission_special_instructions 'No special instructions were received'