Ruthenium complexes with an N-heterocyclic carbene NNC-pincer ligand: preparation and catalytic properties
Mejuto, Carmen; García-Eleno, Marco A.; Guisado-Barrios, Gregorio; Spasyuk, Denis; Gusev, Dmitri; Peris, Eduardo; Organic Chemistry Frontiers 2 (2015) 936–; doi:10.1039/C5QO00137D

data_1553144
_publ_section_title
;
 Ruthenium complexes with an N-heterocyclic carbene NNC-pincer ligand:
 preparation and catalytic properties
;
_journal_issue                   8
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              936
_journal_paper_doi               10.1039/C5QO00137D
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C31 H29 N4 O3 P Ru, 2(H2 O), C H2 Cl2'
_chemical_formula_sum            'C32 H35 Cl2 N4 O5 P Ru'
_chemical_formula_weight         758.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-22 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.3893(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2792(3)
_cell_length_b                   11.74106(11)
_cell_length_c                   17.1049(2)
_cell_measurement_reflns_used    14665
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      69.5530
_cell_measurement_theta_min      4.6190
_cell_volume                     3259.49(9)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector_area_resol_mean 20.8101
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega -113.00  -87.80   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307 -139.0000  154.0000 36

  2 omega -116.00  -79.60   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307 -130.0000  -30.0000 52

  3 omega -129.00  -35.90   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  178.0000   60.0000 133

  4 omega   13.00   40.30   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307   38.0000   30.0000 39

  5 omega  -19.00   46.10   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307   19.0000  -90.0000 93

  6 omega  140.00  167.30   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  111.0000   60.0000 39

  7 omega  100.00  127.30   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  111.0000   60.0000 39

  8 omega   75.00  177.20   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686   45.0000  150.0000 146

  9 omega  101.00  126.90   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  111.0000 -150.0000 37

 10 omega   21.00   57.40   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  -30.0000  -90.0000 52

 11 omega   22.00  107.40   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  -77.0000   30.0000 122

 12 omega   23.00   51.00   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  -30.0000 -120.0000 40

 13 omega   21.00   90.30   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  -30.0000 -180.0000 99

 14 omega   59.00   84.90   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686  178.0000  -30.0000 37

 15 omega -122.00   -3.00   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -77.0000  150.0000 170

 16 omega -116.00   -6.10   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -56.0000   25.0000 157

 17 omega -116.00   -6.10   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -57.0000  -90.0000 157

 18 omega   55.00  127.80   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       37.7307 -178.0000  120.0000 104

 19 omega   71.00  176.70   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686   45.0000 -120.0000 151

 20 omega   66.00  178.00   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686   77.0000    0.0000 160

 21 omega   66.00  178.00   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686   77.0000  -60.0000 160

 22 omega   20.00  114.50   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686 -111.0000 -180.0000 135

 23 omega   66.00  168.20   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686   77.0000 -180.0000 146

 24 omega   71.00  176.70   0.7000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8686   45.0000   90.0000 151
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0945647000
_diffrn_orient_matrix_UB_12      0.0101836000
_diffrn_orient_matrix_UB_13      0.0499228000
_diffrn_orient_matrix_UB_21      0.0075937000
_diffrn_orient_matrix_UB_22      -0.0872613000
_diffrn_orient_matrix_UB_23      -0.0631341000
_diffrn_orient_matrix_UB_31      -0.0030841000
_diffrn_orient_matrix_UB_32      0.0974006000
_diffrn_orient_matrix_UB_33      -0.0618011000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27673
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.660
_diffrn_reflns_theta_min         4.648
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70936
_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    1.546
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.2109
_exptl_crystal_size_mid          0.0957
_exptl_crystal_size_min          0.0355
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0457P)^2^+4.5626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5441
_reflns_number_total             6075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00137d2.cif
_cod_data_source_block           str1610
_cod_database_code               1553144
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C31 H31 Cl2 N4 P Ru'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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, All O(H,H) groups
2.a Free rotating group:
 O5(H5C,H5D), O4(H4A,H4B)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C28(H28), C15(H15), C34(H34), C13(H13), C33(H33), C32(H32),
 C22(H22), C14(H14), C30(H30), C18(H18), C16(H16), C27(H27), C20(H20), C21(H21),
  C19(H19), C31(H31), C24(H24), C26(H26), C3(H3), C25(H25), C4(H4)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'