Specialized Ruthenium Olefin Metathesis Catalysts Bearing Bulky Unsymmetrical NHC Ligands: Computations, Synthesis, and Application
Małecki, Paweł; Gajda, Katarzyna; Gajda, Roman; Woźniak, Krzysztof; Trzaskowski, Bartosz; Kajetanowicz, Anna; Grela, Karol; ACS Catalysis 9 (2018) 587–; doi:10.1021/acscatal.8b04783

data_4515480
_publ_section_title
;
 Specialized Ruthenium Olefin Metathesis Catalysts Bearing Bulky
 Unsymmetrical NHC Ligands: Computations, Synthesis, and Application
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              587
_journal_paper_doi               10.1021/acscatal.8b04783
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C36 H48 Cl2 N2 O Ru'
_chemical_formula_sum            'C36 H48 Cl2 N2 O Ru'
_chemical_formula_weight         696.73
_chemical_name_systematic
;
[N1-(2,6-Bis-(3-pentyl)phenyl)-N2-benzyl)-2-imidazolidinylidene]
(2-isopropoxyphenylmethylene)ruthenium(II) chloride
;
_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   difmap
_audit_creation_date             2017-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7369(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3364(2)
_cell_length_b                   10.43031(12)
_cell_length_c                   16.58648(19)
_cell_measurement_reflns_used    64920
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      53.8830
_cell_measurement_theta_min      2.1800
_cell_volume                     3328.48(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector_area_resol_mean 5.2195
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -12.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1610   57.0000 -150.0000 134

  2 omega   35.00  131.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1610  178.0000 -150.0000 96

  3 omega  -12.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1610   57.0000  -30.0000 134

  4 omega  -12.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1610   57.0000  120.0000 134

  5 omega  -61.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1610  -38.0000  150.0000 132

  6 omega  -16.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1610   89.0000   16.2879 28

  7 omega -131.00  -55.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0360  178.0000 -150.0000 76

  8 omega -132.00   11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0360  -77.0000  120.0000 143

  9 omega -132.00   11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0360  -77.0000  -30.0000 143

 10 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000  -90.0000 124

 11 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000   60.0000 124

 12 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000  -30.0000 124

 13 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000   90.0000 124

 14 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000    0.0000 124

 15 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000  -60.0000 124

 16 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000 -120.0000 124

 17 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000   30.0000 124

 18 omega   34.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000  120.0000 124

 19 omega   34.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000  150.0000 26

 20 omega   34.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000 -180.0000 27

 21 omega   74.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000 -180.0000 84

 22 omega   34.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000 -150.0000 26

 23 omega   75.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000 -150.0000 83

 24 omega   75.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       77.6323   77.0000  150.0000 83

 25 omega -123.00  -45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -79.5073   77.0000  120.0000 78

 26 omega -162.00 -111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -79.5073 -111.0000   60.0000 51

 27 omega -119.00   -4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -79.5073   77.0000  -30.0000 115

 28 omega -144.00  -95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -79.5073  178.0000 -120.0000 49

 29 omega -157.00  -55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -79.5073  178.0000   30.0000 102
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0220271000
_diffrn_orient_matrix_UB_12      -0.0542799000
_diffrn_orient_matrix_UB_13      0.0008053000
_diffrn_orient_matrix_UB_21      0.0005683000
_diffrn_orient_matrix_UB_22      0.0058995000
_diffrn_orient_matrix_UB_23      0.0426582000
_diffrn_orient_matrix_UB_31      -0.0295459000
_diffrn_orient_matrix_UB_32      0.0405810000
_diffrn_orient_matrix_UB_33      -0.0051455000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            205909
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.035
_diffrn_reflns_theta_min         2.117
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       needle
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.3849
_exptl_crystal_size_mid          0.1575
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         16967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0214P)^2^+1.7749P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14828
_reflns_number_total             16967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Ru_9.cif
_cod_data_source_block           Ru_9
_cod_database_code               4515480
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C36H47N2O1Cl2Ru1
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.95
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'