Effect of the bulkiness of indenylidene moieties on the catalytic initiation and efficiency of second-generation ruthenium-based olefin metathesis catalysts
Yu, Baoyi; Luo, Zhixiong; Hamad, Fatma B.; Leus, Karen; van Hecke, Kristof; Verpoort, Francis; Catal. Sci. Technol. 6 (2016) 2092–; doi:10.1039/C5CY01506E

data_1540417
_publ_section_title
;
 Effect of the bulkiness of indenylidene moieties on the catalytic
 initiation and efficiency of second-generation ruthenium-based olefin
 metathesis catalysts
;
_journal_issue                   7
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              2092
_journal_paper_doi               10.1039/C5CY01506E
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C56 H73 Cl2 N2 P Ru'
_chemical_formula_sum            'C56 H73 Cl2 N2 P Ru'
_chemical_formula_weight         977.10
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-02
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_audit_update_record
;
2015-01-14 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.821(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7833(3)
_cell_length_b                   32.7044(10)
_cell_length_c                   13.6983(4)
_cell_measurement_reflns_used    4454
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.7090
_cell_measurement_theta_min      4.2290
_cell_volume                     4900.6(3)
_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
;
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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.9862
_diffrn_measured_fraction_theta_max 0.9862
_diffrn_measurement_details
;
  1 omega  -84.00  -49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798 -161.0000   76.0000 35

  2 omega  -67.00    5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  117.0000  -45.0000 72

  3 omega   19.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -117.0000 -132.0000 74

  4 omega  -68.00  -43.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  117.0000  -45.0000 25

  5 omega -109.00  -84.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000 -161.0000   76.0000 25

  6 omega   89.00  140.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -161.0000   76.0000 51

  7 omega   70.00  118.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  161.0000  105.0000 48

  8 omega   46.00  117.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -117.0000 -132.0000 71

  9 omega  114.00  139.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  117.0000  -45.0000 25

 10 omega  -55.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   45.0000  120.0000 85

 11 omega -126.00  -80.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000  -90.0000 46

 12 omega   33.00   91.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000   30.0000 58

 13 omega   33.00   88.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000   90.0000 55

 14 omega   37.00  138.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -61.0000 -150.0000 101

 15 omega   37.00   91.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000  -30.0000 54
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1288598000
_diffrn_orient_matrix_UB_12      0.0005713000
_diffrn_orient_matrix_UB_13      0.0864737000
_diffrn_orient_matrix_UB_21      -0.0064708000
_diffrn_orient_matrix_UB_22      -0.0466255000
_diffrn_orient_matrix_UB_23      0.0131577000
_diffrn_orient_matrix_UB_31      0.0563276000
_diffrn_orient_matrix_UB_32      -0.0066785000
_diffrn_orient_matrix_UB_33      -0.0838522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.1376
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23338
_diffrn_reflns_theta_full        71.49
_diffrn_reflns_theta_max         71.49
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.186
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.297
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.1805
_exptl_crystal_size_mid          0.1219
_exptl_crystal_size_min          0.1072
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                5667
_reflns_number_total             9380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cy01506e2.cif
_cod_data_source_block           fv045
_cod_depositor_comments
'Adding full bibliography for 1540417--1540419.cif.'
_cod_database_code               1540417
_chemical_oxdiff_formula         'C56 H73 N2 Cl2 P1 Ru1'
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 Ternary CH refined with riding coordinates:
 C39(H39), C45(H45), C51(H51)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C23(H23), C25(H25), C32(H32), C34(H34)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C)
;