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_1540419
_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_absolute_configuration ad
_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      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-07-23 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1500(4)
_cell_length_b                   14.3631(3)
_cell_length_c                   24.5735(4)
_cell_measurement_reflns_used    3273
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.0080
_cell_measurement_theta_min      3.5540
_cell_volume                     4994.27(19)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.9855
_diffrn_measured_fraction_theta_max 0.9855
_diffrn_measurement_details
;
  1 omega   13.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798   65.0000  -89.0000 25

  2 omega  115.00  165.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   81.0000  -82.0000 50

  3 omega   49.00  132.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -75.0000 -140.0000 83

  4 omega  -95.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  125.0000 -120.0000 82

  5 omega -115.00  -82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000    0.0000 33

  6 omega -125.00  -80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000  -60.0000 45

  7 omega   34.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -120.0000 57

  8 omega   36.00   81.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000   30.0000 45

  9 omega   37.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000  120.0000 58
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0756682000
_diffrn_orient_matrix_UB_12      -0.0201684000
_diffrn_orient_matrix_UB_13      0.0435922000
_diffrn_orient_matrix_UB_21      0.0557317000
_diffrn_orient_matrix_UB_22      0.0866260000
_diffrn_orient_matrix_UB_23      -0.0184126000
_diffrn_orient_matrix_UB_31      -0.0550613000
_diffrn_orient_matrix_UB_32      0.0598249000
_diffrn_orient_matrix_UB_33      0.0411316000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.1221
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13803
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         68.00
_diffrn_reflns_theta_min         3.60
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.108
_exptl_absorpt_correction_T_max  0.360
_exptl_absorpt_correction_T_min  0.193
_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    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.2884
_exptl_crystal_size_mid          0.2005
_exptl_crystal_size_min          0.1737
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                6149
_reflns_number_total             8245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cy01506e2.cif
_cod_data_source_block           fv043
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1540417--1540419.cif.
;
_cod_database_code               1540419
_chemical_oxdiff_formula         'C56 H73 N2 P1 Cl2 Ru1'
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.11
_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:
 C51(H51), C39(H39), C45(H45)
2.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C52(H52A,H52B), C53(H53A,H53B), C43(H43A,H43B), C46(H46A,
 H46B), C44(H44A,H44B), C20(H20A,H20B), C50(H50A,H50B), C41(H41A,H41B),
 C54(H54A,H54B), C19(H19A,H19B), C49(H49A,H49B), C40(H40A,H40B), C47(H47A,H47B),
  C55(H55A,H55B), C48(H48A,H48B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C34(H34), C6(H6), C7(H7), C23(H23), C8(H8), C2(H2), C25(H25),
 C13(H13), C14(H14), C16(H16), C15(H15)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C10(H10A,H10B,H10C), C37(H37A,H37B,H37C), C36(H36A,H36B,
 H36C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C38(H38A,
 H38B,H38C)
;