Loss and Reformation of Ruthenium Alkylidene: Connecting Olefin Metathesis, Catalyst Deactivation, Regeneration, and Isomerization.
Engel, Julien; Smit, Wietse; Foscato, Marco; Occhipinti, Giovanni; Törnroos, Karl W; Jensen, Vidar R.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07694

data_4126707
_publ_section_title
;
 Loss and Reformation of Ruthenium Alkylidene: Connecting Olefin
 Metathesis, Catalyst Deactivation, Regeneration, and Isomerization.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07694
_journal_year                    2017
_chemical_formula_moiety         'C31 H40 Cl2 N2 Ru'
_chemical_formula_sum            'C31 H40 Cl2 N2 Ru'
_chemical_formula_weight         612.62
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 103.145(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.76752(16)
_cell_length_b                   24.8251(4)
_cell_length_c                   13.7094(3)
_cell_measurement_reflns_used    6870
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.1900
_cell_measurement_theta_min      2.4810
_cell_volume                     2905.73(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  PILATUS2M
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_type           'synchrotron, Si(111)'
_diffrn_radiation_wavelength     0.6999
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16821
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         24.620
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'synchrotron, BM1A, SNBL, ESRF'
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       'thin lath'
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.100
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0946P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3968
_reflns_number_total             4808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07694_si_002.cif
_cod_data_source_block           Complex5
_cod_original_cell_volume        2905.72(10)
_cod_database_code               4126707
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              2897
_shelx_hkl_checksum              13951