Decomposition of Olefin Metathesis Catalysts by Brønsted Base: Metallacyclobutane Deprotonation as a Primary Deactivating Event.
Bailey, Gwendolyn A.; Lummiss, Justin A. M.; Foscato, Marco; Occhipinti, Giovanni; McDonald, Robert; Jensen, Vidar R.; Fogg, Deryn E.; Journal of the American Chemical Society 139 (2017) 16446–16449; doi:10.1021/jacs.7b08578

data_4131678
_publ_section_title
;
 Decomposition of Olefin Metathesis Catalysts by Br\/onsted Base:
 Metallacyclobutane Deprotonation as a Primary Deactivating Event.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16446
_journal_page_last               16449
_journal_paper_doi               10.1021/jacs.7b08578
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C58 H66 Cl2 N4 Ru2, 2.5(C6 H6)'
_chemical_formula_sum            'C73 H81 Cl2 N4 Ru2'
_chemical_formula_weight         1287.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   11.4339(3)
_cell_length_b                   40.0510(11)
_cell_length_c                   54.661(2)
_cell_measurement_reflns_used    9396
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.26
_cell_measurement_theta_min      2.74
_cell_volume                     25031.4(13)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.273
_diffrn_reflns_theta_min         2.735
_exptl_absorpt_coefficient_mu    5.036
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.5719
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             10704
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0632P)^2^+406.1523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.1877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5031
_reflns_number_total             5972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08578_si_003.cif
_cod_data_source_block           ott1312
_cod_original_cell_volume        25031.3(13)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4131678
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.275
_shelx_estimated_absorpt_t_max   0.654
_shelx_res_checksum              75504
_shelx_hkl_checksum              66452
_shelx_fab_checksum              52652