Kinetic and Thermodynamic Analysis of Processes Relevant to Initiation of Olefin Metathesis by Ruthenium Phosphonium Alkylidene Catalysts
Erin M. Leitao; Edwin F. van der Eide; Patricio E. Romero; Warren, E. Piers; Robert McDonald; Journal of the American Chemical Society 132 (2010) 2784–2794; doi:10.1021/ja910112m

data_4101973
_publ_section_title
;
 Kinetic and Thermodynamic Analysis of Processes Relevant to Initiation of
 Olefin Metathesis by Ruthenium Phosphonium Alkylidene Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2784
_journal_page_last               2794
_journal_paper_doi               10.1021/ja910112m
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C35 H52 Cl3 N2 P Ru, 3(C H Cl3)'
_chemical_formula_sum            'C38 H55 Cl12 N2 P Ru'
_chemical_formula_weight         1097.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.471(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2155(18)
_cell_length_b                   21.905(3)
_cell_length_c                   16.828(2)
_cell_measurement_reflns_used    4936
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.77
_cell_measurement_theta_min      2.38
_cell_volume                     5050.2(11)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38988
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.5232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
 Attempts to refine peaks of residual electron density as solvent chloroform
 chlorine or carbon atoms were unsuccessful.  The data were corrected for
 disordered electron density through use of the SQUEEZE procedure (Sluis,
 P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as
 implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34.
 PLATON - a multipurpose crystallographic tool.  Utrecht University, Utrecht,
 The Netherlands).  A total solvent-accessible void volume of 1322.7
 A^3^ (distributed equally between locations at the crystallographic
 inversion center (0, 1/2, 0) and at (-0.17, 0, 0.33)) with a total electron
 count of 469 (consistent with eight molecules of solvent chloroform, or two
 molecules per formula unit of the ruthenium complex molecule, in addition to
 the one CHCl~3~ molecule that was located and refined) was found in the unit
 cell.
;
_refine_diff_density_max         1.562
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         10339
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0878P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                7692
_reflns_number_total             10339
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja910112m_si_003.cif
_cod_data_source_block           cal0703
_cod_original_cell_volume        5050.3(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4101973