Synthesis and Activity of Ruthenium Alkylidene Complexes Coordinated with Phosphine and N-Heterocyclic Carbene Ligands
Tina M. Trnka; John P. Morgan; Melanie S. Sanford; Thomas E. Wilhelm; Matthias Scholl; Tae-Lim Choi; Sheng Ding; Michael W. Day; Robert H. Grubbs; Journal of the American Chemical Society 125 (2003) 2546–2558; doi:10.1021/ja021146w

data_4113500
_publ_contact_author
;       Lawrence M. Henling
        Beckman Institute
        California Institute of Technology
        Pasadena, CA  91125
        USA
;
_publ_contact_author_email       xray@caltech.edu
_publ_contact_author_fax         '(626) 449 4159'
_publ_contact_author_phone       '(626) 395 2735'
_publ_section_title
;
 Synthesis and Activity of Ruthenium Alkylidene Complexes Coordinated with
 Phosphine and N-Heterocyclic Carbene Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2546
_journal_page_last               2558
_journal_paper_doi               10.1021/ja021146w
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C37 H67 Cl O P2 Ru'
_chemical_formula_weight         726.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.171(1)
_cell_angle_beta                 108.499(1)
_cell_angle_gamma                91.328(1)
_cell_formula_units_Z            1
_cell_length_a                   9.8362(7)
_cell_length_b                   10.2260(7)
_cell_length_c                   10.8212(8)
_cell_measurement_reflns_used    7348
_cell_measurement_temperature    98
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.2
_cell_volume                     926.85(11)
_computing_cell_refinement       'Bruker SMART v5.606'
_computing_data_collection       'Bruker SMART v5.606'
_computing_data_reduction        'Bruker SAINT v6.02'
_computing_molecular_graphics    'Diamond, Bruker SHELXTL v5.1'
_computing_publication_material  'Bruker SHELXTL v5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker SMART 1000 ccd'
_diffrn_measurement_method       '\w scans at 5 fixed \f values'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13967
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        'within counting statistics'
_diffrn_standards_interval_time  'first 75 scans recollected at end of runs'
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'orange-tinged deep-yellow'
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       'flat wedge'
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.523
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.523
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/\s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                3843
_reflns_number_total             4294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja021146w_s1_1.cif
_cod_data_source_block           3b
_cod_database_code               4113500