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_4113502
_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            'C49 H56 Cl2 N4 Ru'
_chemical_formula_weight         872.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'Patterson method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.523(5)
_cell_angle_beta                 95.698(4)
_cell_angle_gamma                90.666(5)
_cell_formula_units_Z            4
_cell_length_a                   11.663(3)
_cell_length_b                   14.676(4)
_cell_length_c                   25.176(7)
_cell_measurement_reflns_used    18648
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.21
_cell_volume                     4274(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT v6.2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans at 8 f settings'
_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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.1023
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            101139
_diffrn_reflns_theta_full        28.62
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    Unrestrained
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     1457
_refine_ls_number_reflns         20088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_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          0.0629
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                12521
_reflns_number_total             20088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja021146w_s1_3.cif
_cod_data_source_block           6a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        4273.5(19)
_cod_database_code               4113502