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_4113501
_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            'C40.5 H59 Cl2 N2 O P Ru'
_chemical_formula_weight         792.84
_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   'Calculated geometric positions'
_atom_sites_solution_primary     'Patterson method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.336(2)
_cell_angle_beta                 103.4280(10)
_cell_angle_gamma                91.8140(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2758(9)
_cell_length_b                   13.0394(11)
_cell_length_c                   14.7233(13)
_cell_measurement_reflns_used    14812
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.27
_cell_volume                     1915.5(3)
_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 0.909
_diffrn_measured_fraction_theta_max 0.909
_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  0.0917
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28236
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.9600
_exptl_absorpt_correction_T_min  0.8550
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       Tabular
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.008
_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          0.0807
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                7057
_reflns_number_total             8728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja021146w_s1_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' 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_formula_sum        'C40.50 H59 Cl2 N2 O P Ru'
_cod_database_code               4113501