Template Synthesis of Ruthenium Complexes with Saturated and Benzannulated NH,NH-Stabilized N-Heterocyclic Carbene Ligands
Kaufhold, Oliver; Flores-Figueroa, Aarón; Pape, Tania; Hahn, F. Ekkehardt; Organometallics 28 (2009) 896–; doi:10.1021/om800964n

data_4068584
_publ_section_title
;
 Template Synthesis of Ruthenium Complexes with Saturated and
 Benzannulated NH,NH-Stabilized N-Heterocyclic Carbene Ligands
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              896
_journal_paper_doi               10.1021/om800964n
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C32 H37 Cl3 N2 O0.5 P Ru'
_chemical_formula_weight         696.03
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.867(4)
_cell_angle_beta                 62.535(3)
_cell_angle_gamma                72.561(4)
_cell_formula_units_Z            2
_cell_length_a                   12.202(3)
_cell_length_b                   12.792(3)
_cell_length_c                   12.965(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1
_cell_measurement_theta_min      22.5
_cell_volume                     1652.9(7)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_sigmaI/netI    0.1344
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16025
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.9844
_exptl_absorpt_correction_T_min  0.9395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.819374  

;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plates'
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.824
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                4492
_reflns_number_total             7602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800964n_si_002.cif
_cod_data_source_block           sad
_cod_original_cell_volume        1652.9(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C32 H37 Cl3 N2 O0.50 P Ru'
_cod_database_code               4068584