Ruthenium Carbene, Vinylidene, and Allenylidene Complexes with a Bis(3,5-dimethylpyrazol-1-yl)acetato Heteroscorpionate Ligand
Kopf, Henning; Pietraszuk, Cezary; Hübner, Eike; Burzlaff, Nicolai; Organometallics 25 (2006) 2533–; doi:10.1021/om060050y

data_4075102
_publ_section_title
;
 Ruthenium Carbene, Vinylidene, and Allenylidene Complexes with a
 Bis(3,5-dimethylpyrazol-1-yl)acetato Heteroscorpionate Ligand
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2533
_journal_paper_doi               10.1021/om060050y
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C31 H30 Cl N4 O3 P Ru, C H2 Cl2'
_chemical_formula_sum            'C32 H32 Cl3 N4 O3 P Ru'
_chemical_formula_weight         759.01
_chemical_name_systematic
;
 Bis(3,5-dimethylpyrazol-1-yl)acetato-chloro-
carbonyl-triphenylphosphine-ruthenium(ii) 
;
_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                82.190(14)
_cell_angle_beta                 71.12(3)
_cell_angle_gamma                78.79(2)
_cell_formula_units_Z            2
_cell_length_a                   10.059(5)
_cell_length_b                   11.478(4)
_cell_length_c                   15.463(4)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      14.037
_cell_measurement_theta_min      11.304
_cell_volume                     1651.9(11)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6203
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        -1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.983
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0602P)^2^+6.0853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                5127
_reflns_number_total             5805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060050ysi20060118_063303.cif
_cod_data_source_block           hkbue1
_cod_original_cell_volume        1652.0(11)
_cod_database_code               4075102