Formation of Metallacyclobutene Complexes via the Addition of Hydrazines to Ruthenium Vinylidene Complexes
Dabb, Serin L.; Messerle, Barbara A.; Wagler, Jörg; Organometallics 27 (2008) 4657–; doi:10.1021/om800494c

data_4071972
_publ_section_title
;
 Formation of Metallacyclobutene Complexes via the Addition of Hydrazines
 to Ruthenium Vinylidene Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4657
_journal_paper_doi               10.1021/om800494c
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C52 H56 Cl N6 P2 Ru, C24 H20 B, C H2 Cl2'
_chemical_formula_sum            'C77 H78 B Cl3 N6 P2 Ru'
_chemical_formula_weight         1367.62
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.1110(10)
_cell_angle_beta                 100.3990(10)
_cell_angle_gamma                91.9250(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4426(2)
_cell_length_b                   13.8014(2)
_cell_length_c                   20.2734(3)
_cell_measurement_reflns_used    121749
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.631
_cell_measurement_theta_min      2.546
_cell_volume                     3392.35(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Collect, KappaCCD'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            102318
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         29739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+1.0242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                25162
_reflns_number_total             29739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800494c_si_002.cif
_cod_data_source_block           sd00101
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4071972