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_4071974
_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
'C45 H58 Cl N6 P2 Ru,  C24 H20 B, 3.5(C4 H8 O) '
_chemical_formula_sum            'C83 H106 B Cl N6 O3.5 P2 Ru'
_chemical_formula_weight         1453.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.834(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.5138(9)
_cell_length_b                   19.7724(6)
_cell_length_c                   26.3039(6)
_cell_measurement_reflns_used    5754
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      2.32
_cell_volume                     15270.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 (Farugia)'
_computing_publication_material  'Shelx-97/ciftab(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            64105
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.8301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             6160
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         16636
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+5.8314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                11827
_reflns_number_total             16636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800494c_si_004.cif
_cod_data_source_block           sd00301
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C83 H106 B Cl N6 O3.50 P2 Ru'
_cod_database_code               4071974