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_4071973
_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         'C50 H60 Cl N6 P2 Ru, C24 H20 B, C4 H8 O '
_chemical_formula_sum            'C78 H88 B Cl N6 O P2 Ru'
_chemical_formula_weight         1334.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.9600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9209(4)
_cell_length_b                   13.9488(3)
_cell_length_c                   25.4091(6)
_cell_measurement_reflns_used    9099
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.43
_cell_volume                     7051.1(3)
_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      250(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            60170
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.9325
_exptl_absorpt_correction_T_min  0.8204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         15371
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                10382
_reflns_number_total             15371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800494c_si_003.cif
_cod_data_source_block           sd00204
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4071973