Stable Carbene and Diazoalkane Complexes of the Same Complex System. Synthesis, Structure, and Reactivity of PNP−Ru(II) Fluorenylidene and Diazofluorene Complexes
Zhang, Jing; Gandelman, Mark; Shimon, Linda J. W.; Milstein, David; Organometallics 27 (2008) 3526–; doi:10.1021/om800294v

data_4071654
_publ_section_title
;
 Stable Carbene and Diazoalkane Complexes of the Same Complex System.
 Synthesis, Structure, and Reactivity of PNP&#x2212;Ru(II) Fluorenylidene
 and Diazofluorene Complexes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3526
_journal_paper_doi               10.1021/om800294v
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C36 H51 Cl2 N3 P2 Ru'
_chemical_formula_sum            'C36 H51 Cl2 N3 P2 Ru'
_chemical_formula_weight         759.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.0783(3)
_cell_length_b                   14.7973(3)
_cell_length_c                   27.1111(6)
_cell_measurement_reflns_used    9105
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_cell_volume                     7252.5(2)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38740
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.8181
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0722P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                5868
_reflns_number_total             8326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800294v-file001.cif
_cod_data_source_block           m406a
_cod_original_cell_volume        7252.2(2)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4071654