Reactivity of a metallacyclopentatriene intermediate: metal-to-ligand-to-metal re-migration of a phosphine ligand versus a 1,2 hydrogen shift
Ruba, Eva; Mereiter, Kurt; Schmid, Roland; Kirchner, Karl; Chemical Communications 19 (2001) 1996–1997; doi:10.1039/B104927P

data_7123819
_publ_section_title
;
 Reactivity of a metallacyclopentatriene intermediate:
 metal-to-ligand-to-metal re-migration of a phosphine ligand versus a 1,2
 hydrogen shift
;
_journal_name_full               'Chemical Communications'
_journal_page_first              1996
_journal_page_last               1997
_journal_paper_doi               10.1039/B104927P
_journal_volume                  19
_journal_year                    2001
_chemical_formula_moiety         '(C33 H34 P Ru)+ , (P F6)-'
_chemical_formula_sum            'C33 H34 F6 P2 Ru'
_chemical_formula_weight         707.61
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.86(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.952(5)
_cell_length_b                   15.229(7)
_cell_length_c                   10.059(6)
_cell_measurement_reflns_used    5860
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      2.4
_cell_volume                     1522.6(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, and XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'BRUKER SMART 3-circle with CCD area detector'
_diffrn_measurement_method       '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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17563
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   'semi-empirical from equivalents (SADABS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_preparation
;    
 crystallized from dichloromethane / diethylether by gas diffusion
 of diethylether at room temperature. Thin plates of red color.
;
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.60
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6607
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+1.3962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                6238
_reflns_number_total             6607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Chem-Comm-2001-19-1996.cif
_cod_data_source_block           compd3b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7123819