Preparation and Characterization of Ruthenium(II) Monophosphaferrocene Complexes. Reactivity, Dynamic Solution Behavior, and X-ray Structure of [RuH2(η2-H2)(PCy3)2(2-phenyl-3,4-dimethylphosphaferrocene)]
Andrew J. Toner; Bruno Donnadieu; Sylviane Sabo-Etienne; Bruno Chaudret; Xavier Sava; François Mathey; Pascal Le Floch; Inorganic Chemistry 40 (2001) 3034–3038; doi:10.1021/ic001404v

data_4319862
_publ_contact_author             ' Sylviane Sabo-Etienne '
_publ_section_title
;
 Preparation and Characterization of Ruthenium(II) Monophosphaferrocene
 Complexes. Reactivity, Dynamic Solution Behavior, and X-ray Structure of
 [RuH2(\h2-H2)(PCy3)2(2-phenyl-3,4-dimethylphosphaferrocene)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3034
_journal_page_last               3038
_journal_paper_doi               10.1021/ic001404v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C57 H95.5 Fe P3 Ru'
_chemical_formula_weight         1030.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.636(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2591(14)
_cell_length_b                   13.7902(13)
_cell_length_c                   34.848(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    140(2)
_cell_volume                     5872.0(11)
_computing_cell_refinement
;
Stoe and Cie (1996) IPDS Manual. Version 2.75
 Stoe and Cie, Darmstadt, Germany
;
_computing_data_collection
;
Stoe and Cie (1996) IPDS Manual. Version 2.75
Stoe and Cie, Darmstadt, Germany
;
_computing_data_reduction
;
Stoe and Cie (1996) IPDS Manual. Version 2.75
Stoe and Cie, Darmstadt, Germany
;
_computing_molecular_graphics
;
Zsolnai,L.(1997). ZORTEP.Molecular Graphics 
Program.University of Heidelberg, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
Altomare, A., Cascarano, G., Giacovazzo G., 
Guagliardi A., Burla M.C., Polidori, G.  & Camalli, M. (1994) SIR92 - a 
program for automatic solution of crystal structures by direct methods.
J. Appl. Cryst. (27), 435
;
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean '2.9 - 48.4'
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type
;
Stoe and Cie (1996) IPDS Manual. Version 2.75. 
Stoe and Cie, Darmstadt, Germany
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\?
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            36440
_diffrn_reflns_theta_full        24.21
_diffrn_reflns_theta_max         24.21
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   Numericals
_exptl_absorpt_process_details
;
Facies of crystal was determined by 
indexation of faces of crystal, theses numericals corrections have been 
optimized by using a set of symmetry equivalent reflections selected with the 
criterion [I>3((I)] such that all directions of the reciprocal space are 
equally represented.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2210
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         8961
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+2.5201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                6899
_reflns_number_total             8961
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic001404v.cif
_cod_data_source_block           C57H95.50FeP3Ru
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_original_formula_sum        'C57 H95.50 Fe P3 Ru'
_cod_database_code               4319862
_cell_measurement_2theta_min     3.7
_cell_measurement_2theta_max     48.3