X-Ray structure and theoretical studies of RuH2(η2-H2)(η2-H-SiPh3)(PCy3)2, a complex with two different η2-coordinated σ bonds
Hussein, Khansaa; Marsden, Colin J.; Barthelat, Jean-Claude; Rodriguez, Venancio; Conejero, Salvador; Sabo-Etienne, Sylviane; Donnadieu, Bruno; Chaudret, Bruno; Chemical Communications  (1999) 1315–; doi:10.1039/a901558b

data_7110506
_publ_section_title
;
 X-Ray structure and theoretical studies of
 RuH2(\h2-H2)(\h2-H-SiPh3)(PCy3)2, a complex with two different
 \h2-coordinated \s bonds
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1315
_journal_paper_doi               10.1039/a901558b
_journal_year                    1999
_chemical_formula_sum            'C58 H91 O P2 Ru Si'
_chemical_formula_weight         995.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.763(14)
_cell_angle_beta                 103.677(14)
_cell_angle_gamma                98.202(15)
_cell_formula_units_Z            4
_cell_length_a                   12.7694(16)
_cell_length_b                   20.991(3)
_cell_length_c                   21.691(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_volume                     5550.1(13)
_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      160(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type
;
Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, 
Darmstadt, Germany
;
_diffrn_measurement_method       ' rotation'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1758
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14181
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         1.79
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'yellow pale'
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.671
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         14181
_refine_ls_number_restraints     447
_refine_ls_restrained_S_all      0.668
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.421
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                6804
_reflns_number_total             14181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            901558bsup1.cif
_cod_data_source_block           1
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5550.0(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110506
_cell_measurement_2theta_min     3.6
_cell_measurement_2theta_max     48.3