Two- and Four-Electron Alkyne Ligands in Osmium-Cyclopentadienyl Chemistry: Consequences of the π⊥→M Interaction
Jorge J. Carbó; Pascale Crochet; Miguel A. Esteruelas; Yves Jean; Agustí Lledós; Ana M. López; Enrique Oñate; Organometallics 21 (2002) 305–314; doi:10.1021/om010645n

data_4060754
_publ_section_title
;
 Two- and Four-Electron Alkyne Ligands in Osmium-Cyclopentadienyl
 Chemistry: Consequences of the \p&#x22A5;\\rightarrow M Interaction
;
_journal_name_full               Organometallics
_journal_page_first              305
_journal_page_last               314
_journal_paper_doi               10.1021/om010645n
_journal_volume                  21
_journal_year                    2002
_chemical_formula_structural
;
[Os(\h^5^C~5~H~5~)(\m^2^-HCC(OH)Ph~2~)(P^i^Pr~3~)]PF~6~
;
_chemical_formula_sum            'C29 H38 F6 O Os P2'
_chemical_formula_weight         768.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   16.842(2)
_cell_length_b                   9.0770(10)
_cell_length_c                   19.643(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     3002.9(6)
_computing_cell_refinement       'xscans (Bruker-Siemens)'
_computing_data_collection       'xscans (Bruker-Siemens)'
_computing_data_reduction        'xscans (Bruker-Siemens)'
_computing_molecular_graphics    'xp, shelxtl v. 4.2 (Bruker-Siemens)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295.0(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Siemens P4'
_diffrn_measurement_method       '\w\2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7844
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.412
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.426(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5282
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.318
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+5.0382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                4447
_reflns_number_total             5282
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4060754