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_4060753
_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~)Cl(\m^2^-HCC(OH)Ph~2~)(P^i^Pr~3~)
;
_chemical_formula_sum            'C29 H38 Cl O Os P'
_chemical_formula_weight         659.21
_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                   13.924(2)
_cell_length_b                   17.670(2)
_cell_length_c                   22.157(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     5451.4(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9377
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.854
_exptl_absorpt_correction_T_max  0.488
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00008(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                3266
_reflns_number_total             4798
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4060753