Generation of Functionally Substituted Cyclopentadienyl Ligands in Osmium(IV) Chemistry
Miguel Baya; Pascale Crochet; Miguel A. Esteruelas; Enrique Oñate; Organometallics 20 (2001) 240–253; doi:10.1021/om000789m

data_4063191
_publ_section_title
;
 Generation of Functionally Substituted Cyclopentadienyl Ligands in
 Osmium(IV) Chemistry
;
_journal_name_full               Organometallics
_journal_page_first              240
_journal_page_last               253
_journal_paper_doi               10.1021/om000789m
_journal_volume                  20
_journal_year                    2001
_chemical_formula_structural
;
OsH=972=97{(\h^5^-C=975=97H=974=97)Si(C=976=97H=974=97)Ph=972=97}(P^i^Pr=973=
=97)
;
_chemical_formula_sum            'C32 H41 Os P Si'
_chemical_formula_weight         674.91
_chemical_name_systematic
;
  ?
;
_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                85.53(1)
_cell_angle_beta                 72.32(1)
_cell_angle_gamma                80.04(1)
_cell_formula_units_Z            2
_cell_length_a                   10.677(1)
_cell_length_b                   11.171(2)
_cell_length_c                   13.241(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     1481.5(4)
_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      200.0(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Siemens P4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus Bruker-Siemens sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6099
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.416
_exptl_absorpt_correction_T_max  0.278
_exptl_absorpt_correction_T_min  0.195
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5185
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.680
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=3D1/[\s^2^(Fo^2^)+(0.0823P)^2^+6.4572P] where P=3D(Fo^2^+2Fc^2^)/3='
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                4683
_reflns_number_total             5185
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063191