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_4063192
_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=97N(CH=972=97CH=3DCH=972=97)=972=97(GePh=973=
=97)(P^i^Pr=973=97)
;
_chemical_formula_sum            'C38 H52 Ge N Os P'
_chemical_formula_weight         816.57
_chemical_name_systematic
;
  ?
;
_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                 91.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.345(2)
_cell_length_b                   20.975(2)
_cell_length_c                   13.932(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     3606.9(9)
_computing_cell_refinement       'DIF4 (Bruker-Siemens STOE)'
_computing_data_collection       'DIF4 (Bruker-Siemens STOE)'
_computing_data_reduction        'REDU4 (Bruker-Siemens STOE)'
_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      298.0(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Siemens STOE AED-2'
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10274
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.423
_exptl_absorpt_correction_T_max  0.448
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.127
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=3D1/[\s^2^(Fo^2^)+(0.0437P)^2^+2.0347P] where P=3D(Fo^2^+2Fc^2^)/3='
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                5183
_reflns_number_total             6330
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4063192