Reaction of a Cationic Osmium(IV) Dihydride with Ethylene: Formation and Structure of the Novel Tetraethylene Dimer Complex [{(PiPr3)(η2-C2H4)2Os}2(μ-OH)2(μ-O2CCH3)]BF4
Esteruelas, Miguel A.; García-Yebra, Cristina; Oliván, Montserrat; Oñate, Enrique; Organometallics 19 (2000) 3260–3262; doi:10.1021/om000214p

data_4077509
_publ_contact_author
;
       Enrique O\-ate Rodr\'iguez
       Departamento de Qu\'imica Inorg'anica
       Facultad de Ciencias
       Universidad de Zaragoza
       50009-Zaragoza
       Spain
;
_publ_section_title
;
 Reaction of a Cationic Osmium(IV) Dihydride with Ethylene:&#x00A0;
 Formation and Structure of the Novel Tetraethylene Dimer Complex
 [{(PiPr3)(\h2-C2H4)2Os}2(\m-OH)2(\m-O2CCH3)]BF4
;
_journal_coden_ASTM              ORGND7
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3260
_journal_page_last               3262
_journal_paper_doi               10.1021/om000214p
_journal_volume                  19
_journal_year                    2000
_chemical_formula_structural
;
[{(P^i^Pr-3-)(\h^2^-C-2-H-4-)-2-Os}-2-(\m-OH)-2-(\m-O-2-CCH-3-)]BF-4-
;
_chemical_formula_sum            'C28 H63 B F4 O4 Os2 P2'
_chemical_formula_weight         992.93
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.371(3)
_cell_length_b                   11.934(3)
_cell_length_c                   19.360(5)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     3551.4(15)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9898
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.290
_exptl_absorpt_correction_T_max  0.190
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.035
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     'not used'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                4220
_reflns_number_total             6202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000214p.cif
_cod_data_source_block           comp1
_cod_original_cell_volume        3551.3(15)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077509