Preparation and Characterization of Novel Os−Diolefin Dimers: New Entry to Os−Cyclooctadiene Complexes
Esteruelas, Miguel A.; García-Yebra, Cristina; Oliván, Montserrat; Oñate, Enrique; Inorganic Chemistry 45 (2006) 10162–10171; doi:10.1021/ic0612799

data_4333018
_publ_section_title
;
 Preparation and Characterization of Novel Os&#x2212;Diolefin
 Dimers:&#x00A0; New Entry to Os&#x2212;Cyclooctadiene Complexes
;
_journal_issue                   25
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10162
_journal_page_last               10171
_journal_paper_doi               10.1021/ic0612799
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C20 H38 Cl4 O2 Os2'
_chemical_formula_weight         832.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.064(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0837(14)
_cell_length_b                   8.6975(13)
_cell_length_c                   15.876(2)
_cell_measurement_reflns_used    918
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1244.8(3)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15632
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    10.642
_exptl_absorpt_correction_T_max  0.297
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    2.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.918
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         6002
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                5363
_reflns_number_total             6002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0612799sup1.cif
_cod_data_source_block           mae175as
_cod_original_cell_volume        1244.7(3)
_cod_database_code               4333018