Osmium(III) Complexes with POP Pincer Ligands: Preparation from Commercially Available OsCl3.3H2O and Their X-ray Structures
Gregorio Asensio; Ana B. Cuenca; Miguel A. Esteruelas; Mercedes Medio-Simón; Montserrat Oliván; Marta Valencia; Inorganic Chemistry 49 (2010) 8665–8667; doi:10.1021/ic101498h

data_4316684
_publ_contact_author
;
  Dr. Montserrat Oliv\'an
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       molivan@unizar.es
_publ_section_title
;
 Osmium(III) Complexes with POP Pincer Ligands: Preparation from
 Commercially Available OsCl3.3H2O and Their X-ray Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8665
_journal_page_last               8667
_journal_paper_doi               10.1021/ic101498h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C27 H40 Cl3 O Os P2'
_chemical_formula_sum            'C27 H40 Cl3 O Os P2'
_chemical_formula_weight         739.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.643(7)
_cell_length_b                   17.961(6)
_cell_length_c                   15.261(5)
_cell_measurement_reflns_used    8004
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     5932(3)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            73081
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.696
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.473
_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.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.297
_refine_diff_density_min         -1.646
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.696
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         14760
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.696
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.564
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0432
_reflns_number_gt                9909
_reflns_number_total             14760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101498h_si_002_4.cif
_cod_data_source_block           mae431bs
_cod_database_code               4316684