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_4316681
_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         'C39 H32 Cl3 O Os P2, O0.50 C2 H5'
_chemical_formula_sum            'C41 H37 Cl3 O1.5 Os P2'
_chemical_formula_weight         912.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.570(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.072(3)
_cell_length_b                   13.377(4)
_cell_length_c                   26.711(7)
_cell_measurement_reflns_used    5178
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     3597.5(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.941
_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    0.0910
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            44481
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.684
_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            yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.415
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8976
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                6481
_reflns_number_total             8976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101498h_si_002_1.cif
_cod_data_source_block           mae390as
_cod_original_cell_volume        3597.5(17)
_cod_original_formula_sum        'C41 H37 Cl3 O1.50 Os P2'
_cod_database_code               4316681