Thermally Activated Site Exchange and Quantum Exchange Coupling Processes in Unsymmetrical Trihydride Osmium Compounds
Amaya Castillo; Guada Barea; Miguel A. Esteruelas; Fernando J. Lahoz; Agustí LLedós; Feliu Maseras; Javier Modrego; Enrique Oñate; Luis A. Oro; Natividad Ruiz; Eduardo Sola; Inorganic Chemistry 38 (1999) 1814–1824; doi:10.1021/ic9804061

data_4321900
_publ_contact_author
;
     Enrique O\~nate Rodr\'iguez
     Departamento de Qu\'imica Inorg\'anica
     Facultad de Ciencias
     Universidad de Zaragoza
     50009-Zaragoza
     Spain
;
_publ_contact_author_email       onate@posta.unizar.es
_publ_section_title
;
 Thermally Activated Site Exchange and Quantum Exchange Coupling Processes
 in Unsymmetrical Trihydride Osmium Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1814
_journal_page_last               1824
_journal_paper_doi               10.1021/ic9804061
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural
;
OsH~3~(\k^2^-N,S-(2-Spy))(P^i^Pr~3~)~2~
;
_chemical_formula_sum            'C23 H49 N Os P2 S'
_chemical_formula_weight         623.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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           PARSTCIF
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 98.23(3)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   8.832(2)
_cell_length_b                   21.124(5)
_cell_length_c                   14.923(4)
_cell_measurement_radiation      'Mo, K\a'
_cell_measurement_reflns_used    64
_cell_measurement_temperature    230.0(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71073
_cell_volume                     2755.5(12)
_computing_cell_refinement       'DIF4 (Siemens-Stoe)'
_computing_data_collection       'DIF4 (Siemens-Stoe)'
_computing_data_reduction        'REDU4 (Siemens-Stoe)'
_computing_molecular_graphics    'XP, SHELXTL v. 4.2 (Siemens)'
_computing_publication_material
;
 PARST (Nardelli, 1983); PARSTCIF (Nardelli, 1991)
;
_computing_structure_refinement  'SHELXTL v. 4.2 (Siemens)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      230.0(2)
_diffrn_measurement_device       'Siemens Stoe AED-2'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus Siemens Mo sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8132
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.8292
_exptl_absorpt_correction_T_max  0.1690
_exptl_absorpt_correction_T_min  0.0321
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.5038
_exptl_crystal_description       block
_exptl_crystal_F_000             1264.0
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.67
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.89
_refine_ls_extinction_coef       'not used'
_refine_ls_extinction_expression 'not used'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.0892
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_obs      1.0892
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_obs          0.0301
_refine_ls_shift/esd_max         0.2
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
calc w=1/[\s^2^(F)+0.000725(F^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0452
_refine_ls_wR_factor_obs         0.0328
_reflns_number_observed          3390
_reflns_number_total             4852
_reflns_observed_criterion       >5sigma(F)
_cod_data_source_file            ic9804061.cif
_cod_data_source_block           comp2
_cod_original_cell_volume        2756.(1)
_cod_database_code               4321900