Solvent-Dependent Formation of Os(0) Complexes by Electrochemical Reduction of [Os(CO)(2,2'-bipyridine)(L)Cl2]; L = Cl(-), PrCN.
Tory, Joanne; King, Lisa; Maroulis, Antonios; Haukka, Matti; Calhorda, Maria José; Hartl, František; Inorganic chemistry 53 (2014) 1382–1396; doi:10.1021/ic402146t

data_4337351
_publ_section_title
;
 Solvent-Dependent Formation of Os(0) Complexes by Electrochemical
 Reduction of [Os(CO)(2,2'-bipyridine)(L)Cl2]; L = Cl(-), PrCN.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1382
_journal_page_last               1396
_journal_paper_doi               10.1021/ic402146t
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C11 H12 Cl3 N2 O Os, C H4 O'
_chemical_formula_sum            'C12 H16 Cl3 N2 O2 Os'
_chemical_formula_weight         516.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5802(3)
_cell_length_b                   14.2081(14)
_cell_length_c                   16.4891(8)
_cell_measurement_reflns_used    7626
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     1541.60(18)
_computing_cell_refinement       'EvalCCD (Duisenberg, 2003)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2008)'
_computing_data_reduction        'EvalCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'Diamond v.3.2g (Brandenburg, 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30832
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    8.792
_exptl_absorpt_correction_T_max  0.5050
_exptl_absorpt_correction_T_min  0.3099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0284
_refine_ls_wR_factor_ref         0.0292
_reflns_number_gt                4201
_reflns_number_total             4464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402146t_si_003.cif
_cod_data_source_block           tn0803e
_cod_database_code               4337351