An alternative synthesis method for [Os(NN)(CO)(2)X(2)] complexes (NN = 2,2'-bipyridine, 4,4'-dimethyl-2,2'-bipyridine; X = Cl, Br, I). Electrochemical and photochemical properties and behavior.
Jakonen, Minna; Hirva, Pipsa; Haukka, Matti; Chardon-Noblat, Sylvie; Lafolet, Frédéric; Chauvin, Jérôme; Deronzier, Alain; Dalton transactions (Cambridge, England : 2003)  (2007) 3314–3324; doi:10.1039/b704931e

data_7005732
_publ_section_title
;
 An alternative synthesis method for [Os(NN)(CO)(2)X(2)] complexes (NN
 = 2,2'-bipyridine, 4,4'-dimethyl-2,2'-bipyridine; X = Cl, Br, I).
 Electrochemical and photochemical properties and behavior.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3314
_journal_page_last               3324
_journal_paper_doi               10.1039/b704931e
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C12 H8 I2 N2 O2 Os'
_chemical_formula_sum            'C12 H8 I2 N2 O2 Os'
_chemical_formula_weight         656.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 101.737(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4170(4)
_cell_length_b                   7.0934(4)
_cell_length_c                   13.1254(6)
_cell_measurement_reflns_used    2570
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     767.27(7)
_computing_cell_refinement       'EvalCCD (Duisenberg, 1998-2003)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998-2003)'
_computing_molecular_graphics    'Diamond v.3.1d (Brandenburg, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      120(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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7768
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    12.331
_exptl_absorpt_correction_T_max  0.5382
_exptl_absorpt_correction_T_min  0.2632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0260
_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          0.0386
_refine_ls_wR_factor_ref         0.0407
_reflns_number_gt                2839
_reflns_number_total             3208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704931e.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7005732