Fragmentation Pathways of [MX2(CO)2(dcbpy)] (M = Ru, Os; X = Cl, Br, I; dcbpy = 2,2′-bipyridine-4,4′-dicarboxylic acid) Complexes
Jänis, Janne; Jakonen, Minna; Oresmaa, Larisa; Hirva, Pipsa; Laurila, Elina; Vlasova, Liubov; Vainiotalo, Pirjo; Haukka, Matti; Organometallics 29 (2010) 1070–; doi:10.1021/om900661t

data_4067261
_publ_section_title
;
 Fragmentation Pathways of [MX2(CO)2(dcbpy)] (M = Ru, Os; X = Cl, Br, I;
 dcbpy = 2,2&#x2032;-bipyridine-4,4&#x2032;-dicarboxylic acid) Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1070
_journal_paper_doi               10.1021/om900661t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C14 H8 Br2 N2 O6 Os, H2 O'
_chemical_formula_sum            'C14 H10 Br2 N2 O7 Os'
_chemical_formula_weight         668.26
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.611(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6047(5)
_cell_length_b                   19.573(2)
_cell_length_c                   13.3682(12)
_cell_measurement_reflns_used    4461
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1724.7(3)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1e (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0923
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12028
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    12.067
_exptl_absorpt_correction_T_max  0.6181
_exptl_absorpt_correction_T_min  0.2592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.070
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0544P)^2^+22.7859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                2093
_reflns_number_total             2991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900661t_si_001.cif
_cod_data_source_block           2
_cod_original_cell_volume        1724.8(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4067261