Unusual Monodentate Binding Mode of 2,2'-Dipyridylamine (L) in Isomeric trans-(acac)2RuII(L)2, trans-[(acac)2RuIII(L)2]ClO4, and cis-(acac)2RuII(L)2 (acac = Acetylacetonate). Synthesis, Structures, and Spectroscopic, Electrochemical, and Magnetic Aspects
Sanjib Kar; Nripen Chanda; Shaikh M. Mobin; Francisco A. Urbanos; Mark Niemeyer; Vedavati G. Puranik; Reyes Jimenez-Aparicio; Goutam Kumar Lahiri; Inorganic Chemistry 44 (2005) 1571–1579; doi:10.1021/ic049219v

data_4308787
_publ_section_title
;
Unusual Monodentate Binding Mode of 2,2'-Dipyridylamine (L) in
Isomeric trans-(acac)2RuII(L)2, trans-[(acac)2RuIII(L)2]ClO4,
and cis-(acac)2RuII(L)2 (acac = Acetylacetonate). Synthesis, Structures, and
Spectroscopic, Electrochemical, and Magnetic Aspects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1571
_journal_page_last               1579
_journal_paper_doi               10.1021/ic049219v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C30 H32 Cl N6 O8 Ru'
_chemical_formula_weight         741.14
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(17)
_cell_angle_beta                 127.129(19)
_cell_angle_gamma                90.000(19)
_cell_formula_units_Z            4
_cell_length_a                   26.6680(17)
_cell_length_b                   7.773(3)
_cell_length_c                   19.494(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.0500
_cell_measurement_theta_min      5.2000
_cell_volume                     3221.7(16)
_computing_cell_refinement       'Argus (Nonius, MACH3 software)'
_computing_data_collection       'Argus (Nonius, MACH3 software)'
_computing_data_reduction        'Maxus (Nonius software)'
_computing_molecular_graphics    Ortep
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.460
_diffrn_measured_fraction_theta_max 0.460
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4447
_diffrn_reflns_theta_full        24.92
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        >3%
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.7425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                2010
_reflns_number_total             2605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049219vsi20040616_080317.cif
_cod_data_source_block           max
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.7425P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.7425P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3221.7(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4308787