Unusual Coordination Mode of Thiosemicarbazone Ligand. Synthesis, Structure, and Redox Properties of Some Ruthenium and Osmium Complexes
Falguni Basuli; Michael Ruf; Cortlandt G. Pierpont; Samaresh Bhattacharya; Inorganic Chemistry 37 (1998) 6113–6116; doi:10.1021/ic980424i

data_4323162
_publ_section_title
;
 Unusual Coordination Mode of Thiosemicarbazone Ligand. Synthesis,
 Structure, and Redox Properties of Some Ruthenium and Osmium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6113
_journal_page_last               6116
_journal_paper_doi               10.1021/ic980424i
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C52 H44 N8 O4 P2 Ru S2'
_chemical_formula_weight         1072.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.560(13)
_cell_angle_beta                 94.313(10)
_cell_angle_gamma                103.531(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4528(13)
_cell_length_b                   11.996(2)
_cell_length_c                   18.347(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      0
_cell_volume                     2407.5(6)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14345
_diffrn_reflns_theta_full        31.21
_diffrn_reflns_theta_max         31.21
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9113
_exptl_absorpt_correction_T_min  0.7615
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         14345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.8214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                12897
_reflns_number_total             14345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980424i.cif
_cod_data_source_block           RUNS
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.8214P] 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^)+(0.0300P)^2^+0.8214P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323162