Variable Coordination Mode of Chloranilic Acid. Synthesis, Structure, and Electrochemical Properties of Some Osmium Complexes
Parna Gupta; Anindya Das; Falguni Basuli; Alfonso Castineiras; William S. Sheldrick; Heike Mayer-Figge; Samaresh Bhattacharya; Inorganic Chemistry 44 (2005) 2081–2088; doi:10.1021/ic049149s

data_4301025
_publ_section_title
;

Variable Coordination Mode of Chloranilic Acid. Synthesis, Structure, and

Electrochemical Properties of Some Osmium Complexes

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2081
_journal_page_last               2088
_journal_paper_doi               10.1021/ic049149s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C106 H84 Cl4 N6 O12 Os2 P4'
_chemical_formula_weight         2279.87
_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                88.500(10)
_cell_angle_beta                 80.518(9)
_cell_angle_gamma                70.631(9)
_cell_formula_units_Z            1
_cell_length_a                   12.1895(9)
_cell_length_b                   12.8575(11)
_cell_length_c                   17.0049(13)
_cell_measurement_temperature    173(2)
_cell_volume                     2478.8(4)
_computing_cell_refinement       'Stoe IPDS measurement'
_computing_data_collection       'Stoe IPDS measurement'
_computing_data_reduction        'STOE Data Reduction'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Stoe IPDS measurement'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33151
_diffrn_reflns_theta_full        29.06
_diffrn_reflns_theta_max         29.06
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.7138
_exptl_absorpt_correction_T_min  0.5865
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.909
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         12139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                10186
_reflns_number_total             12139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049149ssi20040629_024836.cif
_cod_data_source_block           acs2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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^)+(0.0984P)^2^+0.0000P] 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^)+(0.0984P)^2^+0.0000P] 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        2478.8(3)
_cod_database_code               4301025