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_4301027
_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            'C41 H30 Cl O4 Os P2'
_chemical_formula_weight         874.24
_chemical_name_systematic
; 

 ? 

;
_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                99.96(2)
_cell_angle_beta                 105.47(3)
_cell_angle_gamma                104.69(4)
_cell_formula_units_Z            2
_cell_length_a                   10.302(3)
_cell_length_b                   12.262(3)
_cell_length_c                   15.481(5)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1761.4(11)
_computing_cell_refinement       'Siemens R3m/V'
_computing_data_collection       'Siemens R3m/V'
_computing_data_reduction        XDISK
_computing_molecular_graphics    'Siemens SHELXTL-PLUS (VMS)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'Siemens P4 4-circle-diffractometer'
_diffrn_measurement_method       'Profile fitted'
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6084
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.829
_exptl_absorpt_correction_T_max  0.20538
_exptl_absorpt_correction_T_min  0.15134
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0521P)^2^+0.5174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                4188
_reflns_number_total             5110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049149ssi20040629_025031.cif
_cod_data_source_block           bhattaos
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1761.4(9)
_cod_original_formula_sum        'C41 H30 O4 P2 Cl Os'
_cod_database_code               4301027