Isolation and Structure of the First Azo Anion Radical Complexes of Ruthenium
Maya Shivakumar; Kausikisankar Pramanik; Prasanta Ghosh; Animesh Chakravorty; Inorganic Chemistry 37 (1998) 5968–5969; doi:10.1021/ic980719w

data_4323179
_publ_section_title
;
 Isolation and Structure of the First Azo Anion Radical Complexes of
 Ruthenium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5968
_journal_page_last               5969
_journal_paper_doi               10.1021/ic980719w
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C32 H28 Cl N2 O P Ru'
_chemical_formula_weight         624.05
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                85.96(4)
_cell_angle_beta                 83.01(4)
_cell_angle_gamma                78.08(4)
_cell_formula_units_Z            2
_cell_length_a                   9.756(6)
_cell_length_b                   10.802(5)
_cell_length_c                   14.242(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1456.0(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       w-scan
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.1189
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5472
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.93
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.127
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.127
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_obs          0.0770
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2030
_refine_ls_wR_factor_obs         0.1660
_reflns_number_observed          3077
_reflns_number_total             5130
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980719w_3.cif
_cod_data_source_block           '[Ru(pal)(H)(CO)(PPh3)],5'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0949P)^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^)+(0.0949P)^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        1453.9(12)
_cod_original_formula_sum        'C32 H28 N2 O P Cl Ru'
_cod_database_code               4323179