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_4323177
_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            'C48 H39 Cl N3 O P2 Ru'
_chemical_formula_weight         872.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.28(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.244(9)
_cell_length_b                   11.047(4)
_cell_length_c                   22.076(7)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     4171(3)
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0969
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6814
_diffrn_reflns_theta_max         24.05
_diffrn_reflns_theta_min         1.60
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_obs          0.0612
_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^)+(0.0404P)^2^+4.0443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1432
_refine_ls_wR_factor_obs         0.1072
_reflns_number_observed          3940
_reflns_number_total             6571
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980719w_1.cif
_cod_data_source_block           '[Ru(pap._)(Cl)(CO)(PPh3)2],3a'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+4.0443P] 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^)+(0.0404P)^2^+4.0443P] 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        4171.0(3.1)
_cod_original_formula_sum        'C48 H39 N3 O P2 Cl Ru'
_cod_database_code               4323177