Heteroleptic tris-chelates of ruthenium(ii)-bipyridine-arylazoimidazoles: Synthesis, spectral characterisation and electrochemical properties. Single crystal X-ray structure of [(2,2'-bipyridine)-bis-{1-methyl-2-(p-tolylazo)imidazole}ruthenium(ii)] perchlorate
Byabartta, Prithwiraj; Dinda, Joydev; Santra, Prasanta Kumar; Sinha, Chittaranjan; Panneerselvam, Kaliyamoorthy; Liao, Fan-Ling; Lu, Tian-Huey; Journal of the Chemical Society, Dalton Transactions  (2001) 2825–; doi:10.1039/b103782j

data_7010789
_publ_section_title
;
 Heteroleptic tris-chelates of
 ruthenium(ii)-bipyridine-arylazoimidazoles: Synthesis, spectral
 characterisation and electrochemical properties. Single crystal X-ray
 structure of
 [(2,2'-bipyridine)-bis-{1-methyl-2-(p-tolylazo)imidazole}ruthenium(ii)]
 perchlorate
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2825
_journal_paper_doi               10.1039/b103782j
_journal_year                    2001
_chemical_formula_sum            'C33 H34 Cl4 N10 O8 Ru'
_chemical_formula_weight         941.57
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.834(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.649(2)
_cell_length_b                   12.0387(16)
_cell_length_c                   19.374(2)
_cell_measurement_reflns_used    25883
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.18
_cell_volume                     4013.6(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25269
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.9710
_exptl_absorpt_correction_T_min  0.8783
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+8.0655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2281
_reflns_number_gt                5763
_reflns_number_total             9575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103782j.txt
_cod_data_source_block           fb07m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        4013.5(9)
_cod_original_sg_symbol_H-M      P2~1~/c
_cod_database_code               7010789