Stepwise Synthesis of [Ru(trpy)(L)(X)]n+ (trpy = 2,2':6',2''-Terpyridine; L = 2,2'-Dipyridylamine; X = Cl-, H2O, NO2-, NO+, O2-). Crystal Structure, Spectral, Electron-Transfer, and Photophysical Aspects
Nripen Chanda; Shaikh M. Mobin; Vedavati G. Puranik; Anindya Datta; Mark Niemeyer; Goutam Kumar Lahiri; Inorganic Chemistry 43 (2004) 1056–1064; doi:10.1021/ic034902n

data_4310511
_publ_section_title
;
 Stepwise Synthesis of [Ru(trpy)(L)(X)]n+ (trpy = 2,2':6',2''-Terpyridine;
 L = 2,2'-Dipyridylamine; X = Cl-, H2O, NO2-, NO+, O2-). Crystal
 Structure, Spectral, Electron-Transfer, and Photophysical Aspects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1056
_journal_page_last               1064
_journal_paper_doi               10.1021/ic034902n
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C25 H20 O N7 Ru 3(ClO4).CH3CN 0.5(H2O)'
_chemical_formula_sum            'C27 H24 Cl3 N8 O13.5 Ru'
_chemical_formula_weight         883.96
_chemical_name_common            'Ru Complex'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.280(2)
_cell_length_b                   14.7070(12)
_cell_length_c                   12.7170(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.89
_cell_measurement_theta_min      5.28
_cell_volume                     3418.9(6)
_computing_cell_refinement       'Argus(Nonius,MACH# Software)'
_computing_data_collection       'Argus(Nonius,MACH# Software)'
_computing_data_reduction        'Maxus(Nonius,MACH# Software)'
_computing_molecular_graphics    'SHELXTL and PLATON'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2585
_diffrn_reflns_theta_full        24.92
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        <3%
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.9097
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'psi-scan(North, Philips & Mathews, 1968)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Bloc
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         2585
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0423P)^2^+8.9877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                1925
_reflns_number_total             2585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034902nsi20030730_102847.cif
_cod_data_source_block           C25H20ON7Ru3(ClO4).CH3CN0.5(H2O)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_formula_sum        'C27 H24 Cl3 N8 O13.50 Ru'
_cod_database_code               4310511