Photoinduced linkage isomerism of {RuNO}6 complexes with bioligands and related chelators
Zangl, Anna; Klüfers, Peter; Schaniel, Dominik; Woike, Theo; Dalton Transactions  (2009) 1034–1045; doi:10.1039/b812246f

data_7000453
_publ_section_title
;
 Photoinduced linkage isomerism of {RuNO}6 complexes with bioligands
 and related chelators
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1034
_journal_page_last               1045
_journal_paper_doi               10.1039/b812246f
_journal_year                    2009
_chemical_compound_source
;
K2[Ru(NO)Cl5] (658 mg, 1.70 mmol), L-histidine monohydrochloride monohydrate
(358 mg, 1.71 mmol) and KCl (1.26 g, 16.9 mmol) are solved in 250 mL H2O. The
pH value of the solution is adjusted to 4 with 0.1 M HCl. After refluxing for 2
hours the resulting light brown solution is evaporated to dryness on a rotary
evaporator. The residue is suspended in a small amount of H2O and purified by
centrifugation (3 times). Then the resulting brown solid is vacuum-dried.
Crystals suitable for X-ray crystallography can be obtained from a diluted
aqueous solution of the complex in H2O by slow evaporation of the solvent at
room temperature.
;
_chemical_formula_moiety         'C6 H8 Cl2 N4 O3 Ru'
_chemical_formula_sum            'C6 H8 Cl2 N4 O3 Ru'
_chemical_formula_weight         356.13
_chemical_name_common            (Ru(NO)Cl2(L-HisH-1))
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Ru_NO_Cl_Cl_L-HisH-1_kn113_Zangl
_audit_creation_date             27-Mar-07
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2032(2)
_cell_length_b                   10.7355(3)
_cell_length_c                   12.9656(3)
_cell_measurement_reflns_used    9230
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1141.82(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_collimation    0.20
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13632
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program.
University of G\"ottingen, Germany, 2001.

spherical correction included with mu*r = 0.073, leads to Tmin/Tmax = 0.6338
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.07169(9)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                2485
_reflns_number_total             2614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812246f.txt
_cod_data_source_block           1
_cod_database_code               7000453