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_7000454
_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] (802 mg, 2.08 mmol), DL-2,3-Diaminopropionic acid
monohydrochlorid (584 mg, 4.15 mmol) and KCl (1.55 g, 20.8 mmol) are solved in
250 mL H2O. The pH-value of the solution is adjusted to 4 with a concentrated
solution of KOH in H2O. Then the mixture is refluxed for 2 hours and the
resulting orange solution is evaporated to dryness on a rotary evaporator. The
residue is suspended in a small amount of H2O and purified by centrifugation.
This procedure is repeated three times, then the resulting orange solid is
vacuum-dried. Crystals are obtained by heating the solid in little H2O until a
clear solution results which is left standing to slowly cool down to room
temperature. Within a day small orange crystals emerge from the solution.
;
_chemical_formula_moiety         'C3 H7 Cl2 N3 O3 Ru'
_chemical_formula_sum            'C3 H7 Cl2 N3 O3 Ru'
_chemical_formula_weight         305.08
_chemical_name_common            (Ru(NO)Cl2(DL-AmAlaH-1))
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_block_code                Ru_NO_Cl_Cl_DL-AmAlaH-1_ln069_Zangl
_audit_creation_date             09-Feb-07
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.043(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5310(3)
_cell_length_b                   12.4611(5)
_cell_length_c                   10.2292(4)
_cell_measurement_reflns_used    7698
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     832.49(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3660
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    2.494
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet,
Eds., Academic Press (New York).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.43418(18)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1903
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                1563
_reflns_number_total             1903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812246f.txt
_cod_data_source_block           2
_cod_database_code               7000454