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_7000456
_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] (523 mg, 1.35 mmol) is suspended in 100 mL Ethanol/H2O (3/1),
then methyliminodiacetic acid (199 mg, 1.35 mmol) is solved in 5 mL H2O and
added dropwise to the suspension. The pH value of the suspension is adjusted to
5 with a concentrated solution of KOH in H2O. Then the mixture is refluxed for
6 hours and the resulting brown solution is stored in a refrigerator. Within
2 weeks brown crystals are obtained which are filtered, washed with 40 mL
Ethanol/H2O (3/1) and 100 mL diethylether, and vacuum-dried.
;
_chemical_formula_moiety         'C5 H7 Cl2 N2 O5 Ru, K, 0.5(H2 O)'
_chemical_formula_sum            'C5 H8 Cl2 K N2 O5.5 Ru'
_chemical_formula_weight         395.20
_chemical_name_common            'K(Ru(NO)Cl2(MeImDiacH-2)) 0.5(H2O)'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Ru_NO_Cl_Cl_MeImDiacH-2_K_0.5(H2O)_kn189_Zangl
_audit_creation_date             04-May-06
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9859(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.2438(5)
_cell_length_b                   6.43210(10)
_cell_length_c                   13.2528(2)
_cell_measurement_reflns_used    4031
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.999
_cell_measurement_theta_min      3.134
_cell_volume                     2355.11(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7185
_diffrn_reflns_theta_full        31.12
_diffrn_reflns_theta_max         31.12
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    2.149
_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            orange
_exptl_crystal_density_diffrn    2.22922(7)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.106
_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     156
_refine_ls_number_reflns         3764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0265
_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          0.0630
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                3151
_reflns_number_total             3764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812246f.txt
_cod_data_source_block           4
_cod_original_formula_sum        'C5 H8 Cl2 K N2 O5.50 Ru'
_cod_database_code               7000456