Synthesis and Structure of Ruthenium(IV) Complexes Featuring N-Heterocyclic Ligands with an N-H Group as the Hydrogen-Bond Donor: Hydrogen Interactions in Solution and in the Solid State
Josefina Díez; José Gimeno; Isabel Merino; Eduardo Rubio; Francisco J. Suárez; Inorganic Chemistry 50 (2011) 4868–4881; doi:10.1021/ic200547k

data_4325301
_publ_contact_author
;
      Josefina D\'iez
      Departamento de Qu\'imica Org\'anica e Inorg\'anica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33006 Oviedo
      Spain
;
_publ_contact_author_email       jdv@uniovi.es
_publ_contact_author_fax         '0034 98 5103446'
_publ_contact_author_phone       '0034 98 5102960'
_publ_section_title
;
 Synthesis and Structure of Ruthenium(IV) Complexes Featuring
 N-Heterocyclic Ligands with an N-H Group as the Hydrogen-Bond Donor:
 Hydrogen Interactions in Solution and in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4868
_journal_page_last               4881
_journal_paper_doi               10.1021/ic200547k
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C14 H22 Cl2 N2 Ru'
_chemical_formula_sum            'C14 H22 Cl2 N2 Ru'
_chemical_formula_weight         390.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
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_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                   7.6952(1)
_cell_length_b                   22.8324(3)
_cell_length_c                   9.0117(1)
_cell_measurement_reflns_used    5094
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.1345
_cell_measurement_theta_min      3.8689
_cell_volume                     1583.35(3)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device
; 
165 mm Onyx CCD detector in \k-geometry diffractometer
;
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6321
_diffrn_reflns_theta_full        74.30
_diffrn_reflns_theta_max         74.30
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    11.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.250(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2723
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                2565
_reflns_number_total             2723
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200547k_si_002_3.cif
_cod_data_source_block           2b
_cod_database_code               4325301