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_4325303
_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         'C19 H24 Cl2 N2 O Ru'
_chemical_formula_sum            'C19 H24 Cl2 N2 O Ru'
_chemical_formula_weight         468.37
_chemical_name_systematic
;
 ?
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.335(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2255(8)
_cell_length_b                   8.3163(4)
_cell_length_c                   14.5735(4)
_cell_measurement_reflns_used    3457
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_volume                     1965.96(15)
_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_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      293(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_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11668
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3589
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                2412
_reflns_number_total             3589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200547k_si_002_5.cif
_cod_data_source_block           2e
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4325303