Ru^II^‒hydride‒<i>trop</i> complexes: X-ray single-crystal determination and quantum-chemical calculations
Santiso-Quinones, Gustavo; Rodriguez-Lugo, Rafael; Sacchetti, Vittorio; Grützmacher, Hansjörg; Acta Crystallographica Section C 69 (2013) 1421–1426; doi:10.1107/S0108270113024505

data_2019281
_publ_section_title
;
 Ru^II^--hydride--<i>trop</i> complexes: X-ray single-crystal
 determination and quantum-chemical calculations
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1421
_journal_page_last               1426
_journal_paper_doi               10.1107/S0108270113024505
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ru H2 (C21 H18 N2) (C18 H15 P)], C4 H8 O'
_chemical_formula_moiety         'C39 H35 N2 P Ru, C4 H8 O'
_chemical_formula_sum            'C43 H43 N2 O P Ru'
_chemical_formula_weight         735.83
_chemical_name_common
;
(S)-[Ru^II^(H)~2~(N-(pyridine-2-ylmethyl)(tropNH)(PPh~3~)].THF
;
_chemical_name_systematic
'Dihydrido[(\h-10,11)-(<i>SR</i>)<i>N</i>-(pyridine-2-ylmethyl-\k<i>N</i>)-5<i>H</i>-dibenzo[<i>a</i>,<i>d</i>]cyclohepten-5-amine](triphenylphosphane-\k<i>P</i>)ruthenium(II) tetrahydrofuran monosolvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.6590(10)
_cell_angle_beta                 92.2970(10)
_cell_angle_gamma                99.0400(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6656(8)
_cell_length_b                   11.8605(9)
_cell_length_c                   14.6067(11)
_cell_measurement_reflns_used    7529
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.33
_cell_volume                     1720.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14969
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_correction_T_min  0.9302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         7529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.7263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                6442
_reflns_number_total             7529
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fa3321.cif
_cod_data_source_block           I
_cod_database_code               2019281