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_2019283
_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 Cl H (C33 H30 N2)]'
_chemical_formula_moiety         'C33 H31 Cl N2 Ru'
_chemical_formula_sum            'C33 H31 Cl N2 Ru'
_chemical_formula_weight         592.12
_chemical_name_common
;
(S,R)-[Ru^II^(H)(Cl)(<i>trop</i>HN(CH~2~)~3~HN<i>trop</i>)]
;
_chemical_name_systematic
Chlorido{(1<i>SR</i>,2<i>RS</i>)-<i>N</i>,<i>N</i>'-bis[(10,11-\h)-5<i>H</i>-dibenzo[<i>a</i>,<i>d</i>]cyclohepten-5-amine]propane-1,3-diamine-\k^2^<i>N</i>,<i>N</i>'}hydridoruthenium(II)
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.1125(4)
_cell_length_b                   24.1125(4)
_cell_length_c                   18.0487(7)
_cell_measurement_reflns_used    6515
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.20
_cell_volume                     10493.7(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0907
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57769
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.9510
_exptl_absorpt_correction_T_min  0.9310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.529
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                4331
_reflns_number_total             6515
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fa3321.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2019283