Monocationic Trihydride and Dicationic Dihydride-Dihydrogen and Bis(dihydrogen) Osmium Complexes Containing Cyclic and Acyclic Triamine Ligands: Influence of the N-Os-N Angles on the Hydrogen-Hydrogen Interactions
Miguel Baya; Miguel A. Esteruelas; Montserrat Oliván; Enrique Oñate; Inorganic Chemistry 48 (2009) 2677–2686; doi:10.1021/ic8023259

data_4301746
_publ_contact_author
;
  Dr. Enrique O\~nate Rodr\'iguez
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@posta.unizar.es
_publ_section_title
;
Monocationic Trihydride and Dicationic Dihydride-Dihydrogen and
Bis(dihydrogen) Osmium Complexes Containing Cyclic and Acyclic Triamine
Ligands: Influence of the N-Os-N Angles on the Hydrogen-Hydrogen
Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2677
_journal_page_last               2686
_journal_paper_doi               10.1021/ic8023259
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C15 H40 N3 Os P, 2 (B F4), C2 H3 N'
_chemical_formula_sum            'C17 H43 B2 F8 N4 Os P'
_chemical_formula_weight         698.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.868(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1936(14)
_cell_length_b                   33.085(6)
_cell_length_c                   9.7024(16)
_cell_measurement_reflns_used    4514
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2620.7(8)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17705
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.997
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.096
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6245
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                5011
_reflns_number_total             6245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8023259_si_001_3.cif
_cod_data_source_block           mae288as
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301746