Synthesis of the acidic dihydrogen complexes trans-[M(H2)(CN)L2]+ and trans-[M(H2)(CNH)L2]2+ where M = Fe, Ru, Os and L = dppm, dppe, dppp, depe, and dihydrogen substitution by the trifluoromethanesulfonate anion to give trans-[Ru(OTf )(CN)L2] or trans-[Ru(OTf )(CNH)L2]OTf †
Fong, Tina P.; Forde, Cameron E.; Lough, Alan J.; Morris, Robert H.; Rigo, Pierluigi; Rocchini, Eliana; Stephan, Tim; Journal of the Chemical Society, Dalton Transactions  (1999) 4475–; doi:10.1039/a906717e

data_7027778
_publ_section_title
;
 Synthesis of the acidic dihydrogen complexes trans-[M(H2)(CN)L2]+ and
 trans-[M(H2)(CNH)L2]2+ where M&#x2005;=&#x2005;Fe, Ru, Os and
 L&#x2005;=&#x2005;dppm, dppe, dppp, depe, and dihydrogen substitution by
 the trifluoromethanesulfonate anion to give trans-[Ru(OTf&#x200A;)(CN)L2]
 or trans-[Ru(OTf&#x200A;)(CNH)L2]OTf&#x200A;&#x2020;
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4475
_journal_paper_doi               10.1039/a906717e
_journal_year                    1999
_chemical_formula_sum            'C54 H48 F3 N O3 P4 Ru S'
_chemical_formula_weight         1072.94
_chemical_name_systematic
; 
Ru(OSO2CF3)(CN)(dppe)2 
;
_space_group_IT_number           14
_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                 91.978(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6236(5)
_cell_length_b                   17.0227(6)
_cell_length_c                   18.0640(8)
_cell_measurement_temperature    150.0(1)
_cell_volume                     5108.7(3)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD server software (Nonius, 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'Bruker SHELXTL V5.1'
_computing_structure_solution    'Bruker SHELXTL V5.1'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.119
_diffrn_reflns_av_sigmaI/netI    0.8018
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20405
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.8839
_exptl_absorpt_correction_T_min  0.8370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN, (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'block cut from needle'
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         7243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                4314
_reflns_number_total             7243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906717esup1.cif
_cod_data_source_block           k98102
_cod_database_code               7027778