140 H/D Isotopomers Identified by Long-Range NMR Hyperfine Shifts in Ruthenium(III) Ammine Complexes. Hyperconjugation in Ru-NH3 Bonding
W. Michael Laidlaw; Robert G. Denning; Jennifer C. Green; Jonathan Boyd; Jeffrey Harmer; Amber L. Thompson; Inorganic Chemistry 52 (2013) 7280–7294; doi:10.1021/ic400903a

data_4335260
_publ_contact_author             'Robert G. Denning'
_publ_contact_author_email       Bob.Denning@chem.ox.ac.uk
_publ_section_title
;
 140 H/D Isotopomers Identified by Long-Range NMR Hyperfine Shifts in
 Ruthenium(III) Ammine Complexes. Hyperconjugation in Ru-NH3 Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7280
_journal_page_last               7294
_journal_paper_doi               10.1021/ic400903a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C8 H20 Fe N6 O2 Ru, 3(C F3 O3 S), 3(H2 O)'
_chemical_formula_sum            'C11 H26 F9 Fe N6 O14 Ru S3'
_chemical_formula_weight         890.46
_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
_audit_creation_date             09-11-10
_audit_creation_method           CRYSTALS_ver_12.90
_cell_angle_alpha                96.5999(7)
_cell_angle_beta                 91.5260(7)
_cell_angle_gamma                91.9869(9)
_cell_formula_units_Z            2
_cell_length_a                   7.9846(1)
_cell_length_b                   13.3099(2)
_cell_length_c                   14.6247(3)
_cell_measurement_reflns_used    6721
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1542.27(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27540
_diffrn_reflns_theta_full        26.952
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         5.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_orange
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       plate
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9989
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7029
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.0007148
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 18.7 28.1 13.7 3.61 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0939
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0939
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6124
_reflns_number_total             7029
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.66
_oxford_diffrn_Wilson_scale      13.04
_oxford_refine_ls_r_factor_ref   0.0434
_oxford_refine_ls_scale          0.2880(2)
_oxford_reflns_number_all        7029
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 6159
_cod_data_source_file            ic400903a_si_002.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C11 H26 F9 Fe1 N6 O14 Ru1 S3'
_cod_database_code               4335260