An unprecedented up-field shift in the (13)C NMR spectrum of the carboxyl carbons of the lantern-type dinuclear complex TBA[Ru2(O2CCH3)4Cl2] (TBA(+) = tetra(n-butyl)ammonium cation).
Hiraoka, Yuya; Ikeue, Takahisa; Sakiyama, Hiroshi; Guégan, Frédéric; Luneau, Dominique; Gillon, Béatrice; Hiromitsu, Ichiro; Yoshioka, Daisuke; Mikuriya, Masahiro; Kataoka, Yusuke; Handa, Makoto; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13439–13443; doi:10.1039/c5dt01680k

data_7035491
_publ_section_title
;
 An unprecedented up-field shift in the (13)C NMR spectrum of the carboxyl
 carbons of the lantern-type dinuclear complex TBA[Ru2(O2CCH3)4Cl2]
 (TBA(+) = tetra(n-butyl)ammonium cation).
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13439
_journal_page_last               13443
_journal_paper_doi               10.1039/c5dt01680k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C26 H52 Cl6 N O8 Ru2'
_chemical_formula_weight         921.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-05-29 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                76.860(2)
_cell_angle_beta                 82.601(2)
_cell_angle_gamma                86.546(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9262(14)
_cell_length_b                   12.4678(15)
_cell_length_c                   13.3115(16)
_cell_measurement_temperature    90(2)
_cell_volume                     1910.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
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_computing_publication_material  'Bruker SHELXL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.879
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_diffrn_reflns_limit_l_min       -10
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_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.879
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_diffrn_reflns_theta_max         28.309
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.7052
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0310
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.9300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7251
_reflns_number_total             8366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01680k2.cif
_cod_data_source_block           14A0037
_cod_depositor_comments          'Adding full bibliography for 7035491.cif.'
_cod_database_code               7035491
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.520
_shelx_estimated_absorpt_t_max   0.705
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