Proof of Large Positive Zero-Field Splitting in a Ru25+ Paddlewheel
Wei-Zhong Chen; F. Albert Cotton; Naresh S. Dalal; Carlos A. Murillo; Chris M. Ramsey; Tong Ren; Xiaoping Wang; Journal of the American Chemical Society 127 (2005) 12691–12696; doi:10.1021/ja053615a

data_4111900
_publ_section_title
;
 Proof of Large Positive Zero-Field Splitting in a Ru25+ Paddlewheel
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12691
_journal_page_last               12696
_journal_paper_doi               10.1021/ja053615a
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C52 H28 N8 Cl17 Ru2, 0.5(H2O), C6 H14 '
_chemical_formula_sum            'C58 H43 Cl17 N8 O0.5 Ru2'
_chemical_formula_weight         1664.79
_chemical_name_systematic
; 
Tetrakis(N,N'-di(3,5-diclorophenyl)formamidinato) chloro 
diruthenium(II,III) 0.5water hexanes solvate

;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :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            4
_cell_length_a                   15.5980(11)
_cell_length_b                   15.5980(11)
_cell_length_c                   27.063(4)
_cell_measurement_reflns_used    5887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.386
_cell_volume                     6584.4(12)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31871
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.7874
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.632
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2928
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0706
_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^)+(0.0941P)^2^+34.6070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.1959
_reflns_number_gt                2458
_reflns_number_total             2928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja053615asi20050602_113034_2.cif
_cod_data_source_block           100k
_cod_original_cell_volume        6584.5(11)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'C58 H43 Cl17 N8 O0.50 Ru2'
_cod_database_code               4111900