Redox Chemistry of (1,4,7-Tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7- triazacyclononane)ruthenium(III), [RuIIIL]: Synthesis and Characterization of [RuII2(L-L)](BPh4)4.10CH3CN and [LRuRuRuL](PF6)2.H2O
Belén Albela; Eberhard Bothe; Oliver Brosch; Katsura Mochizuki; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 38 (1999) 5131–5138; doi:10.1021/ic9906297

data_4322361
_publ_section_title
;
 Redox Chemistry of (1,4,7-Tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-
 triazacyclononane)ruthenium(III), [RuIIIL]: Synthesis and
 Characterization of [RuII2(L-L)](BPh4)4.10CH3CN and [LRuRuRuL](PF6)2.H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5131
_journal_page_last               5138
_journal_paper_doi               10.1021/ic9906297
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural     '[C78 H102 N6 Ru3 S6]2+, 2 (PF6), H2O'
_chemical_formula_sum            'C78 H110 F12 N6 O P2 Ru3 S6'
_chemical_formula_weight         1933.23
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.755(3)
_cell_length_b                   22.278(4)
_cell_length_c                   21.920(4)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.34
_cell_measurement_theta_min      7.60
_cell_volume                     9155(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       2\q/\w
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12351
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.728
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             3976
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         11761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.1708
_refine_ls_R_factor_obs          0.0842
_refine_ls_shift/esd_max         0.011
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+46.0822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2612
_refine_ls_wR_factor_obs         0.1999
_reflns_number_observed          6395
_reflns_number_total             11928
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9906297_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+46.0822P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+46.0822P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9154.7(28)
_cod_database_code               4322361