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_4322360
_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_sum            'C194 H218 B4 N16 Ru2 S6'
_chemical_formula_weight         3211.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.35(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.734(5)
_cell_length_b                   16.347(3)
_cell_length_c                   37.986(7)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    100(2)
_cell_volume                     17430(6)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens ShelXTL'
_computing_publication_material  'Siemens ShelXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w, 0.3 deg./frame'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -59
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_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.8881
_exptl_absorpt_correction_T_min  0.7342
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick 1994'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6792
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.109
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         23892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_restrained_S_obs      1.149
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_obs          0.0458
_refine_ls_shift/esd_max         0.131
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+40.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1047
_refine_ls_wR_factor_obs         0.0965
_reflns_number_observed          20557
_reflns_number_total             25119
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9906297_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+40.3504P] 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^)+(0.0277P)^2^+40.3504P] 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        17429.7(55)
_cod_database_code               4322360