Electronic Structures of [RuII(cyclam)(Et2dtc)]+, [Ru(cyclam)(tdt)]+, and [Ru(cyclam)(tdt)]2+: An X-ray Absorption Spectroscopic and Computational Study (tdt = toluene-3,4-dithiolate; Et2dtc = N,N-diethyldithiocarbamate(1-))
Carsten Milsmann; Eckhard Bill; Thomas Weyhermüller; Serena DeBeer George; Karl Wieghardt; Inorganic Chemistry 48 (2009) 9754–9766; doi:10.1021/ic9011845

data_4303378
_publ_section_title
;
Electronic Structures of [RuII(cyclam)(Et2dtc)]+, [Ru(cyclam)(tdt)]+, and
[Ru(cyclam)(tdt)]2+: An X-ray Absorption Spectroscopic and Computational
Study (tdt = toluene-3,4-dithiolate; Et2dtc = N,N-diethyldithiocarbamate(1-))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9754
_journal_page_last               9766
_journal_paper_doi               10.1021/ic9011845
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C15 H34 N5 Ru S2, C24 H20 B, 0.16(C H2 CL2)'
_chemical_formula_sum            'C39.16 H54.31 B Cl0.31 N5 Ru S2'
_chemical_formula_weight         781.94
_chemical_name_systematic
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 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.305(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.669(3)
_cell_length_b                   12.777(2)
_cell_length_c                   17.816(3)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      3.19
_cell_volume                     3795.9(11)
_computing_cell_refinement       'Bruker SAINT 7.34a'
_computing_data_collection       'Bruker SAINT 7.34a'
_computing_data_reduction        'Bruker SAINT 7.34a'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method
'frames at 0.5 deg. stepwise rotation in omega and phi, 20 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, INCOTEC Multi-Layer-Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            107818
_diffrn_reflns_theta_full        31.14
_diffrn_reflns_theta_max         31.14
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.9942
_exptl_absorpt_correction_T_min  0.9772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker SADABS Vers. 2008/1, Bruker AXS (2008)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent triangular fragment'
_exptl_crystal_F_000             1642
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         12168
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.616
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0213P)^2^+10.9533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                9773
_reflns_number_total             12168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9011845_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4303378