Sn(III) and Ge(III) in the Thiophenolato-Bridged Complexes [LFeSnFeL]n+ and [LFeGeFeL]n+ (n = 2, 3; L = 1,4,7-(4-tert-Butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane)
Thorsten Glaser; Eckhard Bill; Thomas Weyhermüller; Wolfram Meyer-Klaucke; Karl Wieghardt; Inorganic Chemistry 38 (1999) 2632–2642; doi:10.1021/ic9902018

data_4322054
_publ_section_title
;
 Sn(III) and Ge(III) in the Thiophenolato-Bridged Complexes [LFeSnFeL]n+
 and [LFeGeFeL]n+ (n = 2, 3; L =
 1,4,7-(4-tert-Butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2632
_journal_page_last               2642
_journal_paper_doi               10.1021/ic9902018
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural
'[C78 H108 Fe2 N6 S6 Sn]3+, 3 (ClO4)3-, 4.5 C3H6O'
_chemical_formula_sum            'C91.5 H135 Cl3 Fe2 N6 O16.5 S6 Sn'
_chemical_formula_weight         2112.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                72.95(2)
_cell_angle_beta                 79.09(2)
_cell_angle_gamma                68.50(2)
_cell_formula_units_Z            2
_cell_length_a                   15.772(2)
_cell_length_b                   17.527(2)
_cell_length_c                   20.096(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_volume                     4920.6(14)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan, 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  0.0902
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21356
_diffrn_reflns_theta_max         25.80
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   'SADABS, G. Sheldrick 1994'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             2214
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.012
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1134
_refine_ls_number_reflns         15798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_restrained_S_obs      1.012
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_obs          0.0558
_refine_ls_shift/esd_max         -0.013
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+31.2768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1536
_refine_ls_wR_factor_obs         0.1098
_reflns_number_observed          11261
_reflns_number_total             15809
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9902018_2.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+31.2768P] 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^)+(0.0093P)^2^+31.2768P] 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        4920.4(12)
_cod_database_code               4322054