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_4322055
_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 Ge N12 S6]2+, 2 (C24H20B)-, 6 MeCN'
_chemical_formula_sum            'C138 H166 B2 Fe2 Ge N12 S6'
_chemical_formula_weight         2391.10
_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                100.06(2)
_cell_angle_beta                 112.15(2)
_cell_angle_gamma                112.01(2)
_cell_formula_units_Z            1
_cell_length_a                   13.531(1)
_cell_length_b                   16.578(2)
_cell_length_c                   17.199(2)
_cell_measurement_reflns_used    2866
_cell_measurement_temperature    100(2)
_cell_volume                     3080.4(12)
_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      100(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  0.0896
_diffrn_reflns_av_sigmaI/netI    0.1584
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22503
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   'not measured'
_exptl_crystal_colour            'red almost black'
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         9759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.1612
_refine_ls_R_factor_obs          0.0792
_refine_ls_shift/esd_max         -0.239
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+11.7752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1896
_refine_ls_wR_factor_obs         0.1366
_reflns_number_observed          5528
_reflns_number_total             9769
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9902018_3.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+11.7752P] 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^)+(0.0245P)^2^+11.7752P] 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        3080.3(5)
_cod_database_code               4322055