Spin-Dependent Delocalization in Three Isostructural Complexes [LFeNiFeL]2+/3+/4+ (L = 1,4,7-(4-tert-Butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane)
Thorsten Glaser; Frank Kesting; Thomas Beissel; Eckhard Bill; Thomas Weyhermüller; Wolfram Meyer-Klaucke; Karl Wieghardt; Inorganic Chemistry 38 (1999) 722–732; doi:10.1021/ic9811289

data_4321794
_publ_section_title
;
 Spin-Dependent Delocalization in Three Isostructural Complexes
 [LFeNiFeL]2+/3+/4+ (L =
 1,4,7-(4-tert-Butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              722
_journal_page_last               732
_journal_paper_doi               10.1021/ic9811289
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural     '[C78 H108 Fe2 N6 Ni S6]3+, 3 ClO4-, 8 C3H6O'
_chemical_formula_sum            'C102 H156 Cl3 Fe2 N6 Ni O20 S6'
_chemical_formula_weight         2255.45
_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                114.20(2)
_cell_angle_beta                 96.57(2)
_cell_angle_gamma                98.86(2)
_cell_formula_units_Z            1
_cell_length_a                   13.155(2)
_cell_length_b                   14.747(2)
_cell_length_c                   16.237(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    100(2)
_cell_volume                     2783.2(10)
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26235
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       'opaque block '
_exptl_crystal_F_000             1197
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         12898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_obs          0.0517
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+5.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1397
_refine_ls_wR_factor_obs         0.1256
_reflns_number_observed          10970
_reflns_number_total             13609
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9811289_2.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^)+(0.0546P)^2^+5.3012P] 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^)+(0.0546P)^2^+5.3012P] 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        2783.2(8)
_cod_database_code               4321794