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_4321793
_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]2+, 2 ClO4-, 5 CH3CN'
_chemical_formula_sum            'C88 H123 Cl2 Fe2 N11 Ni O8 S6'
_chemical_formula_weight         1896.64
_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                114.47(3)
_cell_angle_beta                 97.67(3)
_cell_angle_gamma                90.34(3)
_cell_formula_units_Z            1
_cell_length_a                   13.065(2)
_cell_length_b                   13.626(3)
_cell_length_c                   14.043(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      15.80
_cell_volume                     2249.9(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       2\q/\w-scan
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10623
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        'not observed'
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   'not measured'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       'opaque block '
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         10205
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_obs          0.0545
_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^)+(0.0326P)^2^+7.7126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1506
_refine_ls_wR_factor_obs         0.1402
_reflns_number_observed          8136
_reflns_number_total             10205
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9811289_1.cif
_cod_data_source_block           1*
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+7.7126P] 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^)+(0.0326P)^2^+7.7126P] 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        2249.9(9)
_cod_database_code               4321793