Tuning the Electronic Structure of Octahedral Iron Complexes [FeL(X)] (L=1-Alkyl-4,7-bis(4-tert-butyl-2-mercaptobenzyl)- 1,4,7-triazacyclononane, X = Cl, CH3O, CN, NO). The S=1/2 \λeftarrow →S=3/2 Spin Equilibrium of [FeLPr(NO)]
Ming Li; Didier Bonnet; Eckhard Bill; Frank Neese; Thomas Weyhermüller; Nicole Blum; Dieter Sellmann; Karl Wieghardt; Inorganic Chemistry 41 (2002) 3444–3456; doi:10.1021/ic011243a

data_4318136
_publ_section_title
;
 Tuning the Electronic Structure of Octahedral Iron Complexes [FeL(X)]
 (L=1-Alkyl-4,7-bis(4-tert-butyl-2-mercaptobenzyl)-
 1,4,7-triazacyclononane, X = Cl, CH3O, CN, NO). The S=1/2 \\leftarrow
 \\rightarrow S=3/2 Spin Equilibrium of [FeLPr(NO)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3444
_journal_page_last               3456
_journal_paper_doi               10.1021/ic011243a
_journal_volume                  41
_journal_year                    2002
_chemical_formula_analytical     '[C31 H47 Fe N4 O S2], 2.5 CH2Cl2'
_chemical_formula_sum            'C33.5 H52 Cl5 Fe N4 O S2'
_chemical_formula_weight         824.01
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.72(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3331(8)
_cell_length_b                   17.6575(8)
_cell_length_c                   14.9283(8)
_cell_measurement_reflns_used    39226
_cell_measurement_temperature    100(2)
_cell_volume                     3957.5(4)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa CCD-Detector'
_diffrn_measurement_method       '\w-scan,129 images a 1.0 deg., 90 sec.'
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39539
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.879
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         11486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_obs          0.0580
_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^)+(0.0634P)^2^+5.0664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1588
_refine_ls_wR_factor_obs         0.1384
_reflns_number_observed          7802
_reflns_number_total             11507
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011243a_4.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+5.0664P] 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^)+(0.0634P)^2^+5.0664P] 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        3957.5(3)
_cod_original_formula_sum        'C33.50 H52 Cl5 Fe N4 O S2'
_cod_database_code               4318136