Synthesis, Structure, and Characterization of the New [L(OH)Fe(μ-O)Fe(OH2)L]3+ Complex (L = N,N'-Dimethyl-N,N'-bis(2-pyridylmethyl)ethane-1,2-diamine). Detection of an Equilibrium with the Protonated Diamond Form [LFe(μ-O)(μ-OH)FeL]3+ in Acetonitrile
Sandrine Poussereau; Geneviève Blondin; Michèle Cesario; Jean Guilhem; Geneviève Chottard; Florence Gonnet; Jean-Jacques Girerd; Inorganic Chemistry 37 (1998) 3127–3132; doi:10.1021/ic971589e

data_4322863
_publ_section_title
;
 Synthesis, Structure, and Characterization of the New
 [L(OH)Fe(\m-O)Fe(OH2)L]3+ Complex (L =
 N,N'-Dimethyl-N,N'-bis(2-pyridylmethyl)ethane-1,2-diamine). Detection of
 an Equilibrium with the Protonated Diamond Form [LFe(\m-O)(\m-OH)FeL]3+
 in Acetonitrile
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3127
_journal_page_last               3132
_journal_paper_doi               10.1021/ic971589e
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C32 H49 Cl3 Fe2 N8 O16'
_chemical_formula_weight         1019.84
_chemical_name_common
{[(BispicMe2en)Fe]2(OH)(mu-O)(H2O),(ClO4)3,(H2O)
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.283(5)
_cell_length_b                   16.050(9)
_cell_length_c                   20.996(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      9.5
_cell_measurement_theta_min      7.8
_cell_volume                     4476(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Nonius CAD4 diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6900
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.94
_diffrn_standards_interval_time  166
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow-grey
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         6894
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_obs          0.0566
_refine_ls_shift/esd_max         0.724
_refine_ls_shift/esd_mean        0.063
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0895P)^2^+2.2313P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1842
_refine_ls_wR_factor_obs         0.1414
_reflns_number_observed          3783
_reflns_number_total             6900
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971589e.cif
_cod_data_source_block           blan
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0895P)^2^+2.2313P] where P=3D(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=3D1/[\s^2^(Fo^2^)+(0.0895P)^2^+2.2313P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4476.2
_cod_database_code               4322863