μ-Sulfato-1κ<i>O</i>:2κ<i>O</i>-μ-oxo-bis[tris(2-pyridylmethyl)amine-κ^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''']diiron(III) diperchlorate acetonitrile/water (0.75/0.25) solvate
Smith, Christine M.; Norman, Richard E.; Acta Crystallographica Section E 63 (2007) m2480–m2481; doi:10.1107/S1600536807042857

data_2215561
_publ_section_title
;\m-Sulfato-1\k<i>O</i>:2\k<i>O</i>-\m-oxo-bis[tris(2-pyridylmethyl)amine-\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''']diiron(III)
 diperchlorate acetonitrile/water (0.75/0.25) solvate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2480
_journal_page_last               m2481
_journal_paper_doi               10.1107/S1600536807042857
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Fe2 (C18 H18 N4)2 O (S O4)]4 (Cl O4)8, 3C2 H3 N, H2 O'
_chemical_formula_moiety
'4(C36 H36 Fe2 N8 O5 S), 8(Cl O4), 3(C2 H3 N), H2 O'
_chemical_formula_sum            'C150 H155 Cl8 Fe8 N35 O53 S4'
_chemical_formula_weight         4154.72
_chemical_name_systematic
;\m-Sulfato-1\k<i>O</i>:2\k<i>O</i>-\m-oxo-bis[tris(2-pyridylmethyl)amine-\k^4^
<i>N</i>,<i>N</i>',<i>N</i>",<i>N</i>'"]diiron(III)
 diperchlorate
acetonitrile/water (0.75/0.25) solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 103.357(5)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   12.7031(10)
_cell_length_b                   24.477(3)
_cell_length_c                   13.6165(11)
_cell_measurement_reflns_used    14215
_cell_measurement_temperature    90
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.5
_cell_volume                     4119.3(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
'teXsan for Windows (Molecular Structure Corporation, 1999'
_computing_structure_refinement
'teXsan for Windows (Molecular Structure Corporation, 1999)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.04160
_diffrn_reflns_av_sigmaI/netI    0.089
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81911
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        32.0
_diffrn_reflns_theta_max         32.0
_diffrn_reflns_theta_min         2.5
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'<i>HKL SCALEPACK</i> (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       lath
_exptl_crystal_F_000             2132.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.713
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.9022
_refine_ls_goodness_of_fit_ref   1.0195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.000841|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1103
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                8172
_reflns_number_total             14279
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            is2197.cif
_cod_data_source_block           I
_cod_original_cell_volume        4119.3(6)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C150 H155 Cl8 Fe8 N35 O53 S4 '
_cod_database_code               2215561
_cod_database_fobs_code          2215561