Dodeca-μ~2~-hydroxo-di-μ~3~-oxo-hexakis(1,4,7-triazacyclononane-κ^3^<i>N</i>,<i>N</i>',<i>N</i>'')octairon(III) octabromide octahydrate
Mata, Ignasi; Rodríguez, E.; Molins, Elies; Acta Crystallographica Section E 61 (2005) m1988–m1990; doi:10.1107/S1600536805028436

data_2206951
_publ_section_title
;Dodeca-\m~2~-hydroxo-di-\m~3~-oxo-hexakis(1,4,7-triazacyclononane-\k^3^<i>N</i>,<i>N</i>',<i>N</i>'')octairon(III)
 octabromide octahydrate
;
_journal_coeditor_code           HB6243
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1988
_journal_page_last               m1990
_journal_paper_doi               10.1107/S1600536805028436
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe8 O2 (O H)12 (C6 H12 N3)6] Br8, 8H2 O'
_chemical_formula_moiety         'C36 H118 Br8 Fe8 N18 O22'
_chemical_formula_sum            'C36 H118 Br8 Fe8 N18 O22'
_chemical_formula_weight         2241.56
_chemical_name_systematic
;
dodeca-\m~2~-hydroxo-di-\m~3~-oxo-hexakis(1,4,7-triazacyclononane-
\k^3^N,N',N'')octairon(III) octabromide octahydrate
;
_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.150(10)
_cell_angle_beta                 113.340(10)
_cell_angle_gamma                101.430(10)
_cell_formula_units_Z            1
_cell_length_a                   13.257(2)
_cell_length_b                   13.5640(10)
_cell_length_c                   14.831(4)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.6
_cell_measurement_theta_min      10.8
_cell_volume                     2163.0(8)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w/2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13602
_diffrn_reflns_theta_full        30.41
_diffrn_reflns_theta_max         30.41
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 90
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.061
_exptl_absorpt_correction_T_max  0.241
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.528
_refine_diff_density_min         -1.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         13085
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.116P)^2^+2.3967P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.2094
_reflns_number_gt                8217
_reflns_number_total             13085
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6243.cif
_cod_data_source_block           I
_cod_database_code               2206951
_cod_database_fobs_code          2206951