Citrate, in Collaboration with a Guanidinium Ion, as a Generator of Cubane-like Complexes with a Range of Metal Cations: Synthesis, Structures, and Magnetic Properties of [C(NH2)3]8[(MII)4(cit)4]·8H2O (M = Mg, Mn, Fe, Co, Ni, and Zn; cit = Citrate)
Hudson, Timothy A.; Berry, Kevin J.; Moubaraki, Boujemaa; Murray, Keith S.; Robson, Richard; Inorganic Chemistry 45 (2006) 3549–3556; doi:10.1021/ic051779m

data_4331889
_publ_section_title
;
 Citrate, in Collaboration with a Guanidinium Ion, as a Generator of
 Cubane-like Complexes with a Range of Metal Cations: Synthesis,
 Structures, and Magnetic Properties of
 [C(NH2)3]8[(MII)4(cit)4]&#x00B7;8H2O (M = Mg, Mn, Fe, Co, Ni, and Zn; cit
 = Citrate)
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3549
_journal_page_last               3556
_journal_paper_doi               10.1021/ic051779m
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
;
1(Fe 2+), 1(C6 O7 H4 4-), 2(C H6 N3 1+), 2(H2 o)
;
_chemical_formula_sum            'C8 H20 Fe N6 O9'
_chemical_formula_weight         400.15
_chemical_name_systematic        ?
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.2542(8)
_cell_length_b                   16.2542(8)
_cell_length_c                   11.5350(10)
_cell_measurement_reflns_used    3635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.2
_cell_volume                     3047.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18241
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, G. M.  SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+9.7284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1990
_refine_ls_wR_factor_ref         0.2098
_reflns_number_gt                2790
_reflns_number_total             3479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051779msup1.cif
_cod_data_source_block           fecitrate
_cod_depositor_comments
;
The following automatic conversions were performed:
'__computing_data_collection' tag replaced with
'_computing_data_collection'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      P42/n
_cod_database_code               4331889