#------------------------------------------------------------------------------
#$Date: 2016-12-18 19:17:40 +0200 (Sun, 18 Dec 2016) $
#$Revision: 189196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/18/4331889.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4331889
loop_
_publ_author_name
'Hudson, Timothy A.'
'Berry, Kevin J.'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Robson, Richard'
_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]·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/[σ²(Fo²)+(0.0889P)²+9.7284P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_attached_hydrogens
C1 C 0.3123(4) 0.0987(3) 0.8975(5) 0.0490(14) Uani 1 1 d . 0
C3 C 0.2611(3) 0.0836(4) 1.0050(6) 0.0503(14) Uani 1 1 d . 0
H7 H 0.2897 0.0460 1.0564 0.064(19) Uiso 1 1 calc R 0
H8 H 0.2525 0.1350 1.0460 0.029(12) Uiso 1 1 calc R 0
C4 C 0.1799(3) 0.0476(4) 0.9706(6) 0.0520(14) Uani 1 1 d . 0
C5 C 0.4039(4) 0.1085(4) 0.9307(6) 0.0540(15) Uani 1 1 d . 0
H9 H 0.4355 0.1257 0.8636 0.08(2) Uiso 1 1 calc R 0
H10 H 0.4257 0.0564 0.9578 0.11(3) Uiso 1 1 calc R 0
C6 C 0.4102(4) 0.1740(4) 1.0278(5) 0.0599(17) Uani 1 1 d . 0
C2 C 0.3115(3) 0.0181(4) 0.8135(5) 0.0464(13) Uani 1 1 d . 0
C7 C 0.4876(4) 0.4117(3) 0.1439(5) 0.0455(13) Uani 1 1 d . 0
C8 C 0.6757(3) 0.3460(3) 0.3604(5) 0.0453(13) Uani 1 1 d . 0
Fe1 Fe 0.34220(4) 0.29017(4) 0.84531(6) 0.0328(2) Uani 1 1 d . 0
O1 O 0.28506(19) 0.17144(19) 0.8375(3) 0.0340(7) Uani 1 1 d . 0
O7 O 0.1575(3) -0.0166(3) 1.0196(6) 0.0863(18) Uani 1 1 d . 0
O6 O 0.1363(2) 0.0868(2) 0.8942(4) 0.0440(9) Uani 1 1 d . 0
O5 O 0.4377(3) 0.1509(3) 1.1227(4) 0.0676(14) Uani 1 1 d . 0
O4 O 0.3899(2) 0.2469(2) 1.0042(3) 0.0432(9) Uani 1 1 d . 0
O2 O 0.2930(2) 0.0329(2) 0.7110(3) 0.0400(8) Uani 1 1 d . 0
O3 O 0.3201(3) -0.0508(3) 0.8557(4) 0.0718(14) Uani 1 1 d . 0
O8 O 0.5925(3) 0.1951(3) 1.1863(5) 0.0751(14) Uani 1 1 d . 2
N1 N 0.4262(4) 0.3657(3) 0.1824(5) 0.0593(14) Uani 1 1 d . 0
H1A H 0.4097 0.3241 0.1427 0.07(2) Uiso 1 1 calc R 0
H1B H 0.4028 0.3775 0.2472 0.08(3) Uiso 1 1 calc R 0
N2 N 0.5124(3) 0.4746(3) 0.2076(5) 0.0590(14) Uani 1 1 d . 0
H2A H 0.5526 0.5047 0.1845 0.06(2) Uiso 1 1 calc R 0
H2B H 0.4882 0.4854 0.2721 0.07(2) Uiso 1 1 calc R 0
N3 N 0.5229(3) 0.3940(3) 0.0462(4) 0.0534(12) Uani 1 1 d . 0
H3A H 0.5633 0.4234 0.0217 0.043(16) Uiso 1 1 calc R 0
H3B H 0.5060 0.3528 0.0059 0.056(18) Uiso 1 1 calc R 0
N4 N 0.6280(3) 0.2917(4) 0.4134(6) 0.0670(16) Uani 1 1 d . 0
H4A H 0.6203 0.2950 0.4871 0.10(3) Uiso 1 1 calc R 0
H4B H 0.6046 0.2532 0.3743 0.06(2) Uiso 1 1 calc R 0
N5 N 0.7116(4) 0.4050(3) 0.4191(5) 0.0626(15) Uani 1 1 d . 0
H5A H 0.7428 0.4397 0.3840 0.07(2) Uiso 1 1 calc R 0
H5B H 0.7040 0.4089 0.4927 0.07(2) Uiso 1 1 calc R 0
N6 N 0.6874(3) 0.3401(3) 0.2482(5) 0.0592(14) Uani 1 1 d . 0
H6A H 0.7186 0.3750 0.2133 0.036(14) Uiso 1 1 calc R 0
H6B H 0.6639 0.3015 0.2095 0.07(2) Uiso 1 1 calc R 0
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 C1 C3 111.0(5) . .
O1 C1 C5 109.4(4) . .
C3 C1 C5 110.1(5) . .
O1 C1 C2 111.8(4) . .
C3 C1 C2 110.6(4) . .
C5 C1 C2 103.8(5) . .
C4 C3 C1 109.3(5) . .
O7 C4 O6 124.2(5) . .
O7 C4 C3 117.7(6) . .
O6 C4 C3 118.0(5) . .
C1 C5 C6 108.3(5) . .
O5 C6 O4 124.7(6) . .
O5 C6 C5 117.0(6) . .
O4 C6 C5 118.2(5) . .
O3 C2 O2 125.5(6) . .
O3 C2 C1 119.8(5) . .
O2 C2 C1 114.3(5) . .
N3 C7 N2 121.3(6) . .
N3 C7 N1 120.0(5) . .
N2 C7 N1 118.7(6) . .
N5 C8 N6 119.9(5) . .
N5 C8 N4 120.6(6) . .
N6 C8 N4 119.5(6) . .
O6 Fe1 O4 91.30(15) 2 .
O6 Fe1 O1 108.70(15) 2 8_657
O4 Fe1 O1 152.65(14) . 8_657
O6 Fe1 O2 84.44(14) 2 8_657
O4 Fe1 O2 85.51(14) . 8_657
O1 Fe1 O2 78.33(13) 8_657 8_657
O6 Fe1 O1 159.64(14) 2 .
O4 Fe1 O1 84.02(13) . .
O1 Fe1 O1 82.98(13) 8_657 .
O2 Fe1 O1 114.80(14) 8_657 .
O6 Fe1 O1 84.02(12) 2 2
O4 Fe1 O1 118.94(14) . 2
O1 Fe1 O1 82.53(13) 8_657 2
O2 Fe1 O1 153.12(13) 8_657 2
O1 Fe1 O1 81.00(13) . 2
C1 O1 Fe1 112.3(3) . 7_567
C1 O1 Fe1 125.9(3) . .
Fe1 O1 Fe1 96.83(13) 7_567 .
C1 O1 Fe1 120.8(3) . 2
Fe1 O1 Fe1 96.25(13) 7_567 2
Fe1 O1 Fe1 98.80(13) . 2
C4 O6 Fe1 123.9(3) . 2
C6 O4 Fe1 126.7(4) . .
C2 O2 Fe1 118.6(3) . 7_567
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.439(6) .
C1 C3 1.514(8) .
C1 C5 1.545(8) .
C1 C2 1.629(8) .
C3 C4 1.497(8) .
C4 O7 1.242(8) .
C4 O6 1.297(7) .
C5 C6 1.549(9) .
C6 O5 1.241(7) .
C6 O4 1.260(8) .
C2 O3 1.229(7) .
C2 O2 1.243(7) .
C7 N3 1.297(7) .
C7 N2 1.322(7) .
C7 N1 1.324(8) .
C8 N5 1.311(8) .
C8 N6 1.311(8) .
C8 N4 1.325(7) .
Fe1 O6 2.107(4) 2
Fe1 O4 2.110(4) .
Fe1 O1 2.122(4) 8_657
Fe1 O2 2.131(3) 8_657
Fe1 O1 2.144(3) .
Fe1 O1 2.163(3) 2
O1 Fe1 2.122(4) 7_567
O1 Fe1 2.163(3) 2
O6 Fe1 2.107(4) 2
O2 Fe1 2.131(3) 7_567
