#------------------------------------------------------------------------------
#$Date: 2016-12-18 19:17:40 +0200 (Sun, 18 Dec 2016) $
#$Revision: 189196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/18/4331893.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_4331893
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(Zn 2+), 1(C6 H4 O7 4-), 2(C H6 N3 1+), 2(H2 O)
;
_chemical_formula_sum            'C8 H20 N6 O9 Zn'
_chemical_formula_weight         409.67
_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                   16.1337(5)
_cell_length_b                   16.1337(5)
_cell_length_c                   11.6460(7)
_cell_measurement_reflns_used    7189
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.2
_cell_volume                     3031.4(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18480
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.682
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, G. M.  SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0693P)^2^+4.0458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                2990
_reflns_number_total             3466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051779msup1.cif
_cod_data_source_block           zncitrate
_cod_original_sg_symbol_H-M      P42/n
_cod_database_code               4331893
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 0.39899(18) 0.31219(19) 0.1052(3) 0.0361(6) Uani 1 1 d . 0
C3 C 0.3884(2) 0.40389(19) 0.0707(3) 0.0407(7) Uani 1 1 d . 0
H7 H 0.3713 0.4361 0.1369 0.032(8) Uiso 1 1 calc R 0
H8 H 0.4409 0.4258 0.0436 0.059(12) Uiso 1 1 calc R 0
C4 C 0.3234(2) 0.4110(2) -0.0239(3) 0.0461(8) Uani 1 1 d . 0
C2 C 0.4784(2) 0.3090(2) 0.1854(3) 0.0388(7) Uani 1 1 d . 0
C5 C 0.4145(2) 0.25949(19) -0.0026(3) 0.0396(7) Uani 1 1 d . 0
H9 H 0.3627 0.2508 -0.0430 0.046(10) Uiso 1 1 calc R 0
H10 H 0.4521 0.2886 -0.0536 0.047(10) Uiso 1 1 calc R 0
C8 C 0.9113(2) 0.5152(2) 0.1499(3) 0.0444(8) Uani 1 1 d . 0
C7 C 0.3236(2) 0.6553(2) 0.1401(3) 0.0445(8) Uani 1 1 d . 0
C6 C 0.4513(2) 0.17713(19) 0.0297(3) 0.0437(7) Uani 1 1 d . 0
O5 O 0.34540(19) 0.43864(19) -0.1190(2) 0.0626(8) Uani 1 1 d . 0
O4 O 0.24953(14) 0.38888(15) -0.00187(19) 0.0422(5) Uani 1 1 d . 0
O1 O 0.32748(12) 0.28483(12) 0.16494(17) 0.0291(4) Uani 1 1 d . 0
O2 O 0.46654(13) 0.29150(14) 0.28829(19) 0.0394(5) Uani 1 1 d . 0
O3 O 0.54751(16) 0.3201(2) 0.1411(2) 0.0587(7) Uani 1 1 d . 0
O6 O 0.41309(14) 0.13429(13) 0.1070(2) 0.0420(5) Uani 1 1 d . 0
O8 O 0.30604(19) 0.5953(2) -0.1849(3) 0.0673(8) Uani 1 1 d . 2
O7 O 0.51574(17) 0.15432(17) -0.0195(3) 0.0707(9) Uani 1 1 d . 0
N1 N 0.8925(2) 0.47920(19) 0.0525(3) 0.0512(7) Uani 1 1 d . 0
H1A H 0.8500 0.4955 0.0140 0.072(14) Uiso 1 1 calc R 0
H1B H 0.9227 0.4393 0.0270 0.043(10) Uiso 1 1 calc R 0
N2 N 0.9753(2) 0.4896(2) 0.2115(3) 0.0577(8) Uani 1 1 d . 0
H2A H 1.0052 0.4489 0.1877 0.061(13) Uiso 1 1 calc R 0
H2B H 0.9871 0.5137 0.2754 0.058(12) Uiso 1 1 calc R 0
N3 N 0.8646(2) 0.5765(2) 0.1886(3) 0.0590(8) Uani 1 1 d . 0
H3A H 0.8222 0.5925 0.1498 0.069(14) Uiso 1 1 calc R 0
H3B H 0.8767 0.6003 0.2525 0.077(16) Uiso 1 1 calc R 0
N4 N 0.3717(2) 0.7104(2) 0.0891(3) 0.0628(9) Uani 1 1 d . 0
H4A H 0.3949 0.7489 0.1289 0.067(14) Uiso 1 1 calc R 0
H4B H 0.3797 0.7078 0.0162 0.066(14) Uiso 1 1 calc R 0
N5 N 0.3116(2) 0.6596(2) 0.2507(3) 0.0559(8) Uani 1 1 d . 0
H5A H 0.2798 0.6243 0.2841 0.069(14) Uiso 1 1 calc R 0
H5B H 0.3355 0.6978 0.2902 0.068(13) Uiso 1 1 calc R 0
N6 N 0.2868(2) 0.5967(2) 0.0804(3) 0.0583(8) Uani 1 1 d . 0
H6A H 0.2551 0.5616 0.1143 0.051(11) Uiso 1 1 calc R 0
H6B H 0.2945 0.5936 0.0074 0.067(14) Uiso 1 1 calc R 0
Zn1 Zn 0.20847(2) 0.34233(2) 0.15532(3) 0.03085(14) Uani 1 1 d . 0
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0311(14) 0.0379(15) 0.0394(16) 0.0074(12) 0.0058(12) 0.0049(11)
C3 0.0426(16) 0.0329(15) 0.0465(18) 0.0023(13) 0.0031(14) 0.0002(12)
C4 0.053(2) 0.0471(18) 0.0385(17) 0.0044(14) 0.0024(14) 0.0194(15)
C2 0.0390(16) 0.0371(15) 0.0402(16) 0.0048(13) 0.0039(13) 0.0074(12)
C5 0.0396(16) 0.0351(15) 0.0442(17) 0.0000(13) 0.0061(13) 0.0026(12)
C8 0.0425(17) 0.0454(18) 0.0453(18) 0.0073(14) -0.0079(13) 0.0020(14)
C7 0.0409(17) 0.0385(17) 0.054(2) 0.0056(14) 0.0058(14) -0.0022(13)
C6 0.0365(16) 0.0330(15) 0.062(2) 0.0014(14) 0.0025(14) 0.0002(12)
O5 0.0710(18) 0.0752(19) 0.0415(13) 0.0191(13) 0.0175(13) 0.0219(15)
O4 0.0402(12) 0.0520(13) 0.0346(11) 0.0070(9) -0.0027(9) 0.0101(10)
O1 0.0254(9) 0.0287(9) 0.0333(11) 0.0030(7) 0.0042(7) 0.0009(7)
O2 0.0303(10) 0.0520(13) 0.0358(11) 0.0059(9) -0.0025(8) 0.0025(9)
O3 0.0403(13) 0.080(2) 0.0553(15) 0.0131(13) 0.0070(11) -0.0055(13)
O6 0.0389(11) 0.0296(10) 0.0575(14) 0.0045(10) 0.0078(10) 0.0047(9)
O8 0.0541(16) 0.0672(18) 0.081(2) 0.0065(16) -0.0087(15) 0.0100(14)
O7 0.0494(15) 0.0512(15) 0.111(3) 0.0171(16) 0.0330(16) 0.0098(12)
N1 0.0543(17) 0.0464(16) 0.0529(17) -0.0037(13) -0.0156(14) 0.0081(14)
N2 0.0567(19) 0.060(2) 0.056(2) 0.0000(16) -0.0199(15) 0.0130(16)
N3 0.0524(18) 0.071(2) 0.0537(18) -0.0117(16) -0.0149(15) 0.0182(16)
N4 0.064(2) 0.0544(19) 0.070(2) 0.0030(17) 0.0162(17) -0.0179(16)
N5 0.0572(19) 0.0516(18) 0.059(2) -0.0079(15) 0.0117(15) -0.0139(15)
N6 0.077(2) 0.0487(17) 0.0497(19) 0.0041(14) 0.0021(16) -0.0208(16)
Zn1 0.0320(2) 0.02694(19) 0.0337(2) 0.00207(12) -0.00042(12) 0.00376(11)
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'
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'
Zn Zn 0.2839 1.4301 '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 C5 111.2(3) . .
O1 C1 C3 109.7(2) . .
C5 C1 C3 109.7(3) . .
O1 C1 C2 110.9(2) . .
C5 C1 C2 109.4(2) . .
C3 C1 C2 105.9(3) . .
C4 C3 C1 109.7(3) . .
O5 C4 O4 123.3(3) . .
O5 C4 C3 118.2(3) . .
O4 C4 C3 118.5(3) . .
O3 C2 O2 124.7(3) . .
O3 C2 C1 118.4(3) . .
O2 C2 C1 116.8(3) . .
C6 C5 C1 110.5(3) . .
N1 C8 N3 119.7(3) . .
N1 C8 N2 120.8(3) . .
N3 C8 N2 119.5(3) . .
N5 C7 N6 119.6(3) . .
N5 C7 N4 119.7(4) . .
N6 C7 N4 120.8(4) . .
O7 C6 O6 124.2(3) . .
O7 C6 C5 118.5(3) . .
O6 C6 C5 117.3(3) . .
C4 O4 Zn1 125.2(2) . .
C1 O1 Zn1 112.26(17) . 7_566
C1 O1 Zn1 119.63(17) . 2
Zn1 O1 Zn1 97.59(8) 7_566 2
C1 O1 Zn1 124.79(16) . .
Zn1 O1 Zn1 97.58(8) 7_566 .
Zn1 O1 Zn1 99.82(8) 2 .
C2 O2 Zn1 116.43(19) . 7_566
C6 O6 Zn1 122.9(2) . 2
O6 Zn1 O4 89.81(9) 2 .
O6 Zn1 O2 84.95(9) 2 8_656
O4 Zn1 O2 86.05(9) . 8_656
O6 Zn1 O1 109.76(9) 2 8_656
O4 Zn1 O1 153.52(8) . 8_656
O2 Zn1 O1 78.40(8) 8_656 8_656
O6 Zn1 O1 86.11(8) 2 2
O4 Zn1 O1 118.56(9) . 2
O2 Zn1 O1 153.75(8) 8_656 2
O1 Zn1 O1 81.53(8) 8_656 2
O6 Zn1 O1 160.58(8) 2 .
O4 Zn1 O1 85.24(8) . .
O2 Zn1 O1 113.35(8) 8_656 .
O1 Zn1 O1 81.52(8) 8_656 .
O1 Zn1 O1 79.86(8) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.418(3) .
C1 C5 1.536(4) .
C1 C3 1.542(4) .
C1 C2 1.586(4) .
C3 C4 1.526(5) .
C4 O5 1.245(4) .
C4 O4 1.270(4) .
C2 O3 1.242(4) .
C2 O2 1.245(4) .
C5 C6 1.503(4) .
C8 N1 1.310(5) .
C8 N3 1.322(5) .
C8 N2 1.324(4) .
C7 N5 1.305(5) .
C7 N6 1.314(5) .
C7 N4 1.320(4) .
C6 O7 1.243(4) .
C6 O6 1.292(4) .
O4 Zn1 2.087(2) .
O1 Zn1 2.110(2) 7_566
O1 Zn1 2.1350(19) 2
O1 Zn1 2.1354(19) .
O2 Zn1 2.109(2) 7_566
O6 Zn1 2.075(2) 2
Zn1 O6 2.075(2) 2
Zn1 O2 2.109(2) 8_656
Zn1 O1 2.110(2) 8_656
Zn1 O1 2.1350(19) 2