#------------------------------------------------------------------------------
#$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/[σ²(Fo²)+(0.0693P)²+4.0458P] where P=(Fo²+2Fc²)/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_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
