#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:01:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179274 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319481.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319481
loop_
_publ_author_name
'M. Matzapetakis'
'M. Kourgiantakis'
'M. Dakanali'
'C. P. Raptopoulou'
'A. Terzis'
'A. Lakatos'
'T. Kiss'
'I. Banyai'
'L. Iordanidis'
'T. Mavromoustakos'
'A. Salifoglou'
_publ_section_title
;
 Synthesis, pH-Dependent Structural Characterization, and Solution
 Behavior of Aqueous Aluminum and Gallium Citrate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1734
_journal_page_last               1744
_journal_paper_doi               10.1021/ic000461l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_analytical     '(NH4)5{Al(C6H4O7)2}.2H2O '
_chemical_formula_sum            'C12 H32 Al N5 O16'
_chemical_formula_weight         529.41
_chemical_name_systematic
; 
 ? 
;
_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_creation_method           SHELXL
_cell_angle_alpha                90.96(1)
_cell_angle_beta                 105.72(1)
_cell_angle_gamma                119.74(1)
_cell_formula_units_Z            1
_cell_length_a                   9.638(5)
_cell_length_b                   9.715(5)
_cell_length_c                   7.237(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      6.8
_cell_volume                     557.0(5)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-2theta 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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3914
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      1.55
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         1957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_obs          0.0498
_refine_ls_shift/esd_max         0.830
_refine_ls_shift/esd_mean        0.068
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1126P)²+0.1155P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1640
_refine_ls_wR_factor_obs         0.1477
_reflns_number_observed          1494
_reflns_number_total             1957
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000461l_1.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1126P)^2^+0.1155P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1126P)^2^+0.1155P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        557.1(3)
_cod_database_code               4319481
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Al Al 0.0000 0.0000 0.0000 0.0189(3) Uani 1 d S .
O1 O -0.0126(2) 0.1842(2) -0.0890(3) 0.0265(5) Uani 1 d . .
O3 O 0.1853(2) 0.1378(2) 0.2114(3) 0.0203(5) Uani 1 d . .
O4 O 0.3970(3) 0.2467(3) -0.1442(3) 0.0376(6) Uani 1 d . .
C1 C 0.1010(4) 0.3343(3) -0.0484(4) 0.0227(6) Uani 1 d . .
O2 O 0.0753(3) 0.4375(2) -0.1212(3) 0.0352(6) Uani 1 d . .
C2 C 0.2741(3) 0.3906(3) 0.0987(4) 0.0240(7) Uani 1 d . .
C3 C 0.3102(3) 0.2551(3) 0.1403(4) 0.0212(6) Uani 1 d . .
C4 C 0.2947(4) 0.1760(3) -0.0570(4) 0.0243(6) Uani 1 d . .
O5 O 0.1571(2) 0.0384(2) -0.1305(3) 0.0267(5) Uani 1 d . .
C5 C 0.4863(4) 0.3289(4) 0.2898(5) 0.0271(7) Uani 1 d . .
C6 C 0.5511(4) 0.2144(4) 0.3355(5) 0.0290(7) Uani 1 d . .
O6 O 0.6572(4) 0.2492(4) 0.5017(4) 0.0564(8) Uani 1 d . .
O7 O 0.5067(4) 0.1029(3) 0.2058(4) 0.0575(8) Uani 1 d . .
OW O 0.1203(4) 0.2617(4) 0.4964(5) 0.0528(8) Uani 1 d . .
N3 N 0.0000 0.5000 -0.5000 0.064(2) Uani 1 d S .
N1 N 0.2313(4) -0.0290(4) 0.5135(5) 0.0354(7) Uani 1 d . .
N2 N 0.2929(4) -0.2332(4) 0.0909(5) 0.0377(7) Uani 1 d . .
H2A H 0.2931(43) 0.4456(41) 0.2244(53) 0.030(9) Uiso 1 d . .
H2B H 0.3611(41) 0.4758(38) 0.0550(45) 0.023(8) Uiso 1 d . .
H5A H 0.4924(37) 0.3776(36) 0.4164(47) 0.021(8) Uiso 1 d . .
H5B H 0.5691(48) 0.4289(47) 0.2498(56) 0.040(10) Uiso 1 d . .
HOWA H 0.1656(88) 0.2247(79) 0.4107(105) 0.130(24) Uiso 1 d . .
HOWB H 0.0582(109) 0.2683(109) 0.4294(132) 0.182(40) Uiso 1 d . .
HN1A H 0.2639(71) -0.1118(68) 0.5087(85) 0.089(17) Uiso 1 d . .
HN1B H 0.2305(53) 0.0137(51) 0.4063(70) 0.050(11) Uiso 1 d . .
HN1C H 0.2851(50) 0.0473(51) 0.6255(64) 0.043(10) Uiso 1 d . .
HN1D H 0.0983(72) -0.1176(65) 0.4997(75) 0.085(16) Uiso 1 d . .
HN2A H 0.2208(70) -0.3317(68) 0.0328(78) 0.072(15) Uiso 1 d . .
HN2B H 0.3444(77) -0.2359(71) 0.2409(101) 0.104(20) Uiso 1 d . .
HN2C H 0.3654(71) -0.1906(66) 0.0530(83) 0.076(18) Uiso 1 d . .
HN2D H 0.1678(104) -0.2183(99) 0.0421(119) 0.158(30) Uiso 1 d . .
HN3A H -0.0842(114) 0.4380(113) -0.4894(128) 0.038(28) Uiso 0.50 d P .
HN3B H -0.0154(108) 0.5096(105) -0.6371(147) 0.048(22) Uiso 0.50 d P .
HN3C H 0.0419(113) 0.4246(115) -0.4884(138) 0.055(26) Uiso 0.50 d P .
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'
Al Al 0.0645 0.0514 '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
_geom_angle_publ_flag
O3 Al O3 180.0 2 . ?
O3 Al O5 94.36(13) 2 . ?
O3 Al O5 85.64(13) . . ?
O3 Al O5 85.64(13) 2 2 ?
O3 Al O5 94.36(13) . 2 ?
O5 Al O5 180.0 . 2 ?
O3 Al O1 89.70(11) 2 2 ?
O3 Al O1 90.30(11) . 2 ?
O5 Al O1 90.55(10) . 2 ?
O5 Al O1 89.45(10) 2 2 ?
O3 Al O1 90.30(11) 2 . ?
O3 Al O1 89.70(11) . . ?
O5 Al O1 89.45(10) . . ?
O5 Al O1 90.55(10) 2 . ?
O1 Al O1 180.0 2 . ?
C1 O1 Al 129.9(2) . . ?
C3 O3 Al 108.1(2) . . ?
O2 C1 O1 122.6(3) . . ?
O2 C1 C2 118.1(3) . . ?
O1 C1 C2 119.3(2) . . ?
C1 C2 C3 114.2(2) . . ?
O3 C3 C5 111.2(2) . . ?
O3 C3 C2 109.2(2) . . ?
C5 C3 C2 108.3(2) . . ?
O3 C3 C4 108.3(2) . . ?
C5 C3 C4 112.8(2) . . ?
C2 C3 C4 106.8(2) . . ?
O4 C4 O5 123.5(3) . . ?
O4 C4 C3 122.2(3) . . ?
O5 C4 C3 113.9(2) . . ?
C4 O5 Al 111.6(2) . . ?
C6 C5 C3 115.9(3) . . ?
O7 C6 O6 124.7(3) . . ?
O7 C6 C5 119.0(3) . . ?
O6 C6 C5 116.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al O3 1.844(3) 2 ?
Al O3 1.844(3) . ?
Al O5 1.884(3) . ?
Al O5 1.884(3) 2 ?
Al O1 1.961(3) 2 ?
Al O1 1.961(3) . ?
O1 C1 1.280(4) . ?
O3 C3 1.417(3) . ?
O4 C4 1.233(4) . ?
C1 O2 1.240(4) . ?
C1 C2 1.526(4) . ?
C2 C3 1.534(4) . ?
C3 C5 1.529(4) . ?
C3 C4 1.545(4) . ?
C4 O5 1.290(4) . ?
C5 C6 1.525(4) . ?
C6 O7 1.235(4) . ?
C6 O6 1.259(4) . ?
