#------------------------------------------------------------------------------
#$Date: 2020-03-27 12:18:32 +0200 (Fri, 27 Mar 2020) $
#$Revision: 249787 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/23/01/2230126.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2230126
loop_
_publ_author_name
'Zenkhri, Louiza'
'Audebrand, Nathalie'
'Bataille, Thierry'
_publ_section_title
;
 Yttrium ethylenediammonium squarate tetrahydrate
;
_journal_coeditor_code           RU2003
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m529
_journal_page_last               m530
_journal_paper_doi               10.1107/S1600536811011251
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C2 H10 N2)3 [Y (C4 O4)3 (H2 O)4]2'
_chemical_formula_moiety         '3(C2 H10 N2 2+), 2(C12 H8 O16 Y 3-)'
_chemical_formula_sum            'C30 H46 N6 O32 Y2'
_chemical_formula_weight         1180.54
_chemical_name_common
;
Ethylenediammonium yttrium squarate tetrahydrate
;
_chemical_name_systematic
;
catena-poly[sesqui(ethylenediammonium)
[[tetraaquabis(squarato-κO)yttrium(III)]-μ-squarato-
κ²O:O']]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.9350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9780(2)
_cell_length_b                   13.2864(3)
_cell_length_c                   18.3970(4)
_cell_measurement_reflns_used    57148
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2194.20(8)
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 2001)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23285
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    2.746
_exptl_absorpt_correction_T_max  0.7340
_exptl_absorpt_correction_T_min  0.5833
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.772
_refine_diff_density_min         -0.624
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+4.9093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                4140
_reflns_number_total             5016
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ru2003.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2020-03-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C15 H23 N3 O16 Y'
_cod_original_formula_weight         590.27
_cod_original_formula_moiety         '1.5(C2 H10 N2 2+), C12 H8 O16 Y 3-'
_cod_original_formula_iupac          '(C2 H10 N2)1.5 [Y (C4 O4)3 (H2 O)4]'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2230126
_cod_database_fobs_code          2230126
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y Y1 0.81967(3) 0.09385(2) 0.775395(16) 0.01739(9) Uani d . 1 . .
O OW1 0.6982(2) -0.02399(18) 0.69447(13) 0.0255(5) Uani d . 1 . .
H H911 0.6156 -0.0626 0.7085 0.038 Uiso d R 1 . .
H H912 0.7647 -0.0720 0.6785 0.038 Uiso d R 1 . .
O OW2 0.5760(3) 0.15385(18) 0.74497(16) 0.0332(6) Uani d . 1 . .
H H921 0.4774 0.1303 0.7446 0.050 Uiso d R 1 . .
H H922 0.5568 0.2216 0.7550 0.050 Uiso d R 1 . .
O OW3 0.7609(4) 0.1825(2) 0.88343(19) 0.0653(12) Uani d . 1 . .
H H931 0.7880 0.2376 0.9116 0.098 Uiso d R 1 . .
H H932 0.7345 0.1447 0.9243 0.098 Uiso d R 1 . .
O OW4 1.0544(3) 0.16009(19) 0.82212(15) 0.0332(6) Uani d . 1 . .
H H941 1.1451 0.1438 0.8013 0.050 Uiso d R 1 . .
H H942 1.0623 0.2267 0.8356 0.050 Uiso d R 1 . .
C C1 0.3965(4) -0.0751(3) 0.9370(2) 0.0344(9) Uani d . 1 . .
O O1 0.2824(3) -0.0919(3) 0.97182(19) 0.0618(10) Uani d . 1 . .
C C2 0.4625(4) 0.0166(3) 0.90558(19) 0.0308(8) Uani d . 1 . .
O O2 0.4298(4) 0.1078(2) 0.90299(18) 0.0567(9) Uani d . 1 . .
C C3 0.5884(4) -0.0427(2) 0.88126(17) 0.0215(6) Uani d . 1 . .
O O3 0.7096(2) -0.02378(17) 0.84855(13) 0.0260(5) Uani d . 1 . .
C C4 0.5259(4) -0.1337(3) 0.91110(19) 0.0270(7) Uani d . 1 . .
O O4 0.5696(3) -0.2235(2) 0.91517(16) 0.0389(6) Uani d . 1 . .
C C5 0.9863(4) -0.0763(2) 0.60978(17) 0.0212(6) Uani d . 1 . .
O O5 0.8971(3) -0.14412(17) 0.62986(14) 0.0283(5) Uani d . 1 . .
C C6 1.0043(4) 0.0306(2) 0.62387(17) 0.0212(6) Uani d . 1 . .
O O6 0.9443(3) 0.09575(17) 0.66401(13) 0.0278(5) Uani d . 1 . .
C C7 1.1316(4) 0.0349(2) 0.57414(18) 0.0228(6) Uani d . 1 . .
O O7 1.2148(3) 0.10214(18) 0.55251(16) 0.0356(6) Uani d . 1 . .
C C8 1.1158(4) -0.0751(2) 0.56315(18) 0.0227(7) Uani d . 1 . .
O O8 1.1858(3) -0.14202(19) 0.53033(16) 0.0368(6) Uani d . 1 . .
C C9 0.8814(3) 0.4399(2) 0.72880(17) 0.0190(6) Uani d . 1 . .
O O9 1.0131(2) 0.46219(16) 0.71244(13) 0.0244(5) Uani d . 1 . .
C C10 0.7446(4) 0.4939(2) 0.74815(18) 0.0225(6) Uani d . 1 . .
O O10 0.7095(3) 0.58392(18) 0.75490(17) 0.0360(6) Uani d . 1 . .
C C11 0.6683(3) 0.3960(2) 0.75669(18) 0.0216(6) Uani d . 1 . .
O O11 0.5417(3) 0.3661(2) 0.77318(16) 0.0351(6) Uani d . 1 . .
C C12 0.8066(3) 0.3451(2) 0.73838(17) 0.0203(6) Uani d . 1 . .
O O12 0.8488(3) 0.25554(17) 0.73267(15) 0.0316(6) Uani d . 1 . .
N N1 0.1150(3) 0.2173(2) 1.13530(16) 0.0276(6) Uani d . 1 . .
H H11 0.1863 0.2579 1.1230 0.033 Uiso d R 1 . .
H H12 0.1531 0.1615 1.1520 0.033 Uiso d R 1 . .
H H13 0.0618 0.2454 1.1688 0.033 Uiso d R 1 . .
C C13 0.0190(4) 0.1952(3) 1.0706(2) 0.0315(8) Uani d . 1 . .
H H131 -0.0192 0.2581 1.0511 0.038 Uiso calc R 1 . .
H H132 -0.0654 0.1553 1.0858 0.038 Uiso calc R 1 . .
C C14 0.0985(4) 0.1398(3) 1.0114(2) 0.0317(8) Uani d . 1 . .
H H141 0.1488 0.0817 1.0323 0.038 Uiso calc R 1 . .
H H142 0.0257 0.1156 0.9760 0.038 Uiso calc R 1 . .
N N2 0.2096(3) 0.2041(2) 0.97398(16) 0.0300(7) Uani d . 1 . .
H H21 0.2778 0.2278 1.0107 0.036 Uiso d R 1 . .
H H22 0.1607 0.2561 0.9477 0.036 Uiso d R 1 . .
H H23 0.2683 0.1717 0.9464 0.036 Uiso d R 1 . .
N N3 0.4125(4) -0.4070(3) 0.93482(18) 0.0392(8) Uani d . 1 . .
H H31 0.4774 -0.3779 0.9072 0.047 Uiso d R 1 . .
H H32 0.3940 -0.3685 0.9718 0.047 Uiso d R 1 . .
H H33 0.3306 -0.4175 0.9100 0.047 Uiso d R 1 . .
C C15 0.4730(4) -0.5043(3) 0.9610(2) 0.0348(9) Uani d . 1 . .
H H151 0.5550 -0.5246 0.9306 0.042 Uiso calc R 1 . .
H H152 0.3963 -0.5555 0.9574 0.042 Uiso calc R 1 . .
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'
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'
Y Y -2.7962 3.5667 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Y1 O12 . . 152.48(8) ?
O3 Y1 O9 . 2_746 73.35(8) ?
O12 Y1 O9 . 2_746 131.37(8) ?
O3 Y1 O6 . . 137.19(8) ?
O12 Y1 O6 . . 68.55(8) ?
O9 Y1 O6 2_746 . 77.00(8) ?
O3 Y1 OW3 . . 75.14(9) ?
O12 Y1 OW3 . . 81.46(10) ?
O9 Y1 OW3 2_746 . 116.50(12) ?
O6 Y1 OW3 . . 147.03(9) ?
O3 Y1 OW2 . . 87.89(8) ?
O12 Y1 OW2 . . 73.57(8) ?
O9 Y1 OW2 2_746 . 150.02(8) ?
O6 Y1 OW2 . . 103.86(9) ?
OW3 Y1 OW2 . . 79.37(13) ?
O3 Y1 OW1 . . 74.04(8) ?
O12 Y1 OW1 . . 116.61(9) ?
O9 Y1 OW1 2_746 . 81.66(8) ?
O6 Y1 OW1 . . 71.68(8) ?
OW3 Y1 OW1 . . 137.23(10) ?
OW2 Y1 OW1 . . 70.61(9) ?
O3 Y1 OW4 . . 114.74(9) ?
O12 Y1 OW4 . . 71.35(9) ?
O9 Y1 OW4 2_746 . 71.44(8) ?
O6 Y1 OW4 . . 83.21(9) ?
OW3 Y1 OW4 . . 74.20(11) ?
OW2 Y1 OW4 . . 138.51(9) ?
OW1 Y1 OW4 . . 146.71(8) ?
Y1 OW1 H911 . . 122.4 ?
Y1 OW1 H912 . . 110.8 ?
H911 OW1 H912 . . 103.1 ?
Y1 OW2 H921 . . 138.7 ?
Y1 OW2 H922 . . 116.5 ?
H921 OW2 H922 . . 98.3 ?
Y1 OW3 H931 . . 142.9 ?
Y1 OW3 H932 . . 117.9 ?
H931 OW3 H932 . . 92.4 ?
Y1 OW4 H941 . . 122.0 ?
Y1 OW4 H942 . . 120.4 ?
H941 OW4 H942 . . 105.7 ?
O1 C1 C2 . . 133.9(4) ?
O1 C1 C4 . . 136.9(4) ?
C2 C1 C4 . . 89.2(3) ?
O2 C2 C3 . . 134.3(4) ?
O2 C2 C1 . . 136.1(3) ?
C3 C2 C1 . . 89.6(3) ?
O3 C3 C4 . . 133.1(3) ?
O3 C3 C2 . . 135.3(3) ?
C4 C3 C2 . . 91.6(3) ?
C3 O3 Y1 . . 142.0(2) ?
O4 C4 C3 . . 133.9(3) ?
O4 C4 C1 . . 136.4(3) ?
C3 C4 C1 . . 89.6(3) ?
O5 C5 C6 . . 135.6(3) ?
O5 C5 C8 . . 134.0(3) ?
C6 C5 C8 . . 90.4(2) ?
O6 C6 C5 . . 136.6(3) ?
O6 C6 C7 . . 132.6(3) ?
C5 C6 C7 . . 90.7(3) ?
C6 O6 Y1 . . 135.7(2) ?
O7 C7 C6 . . 134.9(3) ?
O7 C7 C8 . . 136.6(3) ?
C6 C7 C8 . . 88.4(2) ?
O8 C8 C5 . . 133.6(3) ?
O8 C8 C7 . . 136.0(3) ?
C5 C8 C7 . . 90.3(2) ?
O9 C9 C12 . . 132.6(3) ?
O9 C9 C10 . . 137.1(3) ?
C12 C9 C10 . . 90.2(2) ?
C9 O9 Y1 . 2_756 139.9(2) ?
O10 C10 C9 . . 135.0(3) ?
O10 C10 C11 . . 135.7(3) ?
C9 C10 C11 . . 89.2(2) ?
O11 C11 C12 . . 133.8(3) ?
O11 C11 C10 . . 137.0(3) ?
C12 C11 C10 . . 89.2(2) ?
O12 C12 C9 . . 132.7(3) ?
O12 C12 C11 . . 135.9(3) ?
C9 C12 C11 . . 91.4(2) ?
C12 O12 Y1 . . 145.1(2) ?
C13 N1 H11 . . 109.5 ?
C13 N1 H12 . . 109.5 ?
H11 N1 H12 . . 109.5 ?
C13 N1 H13 . . 109.5 ?
H11 N1 H13 . . 109.5 ?
H12 N1 H13 . . 109.5 ?
N1 C13 C14 . . 113.6(3) ?
N1 C13 H131 . . 108.8 ?
C14 C13 H131 . . 108.8 ?
N1 C13 H132 . . 108.8 ?
C14 C13 H132 . . 108.8 ?
H131 C13 H132 . . 107.7 ?
N2 C14 C13 . . 112.5(3) ?
N2 C14 H141 . . 109.1 ?
C13 C14 H141 . . 109.1 ?
N2 C14 H142 . . 109.1 ?
C13 C14 H142 . . 109.1 ?
H141 C14 H142 . . 107.8 ?
C14 N2 H21 . . 106.7 ?
C14 N2 H22 . . 110.2 ?
H21 N2 H22 . . 113.9 ?
C14 N2 H23 . . 114.2 ?
H21 N2 H23 . . 101.0 ?
H22 N2 H23 . . 110.5 ?
C15 N3 H31 . . 109.5 ?
C15 N3 H32 . . 109.5 ?
H31 N3 H32 . . 109.5 ?
C15 N3 H33 . . 109.5 ?
H31 N3 H33 . . 109.5 ?
H32 N3 H33 . . 109.5 ?
N3 C15 C15 . 3_647 110.7(4) ?
N3 C15 H151 . . 109.5 ?
C15 C15 H151 3_647 . 109.5 ?
N3 C15 H152 . . 109.5 ?
C15 C15 H152 3_647 . 109.5 ?
H151 C15 H152 . . 108.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Y1 O3 . 2.297(2) ?
Y1 O12 . 2.304(2) ?
Y1 O9 2_746 2.314(2) ?
Y1 O6 . 2.351(2) ?
Y1 OW3 . 2.377(3) ?
Y1 OW2 . 2.386(2) ?
Y1 OW1 . 2.409(2) ?
Y1 OW4 . 2.428(2) ?
OW1 H911 . 0.9405 ?
OW1 H912 . 0.9255 ?
OW2 H921 . 0.9388 ?
OW2 H922 . 0.9354 ?
OW3 H931 . 0.9277 ?
OW3 H932 . 0.9382 ?
OW4 H941 . 0.9307 ?
OW4 H942 . 0.9214 ?
C1 O1 . 1.237(4) ?
C1 C2 . 1.476(5) ?
C1 C4 . 1.484(5) ?
C2 O2 . 1.249(5) ?
C2 C3 . 1.454(5) ?
C3 O3 . 1.277(4) ?
C3 C4 . 1.445(5) ?
C4 O4 . 1.257(5) ?
C5 O5 . 1.265(4) ?
C5 C6 . 1.453(4) ?
C5 C8 . 1.456(4) ?
C6 O6 . 1.264(4) ?
C6 C7 . 1.476(4) ?
C7 O7 . 1.234(4) ?
C7 C8 . 1.482(4) ?
C8 O8 . 1.250(4) ?
C9 O9 . 1.261(4) ?
C9 C12 . 1.439(4) ?
C9 C10 . 1.471(4) ?
O9 Y1 2_756 2.314(2) ?
C10 O10 . 1.244(4) ?
C10 C11 . 1.479(4) ?
C11 O11 . 1.247(4) ?
C11 C12 . 1.458(4) ?
C12 O12 . 1.254(4) ?
N1 C13 . 1.487(5) ?
N1 H11 . 0.8700 ?
N1 H12 . 0.8700 ?
N1 H13 . 0.8700 ?
C13 C14 . 1.504(5) ?
C13 H131 . 0.9700 ?
C13 H132 . 0.9700 ?
C14 N2 . 1.491(5) ?
C14 H141 . 0.9700 ?
C14 H142 . 0.9700 ?
N2 H21 . 0.9571 ?
N2 H22 . 0.9479 ?
N2 H23 . 0.8528 ?
N3 C15 . 1.479(5) ?
N3 H31 . 0.8700 ?
N3 H32 . 0.8700 ?
N3 H33 . 0.8700 ?
C15 C15 3_647 1.512(8) ?
C15 H151 . 0.9700 ?
C15 H152 . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H12 O3 3_657 0.87 2.21 3.027(4) 157
N1 H12 O9 4_466 0.87 2.36 2.929(4) 123
N1 H11 O4 3_657 0.87 2.36 2.995(4) 131
N1 H11 O7 4_466 0.87 2.28 2.987(4) 138
N1 H13 O6 4_466 0.87 2.36 2.970(4) 127
N1 H13 O12 4_466 0.87 2.26 3.032(4) 148
N2 H23 O2 . 0.85 1.87 2.707(4) 167
N2 H21 O4 3_657 0.96 1.92 2.832(4) 159
N2 H21 O7 4_466 0.96 2.46 2.952(4) 112
N2 H22 O5 2_656 0.95 2.01 2.929(4) 163
N3 H31 O4 . 0.87 2.22 2.843(4) 129
N3 H32 O8 4_456 0.87 2.18 2.788(4) 127
N3 H33 OW1 2_646 0.87 2.40 2.997(4) 126
OW1 H911 O11 2_646 0.94 1.74 2.676(3) 175
OW1 H912 O5 . 0.93 1.78 2.687(3) 166
OW2 H922 O11 . 0.94 1.95 2.885(4) 173
OW2 H921 O10 2_646 0.94 1.79 2.726(3) 179
OW3 H931 O8 2_756 0.93 1.94 2.857(4) 172
OW3 H932 O1 3_657 0.94 2.04 2.954(5) 163
OW4 H942 O5 2_756 0.92 1.86 2.779(3) 172
OW4 H941 O10 2_746 0.93 1.86 2.761(4) 163
