#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/46/2234678.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_2234678
loop_
_publ_author_name
'Shi, Fengjuan'
'Deng, Jiguang'
'Dai, Hongxing'
_publ_section_title
;
 Poly[[dodecaaquabis(μ₃-pyridine-2,6-dicarboxylato)tetrakis(μ₂-pyridine-2,6-dicarboxylato)tricalciumdieuropium(III)]
 10.5-hydrate]
;
_journal_coeditor_code           HY2534
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m685
_journal_page_last               m686
_journal_paper_doi               10.1107/S1600536812018028
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ca3 Eu2 (C7 H3 N O4)6 (H2 O)12], 10.5H2 O'
_chemical_formula_moiety         'C42 H63 Ca3 Eu2 N6 O46.50'
_chemical_formula_sum            'C42 H63 Ca3 Eu2 N6 O46.5'
_chemical_formula_weight         1820.14
_chemical_name_systematic
;
Poly[[dodecaaquabis(μ₃-pyridine-2,6-dicarboxylato)tetrakis(μ₂-pyridine-
2,6-dicarboxylato)tricalciumdieuropium(III)] 10.5-hydrate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.685(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.070(4)
_cell_length_b                   9.471(2)
_cell_length_c                   23.540(6)
_cell_measurement_reflns_used    11834
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.3
_cell_volume                     3413.4(14)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2009)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2009)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2009)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.22
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27531
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    2.157
_exptl_absorpt_correction_T_max  0.7241
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2009)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1830
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.313
_refine_diff_density_min         -1.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0424
_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)+(0.0212P)²+16.8621P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                4964
_reflns_number_total             6015
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2534.cif
_cod_data_source_block           I
_cod_original_cell_volume        3413.5(14)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C42 H63 Ca3 Eu2 N6 O46.50'
_cod_database_code               2234678
_cod_database_fobs_code          2234678
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu Eu1 0.296251(16) 0.50554(3) 0.097315(11) 0.00952(9) Uani d . 1 1 . .
Ca Ca1 0.5000 0.0000 0.0000 0.0113(3) Uani d S 1 2 . .
Ca Ca2 0.5000 1.00350(17) 0.2500 0.0138(3) Uani d S 1 2 . .
Ca Ca3 0.0000 0.0000 0.0000 0.0198(4) Uani d S 1 2 . .
O O1 0.3736(2) 0.3233(4) 0.16621(16) 0.0151(8) Uani d . 1 1 . .
O O2 0.4013(3) 0.2000(4) 0.25127(16) 0.0182(9) Uani d . 1 1 . .
O O3 0.1929(2) 0.6789(4) 0.11297(16) 0.0174(9) Uani d . 1 1 . .
O O4 0.1130(3) 0.7722(5) 0.16683(18) 0.0282(11) Uani d . 1 1 . .
O O5 0.3886(2) 0.6872(4) 0.15705(16) 0.0149(8) Uani d . 1 1 . .
O O6 0.5155(2) 0.8058(4) 0.18919(16) 0.0158(9) Uani d . 1 1 . .
O O7 0.3344(2) 0.3313(4) 0.03339(16) 0.0140(8) Uani d . 1 1 . .
O O8 0.4335(2) 0.2095(4) 0.00428(16) 0.0169(9) Uani d . 1 1 . .
O O9 0.2999(2) 0.6871(4) 0.02212(16) 0.0162(9) Uani d . 1 1 . .
O O10 0.2495(3) 0.7858(4) -0.06830(18) 0.0243(10) Uani d . 1 1 . .
O O11 0.1823(2) 0.3273(4) 0.08688(16) 0.0159(9) Uani d . 1 1 . .
O O12 0.0604(3) 0.2142(4) 0.03527(18) 0.0205(9) Uani d . 1 1 . .
O O13 0.6116(2) 0.0662(4) 0.08852(17) 0.0185(9) Uani d D 1 1 . .
H H13A 0.647(2) 0.113(5) 0.075(2) 0.022 Uiso d D 1 1 . .
H H13B 0.639(3) 0.012(5) 0.1167(18) 0.022 Uiso d D 1 1 . .
O O14 0.4145(3) -0.0939(4) 0.05348(17) 0.0222(10) Uani d D 1 1 . .
H H14A 0.419(4) -0.043(5) 0.0840(16) 0.027 Uiso d D 1 1 . .
H H14B 0.380(3) -0.162(4) 0.052(2) 0.027 Uiso d D 1 1 . .
O O15 0.3478(3) 0.9194(4) 0.21233(17) 0.0204(9) Uani d D 1 1 . .
H H15A 0.306(3) 0.974(5) 0.194(2) 0.025 Uiso d D 1 1 . .
H H15B 0.354(4) 0.854(4) 0.1894(18) 0.025 Uiso d D 1 1 . .
O O16 0.4648(3) 1.0983(4) 0.14661(18) 0.0165(9) Uani d . 1 1 . .
H H16A 0.504(4) 1.121(7) 0.135(3) 0.020 Uiso d . 1 1 . .
H H16B 0.437(4) 1.172(7) 0.148(3) 0.020 Uiso d . 1 1 . .
O O17 0.1405(3) -0.0914(5) 0.0396(2) 0.0314(11) Uani d D 1 1 . .
H H17A 0.164(3) -0.161(4) 0.061(3) 0.038 Uiso d D 1 1 . .
H H17B 0.179(3) -0.033(5) 0.036(3) 0.038 Uiso d D 1 1 . .
O O18 -0.0140(3) -0.0554(5) 0.0933(2) 0.0391(12) Uani d D 1 1 . .
H H18A -0.0678(13) -0.048(7) 0.090(3) 0.047 Uiso d D 1 1 . .
H H18B 0.011(3) -0.118(6) 0.118(3) 0.047 Uiso d D 1 1 . .
N N1 0.2624(3) 0.4885(5) 0.19488(18) 0.0125(9) Uani d . 1 1 . .
N N2 0.4526(3) 0.5088(4) 0.09633(18) 0.0106(9) Uani d . 1 1 . .
N N3 0.1693(3) 0.5085(5) 0.00041(19) 0.0132(9) Uani d . 1 1 . .
C C1 0.3627(4) 0.2941(6) 0.2164(2) 0.0140(12) Uani d . 1 1 . .
C C2 0.2960(4) 0.3823(6) 0.2330(2) 0.0158(12) Uani d . 1 1 . .
C C3 0.2680(4) 0.3533(7) 0.2820(2) 0.0227(14) Uani d . 1 1 . .
H H3 0.2916 0.2765 0.3078 0.027 Uiso calc R 1 1 . .
C C4 0.2045(4) 0.4396(8) 0.2922(3) 0.0292(16) Uani d . 1 1 . .
H H4 0.1838 0.4223 0.3253 0.035 Uiso calc R 1 1 . .
C C5 0.1711(4) 0.5518(7) 0.2539(3) 0.0281(16) Uani d . 1 1 . .
H H5 0.1283 0.6128 0.2608 0.034 Uiso calc R 1 1 . .
C C6 0.2015(4) 0.5727(6) 0.2057(2) 0.0184(13) Uani d . 1 1 . .
C C7 0.1659(4) 0.6849(6) 0.1585(2) 0.0170(13) Uani d . 1 1 . .
C C8 0.4686(4) 0.7088(6) 0.1610(2) 0.0124(12) Uani d . 1 1 . .
C C9 0.5084(3) 0.6070(5) 0.1267(2) 0.0119(12) Uani d . 1 1 . .
C C10 0.5932(4) 0.6158(6) 0.1249(2) 0.0169(12) Uani d . 1 1 . .
H H10 0.6311 0.6876 0.1464 0.020 Uiso calc R 1 1 . .
C C11 0.6218(4) 0.5190(6) 0.0915(2) 0.0182(13) Uani d . 1 1 . .
H H11 0.6800 0.5233 0.0896 0.022 Uiso calc R 1 1 . .
C C12 0.5646(4) 0.4142(6) 0.0603(2) 0.0165(12) Uani d . 1 1 . .
H H12 0.5832 0.3458 0.0372 0.020 Uiso calc R 1 1 . .
C C13 0.4797(3) 0.4130(5) 0.0640(2) 0.0116(12) Uani d . 1 1 . .
C C14 0.4114(4) 0.3098(6) 0.0316(2) 0.0134(12) Uani d . 1 1 . .
C C15 0.2437(4) 0.7017(6) -0.0285(3) 0.0172(13) Uani d . 1 1 . .
C C16 0.1646(4) 0.6081(6) -0.0416(2) 0.0147(12) Uani d . 1 1 . .
C C17 0.0927(4) 0.6196(6) -0.0923(2) 0.0192(13) Uani d . 1 1 . .
H H17 0.0898 0.6920 -0.1207 0.023 Uiso calc R 1 1 . .
C C18 0.0254(4) 0.5236(7) -0.1002(3) 0.0258(15) Uani d . 1 1 . .
H H18 -0.0243 0.5285 -0.1346 0.031 Uiso calc R 1 1 . .
C C19 0.0312(4) 0.4197(6) -0.0574(3) 0.0207(14) Uani d . 1 1 . .
H H19 -0.0142 0.3524 -0.0622 0.025 Uiso calc R 1 1 . .
C C20 0.1038(3) 0.4157(6) -0.0079(2) 0.0137(12) Uani d . 1 1 . .
C C21 0.1156(4) 0.3100(6) 0.0415(2) 0.0149(12) Uani d . 1 1 . .
O O19 0.2379(3) 0.0820(5) 0.9928(2) 0.0386(12) Uani d D 1 1 . .
H H19A 0.211(4) 0.121(6) 0.9594(17) 0.046 Uiso d D 1 1 . .
H H19B 0.282(3) 0.132(6) 1.011(2) 0.046 Uiso d D 1 1 . .
O O20 0.2972(3) 0.9062(5) 0.3187(2) 0.0351(12) Uani d D 1 1 . .
H H20A 0.314(4) 0.890(7) 0.2883(16) 0.042 Uiso d D 1 1 . .
H H20B 0.253(3) 0.960(6) 0.309(2) 0.042 Uiso d D 1 1 . .
O O21 0.1986(3) 0.0862(5) 0.15634(18) 0.0290(11) Uani d D 1 1 . .
H H21A 0.196(4) 0.152(4) 0.1311(18) 0.035 Uiso d D 1 1 . .
H H21B 0.176(4) 0.011(3) 0.139(2) 0.035 Uiso d D 1 1 . .
O O22 0.1015(10) 0.9136(14) 0.8459(6) 0.049(4) Uani d P 0.50 1 A 1
O O23 0.1373(5) 0.9971(10) 0.2459(3) 0.030(2) Uani d P 0.50 1 B 1
O O22' 0.1367(9) 0.9633(14) 0.8406(7) 0.049(4) Uani d P 0.50 1 C 2
O O23' 0.0826(8) 1.1594(14) 0.2299(5) 0.066(4) Uani d P 0.50 1 D 2
O O24 0.8088(12) 0.744(2) 0.1251(9) 0.039(5) Uani d PU 0.25 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'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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
O5 Eu1 O7 . . 127.97(12)
O5 Eu1 O1 . . 91.03(12)
O7 Eu1 O1 . . 75.97(12)
O5 Eu1 O3 . . 76.07(12)
O7 Eu1 O3 . . 149.31(12)
O1 Eu1 O3 . . 127.54(13)
O5 Eu1 O11 . . 148.83(13)
O7 Eu1 O11 . . 77.98(12)
O1 Eu1 O11 . . 78.07(12)
O3 Eu1 O11 . . 87.52(13)
O5 Eu1 O9 . . 77.22(12)
O7 Eu1 O9 . . 87.93(12)
O1 Eu1 O9 . . 148.04(13)
O3 Eu1 O9 . . 78.80(13)
O11 Eu1 O9 . . 125.83(12)
O5 Eu1 N2 . . 63.91(13)
O7 Eu1 N2 . . 64.10(13)
O1 Eu1 N2 . . 72.89(13)
O3 Eu1 N2 . . 135.96(13)
O11 Eu1 N2 . . 136.48(13)
O9 Eu1 N2 . . 75.26(13)
O5 Eu1 N1 . . 77.31(13)
O7 Eu1 N1 . . 133.20(13)
O1 Eu1 N1 . . 63.64(13)
O3 Eu1 N1 . . 63.93(13)
O11 Eu1 N1 . . 71.66(13)
O9 Eu1 N1 . . 138.80(13)
N2 Eu1 N1 . . 120.06(13)
O5 Eu1 N3 . . 133.78(14)
O7 Eu1 N3 . . 74.84(13)
O1 Eu1 N3 . . 135.19(13)
O3 Eu1 N3 . . 74.49(13)
O11 Eu1 N3 . . 63.13(13)
O9 Eu1 N3 . . 62.70(13)
N2 Eu1 N3 . . 121.28(13)
N1 Eu1 N3 . . 118.61(14)
O8 Ca1 O8 3_655 . 179.999(2)
O8 Ca1 O14 3_655 3_655 86.94(14)
O8 Ca1 O14 . 3_655 93.06(14)
O8 Ca1 O14 3_655 . 93.07(14)
O8 Ca1 O14 . . 86.93(14)
O14 Ca1 O14 3_655 . 180.0
O8 Ca1 O13 3_655 3_655 88.30(14)
O8 Ca1 O13 . 3_655 91.70(14)
O14 Ca1 O13 3_655 3_655 92.24(14)
O14 Ca1 O13 . 3_655 87.76(14)
O8 Ca1 O13 3_655 . 91.70(14)
O8 Ca1 O13 . . 88.30(14)
O14 Ca1 O13 3_655 . 87.76(14)
O14 Ca1 O13 . . 92.24(14)
O13 Ca1 O13 3_655 . 180.0
O8 Ca1 H13A 3_655 . 92.6(12)
O8 Ca1 H13A . . 87.4(12)
O14 Ca1 H13A 3_655 . 70.1(6)
O14 Ca1 H13A . . 109.9(6)
O13 Ca1 H13A 3_655 . 162.2(6)
O13 Ca1 H13A . . 17.8(6)
O8 Ca1 H14A 3_655 . 103.8(11)
O8 Ca1 H14A . . 76.2(11)
O14 Ca1 H14A 3_655 . 162.7(6)
O14 Ca1 H14A . . 17.3(6)
O13 Ca1 H14A 3_655 . 101.5(10)
O13 Ca1 H14A . . 78.5(10)
H13A Ca1 H14A . . 95.5(12)
O6 Ca2 O6 2_655 . 78.34(19)
O6 Ca2 O2 2_655 1_565 113.44(13)
O6 Ca2 O2 . 1_565 141.21(12)
O6 Ca2 O2 2_655 2_665 141.21(12)
O6 Ca2 O2 . 2_665 113.44(13)
O2 Ca2 O2 1_565 2_665 81.20(19)
O6 Ca2 O15 2_655 2_655 78.83(13)
O6 Ca2 O15 . 2_655 72.14(13)
O2 Ca2 O15 1_565 2_655 144.61(14)
O2 Ca2 O15 2_665 2_655 71.03(13)
O6 Ca2 O15 2_655 . 72.14(13)
O6 Ca2 O15 . . 78.83(13)
O2 Ca2 O15 1_565 . 71.03(13)
O2 Ca2 O15 2_665 . 144.61(14)
O15 Ca2 O15 2_655 . 142.3(2)
O6 Ca2 O16 2_655 2_655 74.59(13)
O6 Ca2 O16 . 2_655 145.52(14)
O2 Ca2 O16 1_565 2_655 70.74(13)
O2 Ca2 O16 2_665 2_655 77.45(14)
O15 Ca2 O16 2_655 2_655 81.92(14)
O15 Ca2 O16 . 2_655 111.92(14)
O6 Ca2 O16 2_655 . 145.52(14)
O6 Ca2 O16 . . 74.59(13)
O2 Ca2 O16 1_565 . 77.45(14)
O2 Ca2 O16 2_665 . 70.74(13)
O15 Ca2 O16 2_655 . 111.91(14)
O15 Ca2 O16 . . 81.92(14)
O16 Ca2 O16 2_655 . 137.8(2)
O6 Ca2 H15B 2_655 . 71.4(11)
O6 Ca2 H15B . . 61.0(6)
O2 Ca2 H15B 1_565 . 86.9(6)
O2 Ca2 H15B 2_665 . 147.2(11)
O15 Ca2 H15B 2_655 . 128.1(6)
O15 Ca2 H15B . . 17.9(6)
O16 Ca2 H15B 2_655 . 126.9(9)
O16 Ca2 H15B . . 76.9(12)
O12 Ca3 O12 . 3 180.00(9)
O12 Ca3 O17 . 3 93.91(15)
O12 Ca3 O17 3 3 86.09(15)
O12 Ca3 O17 . . 86.09(15)
O12 Ca3 O17 3 . 93.91(15)
O17 Ca3 O17 3 . 180.0(3)
O12 Ca3 O18 . . 90.53(16)
O12 Ca3 O18 3 . 89.48(16)
O17 Ca3 O18 3 . 95.84(18)
O17 Ca3 O18 . . 84.16(18)
O12 Ca3 O18 . 3 89.47(16)
O12 Ca3 O18 3 3 90.53(16)
O17 Ca3 O18 3 3 84.16(18)
O17 Ca3 O18 . 3 95.84(18)
O18 Ca3 O18 . 3 180.0
O12 Ca3 H17B . . 72.8(11)
O12 Ca3 H17B 3 . 107.2(11)
O17 Ca3 H17B 3 . 163.3(7)
O17 Ca3 H17B . . 16.7(7)
O18 Ca3 H17B . . 94.3(12)
O18 Ca3 H17B 3 . 85.7(12)
O12 Ca3 H18A . . 95.3(15)
O12 Ca3 H18A 3 . 84.7(15)
O17 Ca3 H18A 3 . 78.7(7)
O17 Ca3 H18A . . 101.3(7)
O18 Ca3 H18A . . 17.5(8)
O18 Ca3 H18A 3 . 162.5(8)
H17B Ca3 H18A . . 111.7(14)
C1 O1 Eu1 . . 125.7(3)
C1 O2 Ca2 . 1_545 137.0(4)
C7 O3 Eu1 . . 125.3(3)
C8 O5 Eu1 . . 125.6(3)
C8 O6 Ca2 . . 137.2(4)
C14 O7 Eu1 . . 124.2(3)
C14 O8 Ca1 . . 153.3(3)
C15 O9 Eu1 . . 125.7(4)
C21 O11 Eu1 . . 125.9(3)
C21 O12 Ca3 . . 153.5(4)
Ca1 O13 H13A . . 103(4)
Ca1 O13 H13B . . 127(4)
H13A O13 H13B . . 111(4)
Ca1 O14 H14A . . 109(3)
Ca1 O14 H14B . . 141(3)
H14A O14 H14B . . 111(5)
Ca2 O15 H15A . . 122(4)
Ca2 O15 H15B . . 99(4)
H15A O15 H15B . . 110(5)
Ca2 O16 H16A . . 118(5)
Ca2 O16 H16B . . 103(4)
H16A O16 H16B . . 106(6)
Ca3 O17 H17A . . 137(4)
Ca3 O17 H17B . . 111(4)
H17A O17 H17B . . 111(5)
Ca3 O18 H18A . . 107(4)
Ca3 O18 H18B . . 131(5)
H18A O18 H18B . . 112(6)
C6 N1 C2 . . 119.0(5)
C6 N1 Eu1 . . 120.3(4)
C2 N1 Eu1 . . 120.0(4)
C9 N2 C13 . . 119.5(5)
C9 N2 Eu1 . . 120.8(3)
C13 N2 Eu1 . . 119.7(3)
C20 N3 C16 . . 119.0(5)
C20 N3 Eu1 . . 120.1(3)
C16 N3 Eu1 . . 120.8(3)
O2 C1 O1 . . 125.8(5)
O2 C1 C2 . . 118.6(5)
O1 C1 C2 . . 115.5(5)
N1 C2 C3 . . 122.4(5)
N1 C2 C1 . . 114.5(5)
C3 C2 C1 . . 123.0(5)
C4 C3 C2 . . 118.0(6)
C4 C3 H3 . . 121.0
C2 C3 H3 . . 121.0
C3 C4 C5 . . 119.9(6)
C3 C4 H4 . . 120.0
C5 C4 H4 . . 120.0
C6 C5 C4 . . 118.6(6)
C6 C5 H5 . . 120.7
C4 C5 H5 . . 120.7
N1 C6 C5 . . 122.0(6)
N1 C6 C7 . . 114.2(5)
C5 C6 C7 . . 123.6(5)
O4 C7 O3 . . 126.0(5)
O4 C7 C6 . . 118.2(5)
O3 C7 C6 . . 115.8(5)
O6 C8 O5 . . 126.2(5)
O6 C8 C9 . . 117.9(5)
O5 C8 C9 . . 115.9(5)
N2 C9 C10 . . 122.3(5)
N2 C9 C8 . . 113.8(5)
C10 C9 C8 . . 123.9(5)
C11 C10 C9 . . 118.8(5)
C11 C10 H10 . . 120.6
C9 C10 H10 . . 120.6
C10 C11 C12 . . 119.5(5)
C10 C11 H11 . . 120.3
C12 C11 H11 . . 120.3
C13 C12 C11 . . 118.2(5)
C13 C12 H12 . . 120.9
C11 C12 H12 . . 120.9
N2 C13 C12 . . 121.6(5)
N2 C13 C14 . . 114.7(5)
C12 C13 C14 . . 123.7(5)
O8 C14 O7 . . 124.7(5)
O8 C14 C13 . . 118.5(5)
O7 C14 C13 . . 116.8(5)
O10 C15 O9 . . 125.4(5)
O10 C15 C16 . . 118.1(5)
O9 C15 C16 . . 116.5(5)
N3 C16 C17 . . 121.9(5)
N3 C16 C15 . . 114.0(5)
C17 C16 C15 . . 124.1(5)
C18 C17 C16 . . 118.5(6)
C18 C17 H17 . . 120.7
C16 C17 H17 . . 120.7
C17 C18 C19 . . 119.3(5)
C17 C18 H18 . . 120.3
C19 C18 H18 . . 120.3
C20 C19 C18 . . 119.1(6)
C20 C19 H19 . . 120.5
C18 C19 H19 . . 120.5
N3 C20 C19 . . 122.1(5)
N3 C20 C21 . . 114.6(5)
C19 C20 C21 . . 123.3(5)
O12 C21 O11 . . 125.4(5)
O12 C21 C20 . . 118.5(5)
O11 C21 C20 . . 116.1(5)
H19A O19 H19B . . 109(5)
H20A O20 H20B . . 110(5)
H21A O21 H21B . . 111(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Eu1 O5 . 2.423(4)
Eu1 O7 . 2.434(4)
Eu1 O1 . 2.435(4)
Eu1 O3 . 2.441(4)
Eu1 O11 . 2.447(4)
Eu1 O9 . 2.481(4)
Eu1 N2 . 2.520(4)
Eu1 N1 . 2.521(4)
Eu1 N3 . 2.557(4)
Ca1 O8 3_655 2.270(4)
Ca1 O8 . 2.270(4)
Ca1 O14 3_655 2.305(4)
Ca1 O14 . 2.305(4)
Ca1 O13 3_655 2.383(4)
Ca1 O13 . 2.383(4)
Ca1 H13A . 2.70(5)
Ca1 H14A . 2.70(4)
Ca2 O6 2_655 2.415(4)
Ca2 O6 . 2.415(4)
Ca2 O2 1_565 2.451(4)
Ca2 O2 2_665 2.451(4)
Ca2 O15 2_655 2.466(4)
Ca2 O15 . 2.466(4)
Ca2 O16 2_655 2.493(4)
Ca2 O16 . 2.493(4)
Ca2 H15B . 2.74(5)
Ca3 O12 . 2.292(4)
Ca3 O12 3 2.292(4)
Ca3 O17 3 2.332(4)
Ca3 O17 . 2.332(4)
Ca3 O18 . 2.334(5)
Ca3 O18 3 2.334(5)
Ca3 H17B . 2.76(4)
Ca3 H18A . 2.70(5)
O1 C1 . 1.276(6)
O2 C1 . 1.243(6)
O2 Ca2 1_545 2.451(4)
O3 C7 . 1.274(7)
O4 C7 . 1.243(7)
O5 C8 . 1.277(6)
O6 C8 . 1.244(6)
O7 C14 . 1.267(6)
O8 C14 . 1.257(6)
O9 C15 . 1.266(7)
O10 C15 . 1.254(7)
O11 C21 . 1.274(6)
O12 C21 . 1.247(7)
O13 H13A . 0.850(10)
O13 H13B . 0.850(10)
O14 H14A . 0.850(10)
O14 H14B . 0.850(10)
O15 H15A . 0.850(10)
O15 H15B . 0.850(10)
O16 H16A . 0.78(6)
O16 H16B . 0.84(6)
O17 H17A . 0.850(10)
O17 H17B . 0.850(10)
O18 H18A . 0.850(10)
O18 H18B . 0.850(10)
N1 C6 . 1.345(7)
N1 C2 . 1.347(7)
N2 C9 . 1.338(7)
N2 C13 . 1.340(7)
N3 C20 . 1.339(7)
N3 C16 . 1.353(7)
C1 C2 . 1.501(8)
C2 C3 . 1.387(8)
C3 C4 . 1.383(9)
C3 H3 . 0.9500
C4 C5 . 1.391(9)
C4 H4 . 0.9500
C5 C6 . 1.379(8)
C5 H5 . 0.9500
C6 C7 . 1.519(8)
C8 C9 . 1.519(7)
C9 C10 . 1.378(8)
C10 C11 . 1.375(8)
C10 H10 . 0.9500
C11 C12 . 1.400(8)
C11 H11 . 0.9500
C12 C13 . 1.392(8)
C12 H12 . 0.9500
C13 C14 . 1.495(8)
C15 C16 . 1.502(8)
C16 C17 . 1.390(8)
C17 C18 . 1.381(8)
C17 H17 . 0.9500
C18 C19 . 1.392(9)
C18 H18 . 0.9500
C19 C20 . 1.375(8)
C19 H19 . 0.9500
C20 C21 . 1.501(8)
O19 H19A . 0.860(10)
O19 H19B . 0.850(10)
O20 H20A . 0.850(10)
O20 H20B . 0.850(10)
O21 H21A . 0.850(10)
O21 H21B . 0.850(10)
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
O13 H13A O10 3_665 0.850(10) 1.97(2) 2.796(6) 163(5)
O13 H13B O20 2_645 0.850(10) 1.850(10) 2.696(6) 175(6)
O14 H14A O16 1_545 0.850(10) 1.96(2) 2.774(6) 160(5)
O14 H14B O9 1_545 0.850(10) 1.91(2) 2.723(5) 160(5)
O15 H15A O21 1_565 0.850(10) 1.990(10) 2.839(6) 172(6)
O15 H15B O5 . 0.850(10) 1.900(10) 2.734(5) 165(5)
O16 H16A O13 1_565 0.78(6) 2.38(7) 3.079(6) 150(6)
O16 H16B O1 1_565 0.84(6) 1.88(7) 2.704(6) 169(6)
O17 H17A O3 1_545 0.850(10) 1.910(10) 2.745(6) 167(5)
O17 H17B O19 1_554 0.850(10) 1.93(3) 2.722(7) 155(6)
O18 H18A O22' 3_566 0.850(10) 2.37(6) 2.990(15) 130(6)
O18 H18A O22 3_566 0.850(10) 2.16(7) 2.657(14) 117(6)
O18 H18B O4 1_545 0.850(10) 1.98(2) 2.772(6) 155(5)
O19 H19A O24 3_666 0.860(10) 2.31(3) 3.12(2) 159(6)
O19 H19B O7 1_556 0.850(10) 2.07(4) 2.828(6) 148(6)
O20 H20A O15 . 0.850(10) 2.04(2) 2.862(6) 161(6)
O20 H20B O23 . 0.850(10) 2.03(4) 2.758(10) 143(6)
O20 H20B O22' 4_575 0.850(10) 2.32(4) 3.042(13) 143(5)
O21 H21A O11 . 0.850(10) 1.94(2) 2.774(6) 167(6)
O21 H21B O17 . 0.850(10) 2.42(4) 3.113(7) 138(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
O5 Eu1 O1 C1 . 78.5(4)
O7 Eu1 O1 C1 . -152.5(4)
O3 Eu1 O1 C1 . 5.4(5)
O11 Eu1 O1 C1 . -72.0(4)
O9 Eu1 O1 C1 . 145.6(4)
N2 Eu1 O1 C1 . 140.8(4)
N1 Eu1 O1 C1 . 3.2(4)
N3 Eu1 O1 C1 . -101.8(4)
O5 Eu1 O3 C7 . -84.6(4)
O7 Eu1 O3 C7 . 129.9(4)
O1 Eu1 O3 C7 . -4.2(5)
O11 Eu1 O3 C7 . 68.7(4)
O9 Eu1 O3 C7 . -164.0(4)
N2 Eu1 O3 C7 . -109.3(4)
N1 Eu1 O3 C7 . -2.1(4)
N3 Eu1 O3 C7 . 131.4(4)
O7 Eu1 O5 C8 . -0.5(5)
O1 Eu1 O5 C8 . 72.5(4)
O3 Eu1 O5 C8 . -159.0(4)
O11 Eu1 O5 C8 . 140.8(4)
O9 Eu1 O5 C8 . -77.5(4)
N2 Eu1 O5 C8 . 2.1(4)
N1 Eu1 O5 C8 . 135.1(4)
N3 Eu1 O5 C8 . -107.2(4)
O6 Ca2 O6 C8 2_655 66.7(5)
O2 Ca2 O6 C8 1_565 -46.3(6)
O2 Ca2 O6 C8 2_665 -152.2(5)
O15 Ca2 O6 C8 2_655 148.6(5)
O15 Ca2 O6 C8 . -7.1(5)
O16 Ca2 O6 C8 2_655 105.5(5)
O16 Ca2 O6 C8 . -91.7(5)
O5 Eu1 O7 C14 . 9.2(4)
O1 Eu1 O7 C14 . -71.0(4)
O3 Eu1 O7 C14 . 145.0(4)
O11 Eu1 O7 C14 . -151.5(4)
O9 Eu1 O7 C14 . 81.2(4)
N2 Eu1 O7 C14 . 6.6(4)
N1 Eu1 O7 C14 . -101.4(4)
N3 Eu1 O7 C14 . 143.4(4)
O14 Ca1 O8 C14 3_655 -123.5(8)
O14 Ca1 O8 C14 . 56.5(8)
O13 Ca1 O8 C14 3_655 144.1(8)
O13 Ca1 O8 C14 . -35.9(8)
O5 Eu1 O9 C15 . -157.9(4)
O7 Eu1 O9 C15 . 72.4(4)
O1 Eu1 O9 C15 . 131.3(4)
O3 Eu1 O9 C15 . -79.8(4)
O11 Eu1 O9 C15 . -1.2(5)
N2 Eu1 O9 C15 . 136.1(4)
N1 Eu1 O9 C15 . -104.8(4)
N3 Eu1 O9 C15 . -1.6(4)
O5 Eu1 O11 C21 . 133.3(4)
O7 Eu1 O11 C21 . -77.0(4)
O1 Eu1 O11 C21 . -155.0(4)
O3 Eu1 O11 C21 . 75.8(4)
O9 Eu1 O11 C21 . 1.5(5)
N2 Eu1 O11 C21 . -106.3(4)
N1 Eu1 O11 C21 . 139.1(4)
N3 Eu1 O11 C21 . 1.9(4)
O17 Ca3 O12 C21 3 -129.5(8)
O17 Ca3 O12 C21 . 50.5(8)
O18 Ca3 O12 C21 . 134.6(8)
O18 Ca3 O12 C21 3 -45.4(8)
O5 Eu1 N1 C6 . 85.5(4)
O7 Eu1 N1 C6 . -143.7(4)
O1 Eu1 N1 C6 . -176.9(4)
O3 Eu1 N1 C6 . 4.9(4)
O11 Eu1 N1 C6 . -91.5(4)
O9 Eu1 N1 C6 . 32.4(5)
N2 Eu1 N1 C6 . 134.8(4)
N3 Eu1 N1 C6 . -47.8(4)
O5 Eu1 N1 C2 . -103.9(4)
O7 Eu1 N1 C2 . 26.9(5)
O1 Eu1 N1 C2 . -6.3(4)
O3 Eu1 N1 C2 . 175.6(4)
O11 Eu1 N1 C2 . 79.2(4)
O9 Eu1 N1 C2 . -156.9(3)
N2 Eu1 N1 C2 . -54.5(4)
N3 Eu1 N1 C2 . 122.9(4)
O5 Eu1 N2 C9 . -1.6(3)
O7 Eu1 N2 C9 . 176.1(4)
O1 Eu1 N2 C9 . -101.5(4)
O3 Eu1 N2 C9 . 25.3(4)
O11 Eu1 N2 C9 . -151.8(3)
O9 Eu1 N2 C9 . 81.1(4)
N1 Eu1 N2 C9 . -57.2(4)
N3 Eu1 N2 C9 . 125.5(4)
O5 Eu1 N2 C13 . 179.9(4)
O7 Eu1 N2 C13 . -2.4(3)
O1 Eu1 N2 C13 . 80.0(4)
O3 Eu1 N2 C13 . -153.2(3)
O11 Eu1 N2 C13 . 29.7(4)
O9 Eu1 N2 C13 . -97.3(4)
N1 Eu1 N2 C13 . 124.4(4)
N3 Eu1 N2 C13 . -53.0(4)
O5 Eu1 N3 C20 . -146.2(4)
O7 Eu1 N3 C20 . 85.3(4)
O1 Eu1 N3 C20 . 34.3(5)
O3 Eu1 N3 C20 . -93.9(4)
O11 Eu1 N3 C20 . 1.3(4)
O9 Eu1 N3 C20 . -179.1(4)
N2 Eu1 N3 C20 . 131.3(4)
N1 Eu1 N3 C20 . -46.0(4)
O5 Eu1 N3 C16 . 30.0(5)
O7 Eu1 N3 C16 . -98.5(4)
O1 Eu1 N3 C16 . -149.5(4)
O3 Eu1 N3 C16 . 82.3(4)
O11 Eu1 N3 C16 . 177.5(4)
O9 Eu1 N3 C16 . -2.9(4)
N2 Eu1 N3 C16 . -52.5(4)
N1 Eu1 N3 C16 . 130.2(4)
Ca2 O2 C1 O1 1_545 -8.5(9)
Ca2 O2 C1 C2 1_545 170.7(3)
Eu1 O1 C1 O2 . 179.0(4)
Eu1 O1 C1 C2 . -0.2(6)
C6 N1 C2 C3 . 2.3(8)
Eu1 N1 C2 C3 . -168.5(4)
C6 N1 C2 C1 . 179.4(5)
Eu1 N1 C2 C1 . 8.6(6)
O2 C1 C2 N1 . 175.2(5)
O1 C1 C2 N1 . -5.5(7)
O2 C1 C2 C3 . -7.8(8)
O1 C1 C2 C3 . 171.5(5)
N1 C2 C3 C4 . -1.5(9)
C1 C2 C3 C4 . -178.3(5)
C2 C3 C4 C5 . -0.2(9)
C3 C4 C5 C6 . 1.1(10)
C2 N1 C6 C5 . -1.3(8)
Eu1 N1 C6 C5 . 169.5(4)
C2 N1 C6 C7 . -177.7(5)
Eu1 N1 C6 C7 . -7.0(6)
C4 C5 C6 N1 . -0.4(9)
C4 C5 C6 C7 . 175.7(6)
Eu1 O3 C7 O4 . -179.7(4)
Eu1 O3 C7 C6 . -0.5(7)
N1 C6 C7 O4 . -175.9(5)
C5 C6 C7 O4 . 7.8(9)
N1 C6 C7 O3 . 4.9(7)
C5 C6 C7 O3 . -171.4(5)
Ca2 O6 C8 O5 . -0.2(9)
Ca2 O6 C8 C9 . 178.4(3)
Eu1 O5 C8 O6 . 176.3(4)
Eu1 O5 C8 C9 . -2.3(6)
C13 N2 C9 C10 . 1.6(8)
Eu1 N2 C9 C10 . -176.9(4)
C13 N2 C9 C8 . 179.7(4)
Eu1 N2 C9 C8 . 1.2(6)
O6 C8 C9 N2 . -178.1(4)
O5 C8 C9 N2 . 0.6(7)
O6 C8 C9 C10 . -0.1(8)
O5 C8 C9 C10 . 178.7(5)
N2 C9 C10 C11 . -1.0(8)
C8 C9 C10 C11 . -178.9(5)
C9 C10 C11 C12 . -0.1(8)
C10 C11 C12 C13 . 0.6(8)
C9 N2 C13 C12 . -1.0(7)
Eu1 N2 C13 C12 . 177.5(4)
C9 N2 C13 C14 . -179.4(4)
Eu1 N2 C13 C14 . -0.9(6)
C11 C12 C13 N2 . 0.0(8)
C11 C12 C13 C14 . 178.2(5)
Ca1 O8 C14 O7 . -107.4(8)
Ca1 O8 C14 C13 . 73.3(9)
Eu1 O7 C14 O8 . 171.1(4)
Eu1 O7 C14 C13 . -9.5(6)
N2 C13 C14 O8 . -174.2(5)
C12 C13 C14 O8 . 7.5(8)
N2 C13 C14 O7 . 6.5(7)
C12 C13 C14 O7 . -171.9(5)
Eu1 O9 C15 O10 . -173.7(4)
Eu1 O9 C15 C16 . 5.3(7)
C20 N3 C16 C17 . 2.0(8)
Eu1 N3 C16 C17 . -174.3(4)
C20 N3 C16 C15 . -177.5(5)
Eu1 N3 C16 C15 . 6.3(6)
O10 C15 C16 N3 . 171.7(5)
O9 C15 C16 N3 . -7.4(7)
O10 C15 C16 C17 . -7.7(8)
O9 C15 C16 C17 . 173.2(5)
N3 C16 C17 C18 . -1.8(9)
C15 C16 C17 C18 . 177.6(5)
C16 C17 C18 C19 . 0.6(9)
C17 C18 C19 C20 . 0.4(9)
C16 N3 C20 C19 . -1.0(8)
Eu1 N3 C20 C19 . 175.3(4)
C16 N3 C20 C21 . -180.0(5)
Eu1 N3 C20 C21 . -3.7(6)
C18 C19 C20 N3 . -0.2(9)
C18 C19 C20 C21 . 178.7(5)
Ca3 O12 C21 O11 . -98.7(9)
Ca3 O12 C21 C20 . 81.6(9)
Eu1 O11 C21 O12 . 175.9(4)
Eu1 O11 C21 C20 . -4.4(7)
N3 C20 C21 O12 . -175.2(5)
C19 C20 C21 O12 . 5.8(8)
N3 C20 C21 O11 . 5.1(7)
C19 C20 C21 O11 . -173.9(5)
