#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180381 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/50/7205093.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_7205093
loop_
_publ_author_name
'Henry, Natacha'
'Costenoble, Sylvain'
'Lagrenée, Michel'
'Loiseau, Thierry'
'Abraham, Francis'
_publ_section_title
;
 Lanthanide-based 0D and 2D molecular assemblies with the
 pyridazine-3,6-dicarboxylate linker
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              251
_journal_paper_doi               10.1039/c0ce00013b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety
;
'2(Er 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)'
;
_chemical_formula_sum            'C18 H24 Er2 N6 O21'
_chemical_formula_weight         994.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.854(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8162(8)
_cell_length_b                   19.4943(13)
_cell_length_c                   15.0763(10)
_cell_measurement_reflns_used    9612
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.343
_cell_measurement_theta_min      2.502
_cell_volume                     3385.8(4)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART/SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62837
_diffrn_reflns_theta_full        33.32
_diffrn_reflns_theta_max         33.32
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    5.010
_exptl_absorpt_correction_T_max  0.6858
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.990
_refine_diff_density_min         -2.130
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         12985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0760P)²+9.1810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                9587
_reflns_number_total             12985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00013B.TXT
_cod_data_source_block           770970
_cod_database_code               7205093
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.789407(19) 0.017616(10) 0.807443(16) 0.02761(7) Uani 1 1 d . . .
Er2 Er 0.670569(19) 0.224561(10) 0.747414(16) 0.02726(7) Uani 1 1 d . . .
O5H O 0.9192(4) 0.0550(2) 0.9384(3) 0.0425(9) Uani 1 1 d . . .
O6H O 0.8108(4) -0.08583(18) 0.8788(3) 0.0342(8) Uani 1 1 d . . .
O4H O 0.5907(4) -0.01868(19) 0.7639(3) 0.0378(9) Uani 1 1 d . . .
O3A O 0.9761(4) -0.01283(19) 0.7925(4) 0.0427(10) Uani 1 1 d . . .
N2A N 0.9103(4) 0.1145(2) 0.7534(3) 0.0301(8) Uani 1 1 d . . .
N1A N 0.8765(4) 0.1805(2) 0.7419(3) 0.0300(8) Uani 1 1 d . . .
O1C O 0.6980(3) 0.12011(17) 0.8274(3) 0.0304(7) Uani 1 1 d . . .
N1B N 0.6626(4) 0.1293(2) 0.6264(3) 0.0324(9) Uani 1 1 d . . .
O2C O 0.6034(4) 0.1964(2) 0.8928(3) 0.0431(10) Uani 1 1 d . . .
O1H O 0.4781(4) 0.1840(2) 0.7152(4) 0.0514(12) Uani 1 1 d . . .
O3H O 0.8036(4) 0.2644(2) 0.8844(3) 0.0430(10) Uani 1 1 d . . .
O1B O 0.5878(4) 0.2569(2) 0.5989(3) 0.0402(9) Uani 1 1 d . . .
O1A O 0.7926(4) 0.3038(2) 0.7033(3) 0.0426(10) Uani 1 1 d . . .
O2H O 0.5875(4) 0.32583(19) 0.7790(3) 0.0411(9) Uani 1 1 d . . .
N2B N 0.6951(4) 0.0643(2) 0.6451(3) 0.0327(9) Uani 1 1 d . . .
O2A O 0.9705(4) 0.3470(2) 0.7155(4) 0.0575(14) Uani 1 1 d . . .
C1A C 0.9019(5) 0.2991(3) 0.7130(5) 0.0380(12) Uani 1 1 d . . .
C2A C 0.9493(5) 0.2272(3) 0.7227(4) 0.0342(11) Uani 1 1 d . . .
C5A C 1.0143(5) 0.0971(3) 0.7400(4) 0.0353(11) Uani 1 1 d . . .
O2B O 0.5425(5) 0.2419(2) 0.4481(3) 0.0483(11) Uani 1 1 d . . .
O3B O 0.7750(4) -0.0607(2) 0.6879(3) 0.0381(9) Uani 1 1 d . . .
C1B C 0.5790(5) 0.2216(3) 0.5276(4) 0.0366(12) Uani 1 1 d . . .
C2B C 0.6146(5) 0.1472(3) 0.5403(4) 0.0375(12) Uani 1 1 d . . .
C5B C 0.6774(6) 0.0180(3) 0.5796(4) 0.0396(13) Uani 1 1 d . . .
C3A C 1.0592(6) 0.2110(3) 0.7102(5) 0.0464(15) Uani 1 1 d . . .
H3A H 1.1091 0.2448 0.6979 0.056 Uiso 1 1 calc R . .
C4A C 1.0911(5) 0.1443(3) 0.7165(5) 0.0461(15) Uani 1 1 d . . .
H4A H 1.1620 0.1303 0.7055 0.055 Uiso 1 1 calc R . .
C6A C 1.0446(5) 0.0214(3) 0.7546(5) 0.0400(13) Uani 1 1 d . . .
O4A O 1.1332(5) 0.0006(3) 0.7348(5) 0.0635(15) Uani 1 1 d . . .
C6B C 0.7154(6) -0.0547(3) 0.6086(4) 0.0392(12) Uani 1 1 d . . .
O4B O 0.6853(6) -0.1014(2) 0.5548(4) 0.0627(15) Uani 1 1 d . . .
C3B C 0.5966(7) 0.1010(3) 0.4693(5) 0.0486(16) Uani 1 1 d . . .
H3B H 0.5651 0.1150 0.4100 0.058 Uiso 1 1 calc R . .
C4B C 0.6268(7) 0.0336(3) 0.4889(5) 0.0519(17) Uani 1 1 d . . .
H4B H 0.6141 0.0000 0.4440 0.062 Uiso 1 1 calc R . .
C1C C 0.6492(5) 0.1386(3) 0.8934(4) 0.0339(10) Uani 1 1 d . . .
C2C C 0.6478(5) 0.0883(3) 0.9667(4) 0.0340(11) Uani 1 1 d . . .
C3C C 0.6057(6) 0.1047(3) 1.0432(4) 0.0425(13) Uani 1 1 d . . .
H3C H 0.5772 0.1482 1.0511 0.051 Uiso 1 1 calc R . .
N1C N 0.6918(4) 0.0280(2) 0.9511(3) 0.0360(10) Uani 1 1 d . . .
N2C N 0.6871(5) -0.0240(2) 1.0117(4) 0.0370(10) Uani 1 1 d . . .
C4C C 0.6079(6) 0.0539(3) 1.1064(5) 0.0455(14) Uani 1 1 d . . .
H4C H 0.5862 0.0624 1.1610 0.055 Uiso 1 1 calc R . .
C5C C 0.6445(5) -0.0121(3) 1.0852(4) 0.0361(11) Uani 1 1 d . . .
O3C O 0.6929(5) -0.1257(2) 1.1341(4) 0.0593(14) Uani 1 1 d . . .
O4C O 0.5726(4) -0.0677(2) 1.2003(3) 0.0485(11) Uani 1 1 d . . .
O7H O 0.2857(8) 0.2414(9) 0.6069(11) 0.113(7) Uani 0.50 1 d P . .
O8H O 0.3640(9) 0.3577(5) 0.7588(11) 0.075(4) Uani 0.50 1 d P . .
O9H O 0.6225(4) 0.3771(2) 0.4443(3) 0.0436(9) Uani 1 1 d . . .
O10H O 0.4137(7) 0.3668(4) 0.5819(5) 0.099(3) Uani 1 1 d . . .
C6C C 0.6370(5) -0.0739(3) 1.1455(4) 0.0395(12) Uani 1 1 d . . .
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'
Er Er -0.2586 4.9576 '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
O6H Er1 O1C 135.09(14) . . ?
O6H Er1 O5H 83.89(15) . . ?
O1C Er1 O5H 81.87(15) . . ?
O6H Er1 O3B 76.53(14) . . ?
O1C Er1 O3B 134.82(14) . . ?
O5H Er1 O3B 141.10(15) . . ?
O6H Er1 O3A 79.19(15) . . ?
O1C Er1 O3A 134.84(13) . . ?
O5H Er1 O3A 72.81(17) . . ?
O3B Er1 O3A 70.71(16) . . ?
O6H Er1 O4H 82.35(14) . . ?
O1C Er1 O4H 80.46(14) . . ?
O5H Er1 O4H 137.99(16) . . ?
O3B Er1 O4H 72.41(15) . . ?
O3A Er1 O4H 141.62(15) . . ?
O6H Er1 N2A 141.25(14) . . ?
O1C Er1 N2A 73.73(13) . . ?
O5H Er1 N2A 74.62(15) . . ?
O3B Er1 N2A 100.57(15) . . ?
O3A Er1 N2A 63.91(13) . . ?
O4H Er1 N2A 134.39(14) . . ?
O6H Er1 N2B 136.95(14) . . ?
O1C Er1 N2B 73.03(14) . . ?
O5H Er1 N2B 138.27(15) . . ?
O3B Er1 N2B 64.12(14) . . ?
O3A Er1 N2B 102.27(16) . . ?
O4H Er1 N2B 70.12(15) . . ?
N2A Er1 N2B 66.70(14) . . ?
O6H Er1 N1C 72.98(14) . . ?
O1C Er1 N1C 62.22(13) . . ?
O5H Er1 N1C 67.15(15) . . ?
O3B Er1 N1C 134.59(15) . . ?
O3A Er1 N1C 132.89(17) . . ?
O4H Er1 N1C 70.87(15) . . ?
N2A Er1 N1C 124.22(14) . . ?
N2B Er1 N1C 124.04(15) . . ?
O2H Er2 O1A 78.95(15) . . ?
O2H Er2 O1B 81.88(16) . . ?
O1A Er2 O1B 72.35(16) . . ?
O2H Er2 O1C 130.80(15) . . ?
O1A Er2 O1C 134.66(14) . . ?
O1B Er2 O1C 135.21(14) . . ?
O2H Er2 O1H 83.89(17) . . ?
O1A Er2 O1H 143.27(16) . . ?
O1B Er2 O1H 73.25(16) . . ?
O1C Er2 O1H 80.33(15) . . ?
O2H Er2 O3H 77.01(16) . . ?
O1A Er2 O3H 72.78(17) . . ?
O1B Er2 O3H 141.97(16) . . ?
O1C Er2 O3H 81.44(15) . . ?
O1H Er2 O3H 134.08(18) . . ?
O2H Er2 O2C 77.21(14) . . ?
O1A Er2 O2C 136.47(16) . . ?
O1B Er2 O2C 137.90(16) . . ?
O1C Er2 O2C 53.63(12) . . ?
O1H Er2 O2C 68.54(17) . . ?
O3H Er2 O2C 66.68(16) . . ?
O2H Er2 N1B 144.12(15) . . ?
O1A Er2 N1B 101.74(16) . . ?
O1B Er2 N1B 64.78(14) . . ?
O1C Er2 N1B 73.72(13) . . ?
O1H Er2 N1B 74.45(18) . . ?
O3H Er2 N1B 138.04(15) . . ?
O2C Er2 N1B 118.77(14) . . ?
O2H Er2 N1A 137.36(15) . . ?
O1A Er2 N1A 64.07(14) . . ?
O1B Er2 N1A 104.81(15) . . ?
O1C Er2 N1A 72.95(13) . . ?
O1H Er2 N1A 138.68(17) . . ?
O3H Er2 N1A 72.49(15) . . ?
O2C Er2 N1A 115.37(14) . . ?
N1B Er2 N1A 68.19(14) . . ?
O2H Er2 C1C 103.41(16) . . ?
O1A Er2 C1C 142.35(16) . . ?
O1B Er2 C1C 145.25(16) . . ?
O1C Er2 C1C 27.40(14) . . ?
O1H Er2 C1C 73.24(16) . . ?
O3H Er2 C1C 71.31(16) . . ?
O2C Er2 C1C 26.26(14) . . ?
N1B Er2 C1C 97.37(15) . . ?
N1A Er2 C1C 94.33(15) . . ?
C6A O3A Er1 127.9(4) . . ?
C5A N2A N1A 118.8(4) . . ?
C5A N2A Er1 116.8(3) . . ?
N1A N2A Er1 124.4(3) . . ?
C2A N1A N2A 119.7(4) . . ?
C2A N1A Er2 115.9(3) . . ?
N2A N1A Er2 124.4(3) . . ?
C1C O1C Er1 129.2(3) . . ?
C1C O1C Er2 96.8(3) . . ?
Er1 O1C Er2 133.93(16) . . ?
N2B N1B C2B 119.3(5) . . ?
N2B N1B Er2 124.6(3) . . ?
C2B N1B Er2 115.9(4) . . ?
C1C O2C Er2 89.0(3) . . ?
C1B O1B Er2 127.6(3) . . ?
C1A O1A Er2 127.1(3) . . ?
C5B N2B N1B 120.1(5) . . ?
C5B N2B Er1 115.1(3) . . ?
N1B N2B Er1 124.7(3) . . ?
O2A C1A O1A 126.5(5) . . ?
O2A C1A C2A 118.3(5) . . ?
O1A C1A C2A 115.2(5) . . ?
N1A C2A C3A 122.9(5) . . ?
N1A C2A C1A 114.5(5) . . ?
C3A C2A C1A 122.6(5) . . ?
N2A C5A C4A 123.1(5) . . ?
N2A C5A C6A 114.9(5) . . ?
C4A C5A C6A 122.0(5) . . ?
C6B O3B Er1 127.2(4) . . ?
O2B C1B O1B 126.3(5) . . ?
O2B C1B C2B 117.1(6) . . ?
O1B C1B C2B 116.7(5) . . ?
N1B C2B C3B 122.8(5) . . ?
N1B C2B C1B 114.7(5) . . ?
C3B C2B C1B 122.5(5) . . ?
N2B C5B C4B 123.0(5) . . ?
N2B C5B C6B 115.8(5) . . ?
C4B C5B C6B 121.2(5) . . ?
C4A C3A C2A 117.7(5) . . ?
C4A C3A H3A 121.2 . . ?
C2A C3A H3A 121.2 . . ?
C3A C4A C5A 117.7(6) . . ?
C3A C4A H4A 121.1 . . ?
C5A C4A H4A 121.1 . . ?
O4A C6A O3A 126.8(5) . . ?
O4A C6A C5A 118.3(6) . . ?
O3A C6A C5A 114.7(5) . . ?
O4B C6B O3B 125.8(6) . . ?
O4B C6B C5B 118.7(6) . . ?
O3B C6B C5B 115.4(5) . . ?
C2B C3B C4B 117.9(6) . . ?
C2B C3B H3B 121.0 . . ?
C4B C3B H3B 121.0 . . ?
C3B C4B C5B 116.8(6) . . ?
C3B C4B H4B 121.6 . . ?
C5B C4B H4B 121.6 . . ?
O2C C1C O1C 120.5(5) . . ?
O2C C1C C2C 121.7(5) . . ?
O1C C1C C2C 117.8(5) . . ?
O2C C1C Er2 64.7(3) . . ?
O1C C1C Er2 55.8(2) . . ?
C2C C1C Er2 173.4(4) . . ?
N1C C2C C3C 125.3(5) . . ?
N1C C2C C1C 112.6(5) . . ?
C3C C2C C1C 122.2(5) . . ?
C4C C3C C2C 117.1(5) . . ?
C4C C3C H3C 121.4 . . ?
C2C C3C H3C 121.4 . . ?
C2C N1C N2C 117.4(5) . . ?
C2C N1C Er1 117.9(4) . . ?
N2C N1C Er1 124.7(3) . . ?
C5C N2C N1C 120.1(5) . . ?
C3C C4C C5C 117.3(6) . . ?
C3C C4C H4C 121.4 . . ?
C5C C4C H4C 121.4 . . ?
N2C C5C C4C 122.4(5) . . ?
N2C C5C C6C 116.1(5) . . ?
C4C C5C C6C 121.5(5) . . ?
O3C C6C O4C 126.5(5) . . ?
O3C C6C C5C 117.2(5) . . ?
O4C C6C C5C 116.3(5) . . ?
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
Er1 O6H 2.273(4) . ?
Er1 O1C 2.322(3) . ?
Er1 O5H 2.331(4) . ?
Er1 O3B 2.339(4) . ?
Er1 O3A 2.343(4) . ?
Er1 O4H 2.399(4) . ?
Er1 N2A 2.606(4) . ?
Er1 N2B 2.617(4) . ?
Er1 N1C 2.678(5) . ?
Er2 O2H 2.301(4) . ?
Er2 O1A 2.310(4) . ?
Er2 O1B 2.323(4) . ?
Er2 O1C 2.352(3) . ?
Er2 O1H 2.354(4) . ?
Er2 O3H 2.428(4) . ?
Er2 O2C 2.552(4) . ?
Er2 N1B 2.590(5) . ?
Er2 N1A 2.599(4) . ?
Er2 C1C 2.822(5) . ?
O3A C6A 1.279(7) . ?
N2A C5A 1.332(7) . ?
N2A N1A 1.347(6) . ?
N1A C2A 1.328(7) . ?
O1C C1C 1.308(6) . ?
N1B N2B 1.336(6) . ?
N1B C2B 1.341(7) . ?
O2C C1C 1.249(7) . ?
O1B C1B 1.261(8) . ?
O1A C1A 1.270(7) . ?
N2B C5B 1.320(7) . ?
O2A C1A 1.232(7) . ?
C1A C2A 1.504(7) . ?
C2A C3A 1.390(8) . ?
C5A C4A 1.393(8) . ?
C5A C6A 1.522(7) . ?
O2B C1B 1.245(7) . ?
O3B C6B 1.250(7) . ?
C1B C2B 1.511(8) . ?
C2B C3B 1.378(9) . ?
C5B C4B 1.398(9) . ?
C5B C6B 1.521(8) . ?
C3A C4A 1.351(8) . ?
C3A H3A 0.9300 . ?
C4A H4A 0.9300 . ?
C6A O4A 1.219(7) . ?
C6B O4B 1.218(7) . ?
C3B C4B 1.378(9) . ?
C3B H3B 0.9300 . ?
C4B H4B 0.9300 . ?
C1C C2C 1.480(8) . ?
C2C N1C 1.327(7) . ?
C2C C3C 1.390(8) . ?
C3C C4C 1.371(9) . ?
C3C H3C 0.9300 . ?
N1C N2C 1.375(7) . ?
N2C C5C 1.336(8) . ?
C4C C5C 1.416(8) . ?
C4C H4C 0.9300 . ?
C5C C6C 1.523(8) . ?
O3C C6C 1.238(8) . ?
O4C C6C 1.248(7) . ?
