#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180381 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/50/7205092.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_7205092
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(Dy 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)'
;
_chemical_formula_sum            'C18 H24 Dy2 N6 O21'
_chemical_formula_weight         985.41
_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                 102.6320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8365(3)
_cell_length_b                   19.5914(5)
_cell_length_c                   15.0554(4)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.089
_cell_measurement_theta_min      2.499
_cell_volume                     3406.74(15)
_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_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            138135
_diffrn_reflns_theta_full        36.28
_diffrn_reflns_theta_max         36.28
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    4.960
_exptl_absorpt_correction_T_max  0.6265
_exptl_absorpt_correction_T_min  0.1993
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1845
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.784
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.389
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         16270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0352
_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)+(0.0818P)²+5.4059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                12175
_reflns_number_total             16270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00013B.TXT
_cod_data_source_block           770969
_cod_database_code               7205092
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
Dy1 Dy 0.789943(14) 0.017095(7) 0.806984(11) 0.02346(5) Uani 1 1 d . . .
Dy2 Dy 0.670524(14) 0.224690(8) 0.746242(12) 0.02440(5) Uani 1 1 d . . .
O5H O 0.9200(3) 0.05517(17) 0.9392(2) 0.0392(7) Uani 1 1 d . . .
O6H O 0.8130(3) -0.08703(13) 0.87887(19) 0.0307(5) Uani 1 1 d . . .
O4H O 0.5901(3) -0.01984(15) 0.7628(2) 0.0351(6) Uani 1 1 d . . .
O3A O 0.9786(3) -0.01277(14) 0.7908(3) 0.0390(7) Uani 1 1 d . . .
N2A N 0.9115(3) 0.11471(15) 0.7515(2) 0.0267(5) Uani 1 1 d . . .
N1A N 0.8777(3) 0.18008(15) 0.7394(2) 0.0268(5) Uani 1 1 d . . .
O1C O 0.6977(2) 0.12003(13) 0.82741(19) 0.0281(5) Uani 1 1 d . . .
N1B N 0.6625(3) 0.12850(16) 0.6234(2) 0.0298(6) Uani 1 1 d . . .
O2C O 0.6046(3) 0.19524(14) 0.8940(2) 0.0375(6) Uani 1 1 d . . .
O1H O 0.4776(3) 0.18373(18) 0.7145(3) 0.0469(8) Uani 1 1 d . . .
O3H O 0.8047(3) 0.26509(18) 0.8836(3) 0.0423(7) Uani 1 1 d . . .
O1B O 0.5879(3) 0.25580(15) 0.5956(2) 0.0379(6) Uani 1 1 d . . .
O1A O 0.7936(3) 0.30330(15) 0.7002(3) 0.0401(7) Uani 1 1 d . . .
O2H O 0.5866(3) 0.32652(14) 0.7797(3) 0.0388(7) Uani 1 1 d . . .
N2B N 0.6954(3) 0.06373(16) 0.6429(2) 0.0301(6) Uani 1 1 d . . .
O2A O 0.9713(3) 0.34632(16) 0.7124(3) 0.0531(10) Uani 1 1 d . . .
C1A C 0.9034(4) 0.2982(2) 0.7101(3) 0.0355(8) Uani 1 1 d . . .
C2A C 0.9498(3) 0.22665(18) 0.7197(3) 0.0308(7) Uani 1 1 d . . .
C5A C 1.0152(3) 0.09672(19) 0.7375(3) 0.0315(7) Uani 1 1 d . . .
O2B O 0.5439(3) 0.24089(18) 0.4450(2) 0.0461(8) Uani 1 1 d . . .
O3B O 0.7749(3) -0.06070(14) 0.6856(2) 0.0345(6) Uani 1 1 d . . .
C1B C 0.5796(4) 0.2205(2) 0.5248(3) 0.0342(8) Uani 1 1 d . . .
C2B C 0.6150(4) 0.1465(2) 0.5378(3) 0.0339(8) Uani 1 1 d . . .
C5B C 0.6780(4) 0.01740(19) 0.5768(3) 0.0360(8) Uani 1 1 d . . .
C3A C 1.0602(4) 0.2106(2) 0.7069(4) 0.0428(10) Uani 1 1 d . . .
H3A H 1.1099 0.2442 0.6942 0.051 Uiso 1 1 calc R . .
C4A C 1.0918(4) 0.1437(2) 0.7136(4) 0.0425(10) Uani 1 1 d . . .
H4A H 1.1625 0.1298 0.7026 0.051 Uiso 1 1 calc R . .
C6A C 1.0460(4) 0.0218(2) 0.7536(3) 0.0364(9) Uani 1 1 d . . .
O4A O 1.1339(3) 0.0008(2) 0.7321(4) 0.0598(11) Uani 1 1 d . . .
C6B C 0.7157(4) -0.0548(2) 0.6059(3) 0.0368(8) Uani 1 1 d . . .
O4B O 0.6850(5) -0.10138(18) 0.5523(3) 0.0622(12) Uani 1 1 d . . .
C3B C 0.5972(5) 0.1003(3) 0.4656(3) 0.0481(12) Uani 1 1 d . . .
H3B H 0.5657 0.1141 0.4063 0.058 Uiso 1 1 calc R . .
C4B C 0.6283(6) 0.0334(3) 0.4858(3) 0.0503(13) Uani 1 1 d . . .
H4B H 0.6167 0.0001 0.4407 0.060 Uiso 1 1 calc R . .
C1C C 0.6499(3) 0.13850(18) 0.8939(3) 0.0287(6) Uani 1 1 d . . .
C2C C 0.6484(3) 0.08764(17) 0.9672(3) 0.0268(6) Uani 1 1 d . . .
C3C C 0.6066(4) 0.1036(2) 1.0442(3) 0.0366(8) Uani 1 1 d . . .
H3C H 0.5786 0.1469 1.0527 0.044 Uiso 1 1 calc R . .
N1C N 0.6915(3) 0.02675(16) 0.9527(2) 0.0292(6) Uani 1 1 d . . .
N2C N 0.6880(3) -0.02435(16) 1.0117(2) 0.0315(6) Uani 1 1 d . . .
C4C C 0.6086(4) 0.0531(2) 1.1068(3) 0.0377(9) Uani 1 1 d . . .
H4C H 0.5868 0.0614 1.1615 0.045 Uiso 1 1 calc R . .
C5C C 0.6451(3) -0.01246(18) 1.0854(3) 0.0288(7) Uani 1 1 d . . .
C6C C 0.6371(3) -0.0743(2) 1.1456(3) 0.0328(7) Uani 1 1 d . . .
O3C O 0.6917(3) -0.12606(17) 1.1339(3) 0.0501(9) Uani 1 1 d . . .
O4C O 0.5718(3) -0.06771(17) 1.2005(2) 0.0420(7) Uani 1 1 d . . .
O7H O 0.2851(7) 0.2384(8) 0.6054(9) 0.122(6) Uani 0.50 1 d P . .
O8H O 0.3630(7) 0.3590(4) 0.7578(9) 0.075(3) Uani 0.50 1 d P . .
O9H O 0.6217(3) 0.37630(16) 0.4438(2) 0.0382(6) Uani 1 1 d . . .
O10H O 0.4130(5) 0.3662(4) 0.5830(4) 0.103(2) 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'
Dy Dy -0.1892 4.4098 '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 Dy1 O1C 135.44(10) . . ?
O6H Dy1 O5H 83.96(11) . . ?
O1C Dy1 O5H 81.59(11) . . ?
O6H Dy1 O3B 76.82(10) . . ?
O1C Dy1 O3B 134.40(10) . . ?
O5H Dy1 O3B 141.69(11) . . ?
O6H Dy1 O3A 79.15(10) . . ?
O1C Dy1 O3A 134.53(10) . . ?
O5H Dy1 O3A 73.07(12) . . ?
O3B Dy1 O3A 70.96(12) . . ?
O6H Dy1 O4H 82.66(10) . . ?
O1C Dy1 O4H 80.70(10) . . ?
O5H Dy1 O4H 138.12(12) . . ?
O3B Dy1 O4H 71.98(11) . . ?
O3A Dy1 O4H 141.50(11) . . ?
O6H Dy1 N2A 140.94(10) . . ?
O1C Dy1 N2A 73.73(9) . . ?
O5H Dy1 N2A 74.75(11) . . ?
O3B Dy1 N2A 100.21(11) . . ?
O3A Dy1 N2A 63.59(9) . . ?
O4H Dy1 N2A 134.21(10) . . ?
O6H Dy1 N2B 136.88(10) . . ?
O1C Dy1 N2B 73.21(10) . . ?
O5H Dy1 N2B 138.21(11) . . ?
O3B Dy1 N2B 63.51(10) . . ?
O3A Dy1 N2B 101.84(12) . . ?
O4H Dy1 N2B 70.03(11) . . ?
N2A Dy1 N2B 66.54(10) . . ?
O6H Dy1 N1C 73.02(10) . . ?
O1C Dy1 N1C 62.51(9) . . ?
O5H Dy1 N1C 67.08(11) . . ?
O3B Dy1 N1C 134.51(11) . . ?
O3A Dy1 N1C 133.02(12) . . ?
O4H Dy1 N1C 71.08(11) . . ?
N2A Dy1 N1C 124.59(10) . . ?
N2B Dy1 N1C 124.36(11) . . ?
O1A Dy2 O2H 79.74(11) . . ?
O1A Dy2 O1B 72.27(12) . . ?
O2H Dy2 O1B 83.07(12) . . ?
O1A Dy2 O1H 143.38(11) . . ?
O2H Dy2 O1H 84.04(13) . . ?
O1B Dy2 O1H 73.33(12) . . ?
O1A Dy2 O1C 134.60(10) . . ?
O2H Dy2 O1C 130.13(11) . . ?
O1B Dy2 O1C 134.71(10) . . ?
O1H Dy2 O1C 80.07(11) . . ?
O1A Dy2 O3H 72.84(13) . . ?
O2H Dy2 O3H 76.65(12) . . ?
O1B Dy2 O3H 142.12(12) . . ?
O1H Dy2 O3H 134.36(13) . . ?
O1C Dy2 O3H 81.63(11) . . ?
O1A Dy2 O2C 137.09(12) . . ?
O2H Dy2 O2C 77.40(10) . . ?
O1B Dy2 O2C 138.73(12) . . ?
O1H Dy2 O2C 68.78(12) . . ?
O1C Dy2 O2C 52.76(9) . . ?
O3H Dy2 O2C 66.82(12) . . ?
O1A Dy2 N1B 101.17(12) . . ?
O2H Dy2 N1B 144.48(11) . . ?
O1B Dy2 N1B 64.05(10) . . ?
O1H Dy2 N1B 74.32(13) . . ?
O1C Dy2 N1B 73.89(9) . . ?
O3H Dy2 N1B 138.05(11) . . ?
O2C Dy2 N1B 118.38(10) . . ?
O1A Dy2 N1A 63.77(10) . . ?
O2H Dy2 N1A 137.59(10) . . ?
O1B Dy2 N1A 104.12(11) . . ?
O1H Dy2 N1A 138.30(12) . . ?
O1C Dy2 N1A 73.13(9) . . ?
O3H Dy2 N1A 72.64(11) . . ?
O2C Dy2 N1A 114.87(10) . . ?
N1B Dy2 N1A 67.94(10) . . ?
O1A Dy2 C1C 142.39(12) . . ?
O2H Dy2 C1C 103.05(11) . . ?
O1B Dy2 C1C 145.19(11) . . ?
O1H Dy2 C1C 73.31(11) . . ?
O1C Dy2 C1C 27.07(10) . . ?
O3H Dy2 C1C 71.49(12) . . ?
O2C Dy2 C1C 25.71(9) . . ?
N1B Dy2 C1C 97.36(10) . . ?
N1A Dy2 C1C 94.22(10) . . ?
C6A O3A Dy1 127.7(3) . . ?
C5A N2A N1A 119.2(3) . . ?
C5A N2A Dy1 116.2(2) . . ?
N1A N2A Dy1 124.6(2) . . ?
C2A N1A N2A 119.9(3) . . ?
C2A N1A Dy2 115.6(2) . . ?
N2A N1A Dy2 124.5(2) . . ?
C1C O1C Dy1 129.2(2) . . ?
C1C O1C Dy2 97.0(2) . . ?
Dy1 O1C Dy2 133.65(12) . . ?
C2B N1B N2B 120.1(3) . . ?
C2B N1B Dy2 115.6(3) . . ?
N2B N1B Dy2 124.1(2) . . ?
C1C O2C Dy2 89.2(2) . . ?
C1B O1B Dy2 128.0(3) . . ?
C1A O1A Dy2 126.9(2) . . ?
C5B N2B N1B 119.5(3) . . ?
C5B N2B Dy1 115.4(2) . . ?
N1B N2B Dy1 125.1(2) . . ?
O2A C1A O1A 125.6(4) . . ?
O2A C1A C2A 119.2(4) . . ?
O1A C1A C2A 115.1(3) . . ?
N1A C2A C3A 122.9(4) . . ?
N1A C2A C1A 115.1(3) . . ?
C3A C2A C1A 122.0(3) . . ?
N2A C5A C4A 122.5(4) . . ?
N2A C5A C6A 115.2(3) . . ?
C4A C5A C6A 122.2(4) . . ?
C6B O3B Dy1 127.8(3) . . ?
O2B C1B O1B 126.0(4) . . ?
O2B C1B C2B 117.2(4) . . ?
O1B C1B C2B 116.8(4) . . ?
N1B C2B C3B 122.7(4) . . ?
N1B C2B C1B 115.1(4) . . ?
C3B C2B C1B 122.2(4) . . ?
N2B C5B C4B 122.8(4) . . ?
N2B C5B C6B 115.7(4) . . ?
C4B C5B C6B 121.5(4) . . ?
C4A C3A C2A 117.1(4) . . ?
C4A C3A H3A 121.4 . . ?
C2A C3A H3A 121.4 . . ?
C3A C4A C5A 118.2(4) . . ?
C3A C4A H4A 120.9 . . ?
C5A C4A H4A 120.9 . . ?
O4A C6A O3A 126.2(4) . . ?
O4A C6A C5A 118.0(4) . . ?
O3A C6A C5A 115.8(3) . . ?
O4B C6B O3B 125.9(4) . . ?
O4B C6B C5B 118.7(4) . . ?
O3B C6B C5B 115.4(4) . . ?
C4B C3B C2B 117.3(4) . . ?
C4B C3B H3B 121.3 . . ?
C2B C3B H3B 121.3 . . ?
C3B C4B C5B 117.5(4) . . ?
C3B C4B H4B 121.2 . . ?
C5B C4B H4B 121.2 . . ?
O2C C1C O1C 120.8(3) . . ?
O2C C1C C2C 121.7(3) . . ?
O1C C1C C2C 117.4(3) . . ?
O2C C1C Dy2 65.0(2) . . ?
O1C C1C Dy2 55.88(17) . . ?
C2C C1C Dy2 173.2(3) . . ?
N1C C2C C3C 123.7(3) . . ?
N1C C2C C1C 114.2(3) . . ?
C3C C2C C1C 122.1(3) . . ?
C4C C3C C2C 117.2(4) . . ?
C4C C3C H3C 121.4 . . ?
C2C C3C H3C 121.4 . . ?
C2C N1C N2C 119.3(3) . . ?
C2C N1C Dy1 116.3(2) . . ?
N2C N1C Dy1 124.4(2) . . ?
C5C N2C N1C 119.4(3) . . ?
C3C C4C C5C 117.5(4) . . ?
C3C C4C H4C 121.3 . . ?
C5C C4C H4C 121.3 . . ?
N2C C5C C4C 122.5(3) . . ?
N2C C5C C6C 115.9(3) . . ?
C4C C5C C6C 121.5(4) . . ?
O3C C6C O4C 126.5(4) . . ?
O3C C6C C5C 117.6(4) . . ?
O4C C6C C5C 115.8(4) . . ?
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
Dy1 O6H 2.297(3) . ?
Dy1 O1C 2.345(3) . ?
Dy1 O5H 2.356(3) . ?
Dy1 O3B 2.356(3) . ?
Dy1 O3A 2.371(3) . ?
Dy1 O4H 2.424(3) . ?
Dy1 N2A 2.637(3) . ?
Dy1 N2B 2.642(3) . ?
Dy1 N1C 2.707(3) . ?
Dy2 O1A 2.327(3) . ?
Dy2 O2H 2.332(3) . ?
Dy2 O1B 2.346(3) . ?
Dy2 O1H 2.369(3) . ?
Dy2 O1C 2.373(2) . ?
Dy2 O3H 2.447(3) . ?
Dy2 O2C 2.579(3) . ?
Dy2 N1B 2.627(3) . ?
Dy2 N1A 2.626(3) . ?
Dy2 C1C 2.844(4) . ?
O3A C6A 1.267(5) . ?
N2A C5A 1.337(5) . ?
N2A N1A 1.342(4) . ?
N1A C2A 1.327(5) . ?
O1C C1C 1.304(4) . ?
N1B C2B 1.336(5) . ?
N1B N2B 1.341(4) . ?
O2C C1C 1.234(4) . ?
O1B C1B 1.255(6) . ?
O1A C1A 1.279(5) . ?
N2B C5B 1.329(5) . ?
O2A C1A 1.234(5) . ?
C1A C2A 1.501(5) . ?
C2A C3A 1.399(6) . ?
C5A C4A 1.394(6) . ?
C5A C6A 1.519(5) . ?
O2B C1B 1.250(5) . ?
O3B C6B 1.256(5) . ?
C1B C2B 1.510(6) . ?
C2B C3B 1.394(7) . ?
C5B C4B 1.404(6) . ?
C5B C6B 1.519(6) . ?
C3A C4A 1.360(6) . ?
C3A H3A 0.9300 . ?
C4A H4A 0.9300 . ?
C6A O4A 1.227(5) . ?
C6B O4B 1.219(5) . ?
C3B C4B 1.377(7) . ?
C3B H3B 0.9300 . ?
C4B H4B 0.9300 . ?
C1C C2C 1.490(5) . ?
C2C N1C 1.334(5) . ?
C2C C3C 1.392(5) . ?
C3C C4C 1.363(6) . ?
C3C H3C 0.9300 . ?
N1C N2C 1.345(4) . ?
N2C C5C 1.337(5) . ?
C4C C5C 1.414(5) . ?
C4C H4C 0.9300 . ?
C5C C6C 1.529(5) . ?
C6C O3C 1.235(5) . ?
C6C O4C 1.255(5) . ?
