#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180381 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/50/7205090.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_7205090
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(Gd 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)'
;
_chemical_formula_sum            'C18 H24 Gd2 N6 O21'
_chemical_formula_weight         974.91
_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                 102.5080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8519(2)
_cell_length_b                   19.6425(3)
_cell_length_c                   14.9977(3)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.052
_cell_measurement_theta_min      2.497
_cell_volume                     3408.61(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            103337
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    3.944
_exptl_absorpt_correction_T_max  0.9333
_exptl_absorpt_correction_T_min  0.7463
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1794
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.714
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         10419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0355
_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)+(0.0862P)²+9.5627P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                8386
_reflns_number_total             10419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00013B.TXT
_cod_data_source_block           770967
_cod_database_code               7205090
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
Gd1 Gd 0.79029(2) 0.015840(11) 0.806234(16) 0.02196(7) Uani 1 1 d . . .
Gd2 Gd 0.67014(2) 0.224391(11) 0.744765(16) 0.02348(7) Uani 1 1 d . . .
O5H O 0.9220(4) 0.0553(2) 0.9396(3) 0.0396(9) Uani 1 1 d . . .
O6H O 0.8136(3) -0.08885(18) 0.8799(3) 0.0298(7) Uani 1 1 d . . .
O4H O 0.5883(3) -0.0217(2) 0.7616(3) 0.0340(8) Uani 1 1 d . . .
O3A O 0.9796(4) -0.0129(2) 0.7885(3) 0.0393(10) Uani 1 1 d . . .
N2A N 0.9131(4) 0.1138(2) 0.7486(3) 0.0265(8) Uani 1 1 d . . .
N1A N 0.8795(4) 0.1791(2) 0.7370(3) 0.0255(8) Uani 1 1 d . . .
O1C O 0.6975(3) 0.11913(17) 0.8271(2) 0.0268(7) Uani 1 1 d . . .
N1B N 0.6631(4) 0.1270(2) 0.6202(3) 0.0288(9) Uani 1 1 d . . .
O2C O 0.6058(4) 0.19415(19) 0.8947(3) 0.0360(9) Uani 1 1 d . . .
O1H O 0.4751(4) 0.1830(2) 0.7128(3) 0.0449(11) Uani 1 1 d . . .
O3H O 0.8062(4) 0.2655(2) 0.8834(3) 0.0439(10) Uani 1 1 d . . .
O1B O 0.5875(4) 0.2543(2) 0.5916(3) 0.0359(9) Uani 1 1 d . . .
O1A O 0.7963(4) 0.3021(2) 0.6970(3) 0.0404(10) Uani 1 1 d . . .
O2H O 0.5856(4) 0.32695(19) 0.7790(3) 0.0378(9) Uani 1 1 d . . .
N2B N 0.6949(4) 0.0621(2) 0.6395(3) 0.0285(9) Uani 1 1 d . . .
O2A O 0.9727(4) 0.3446(2) 0.7100(4) 0.0502(12) Uani 1 1 d . . .
C1A C 0.9051(5) 0.2972(3) 0.7075(4) 0.0347(11) Uani 1 1 d . . .
C2A C 0.9508(5) 0.2252(3) 0.7163(4) 0.0287(10) Uani 1 1 d . . .
C5A C 1.0156(5) 0.0960(3) 0.7345(4) 0.0304(10) Uani 1 1 d . . .
O2B O 0.5463(4) 0.2391(2) 0.4411(3) 0.0450(11) Uani 1 1 d . . .
O3B O 0.7747(4) -0.0619(2) 0.6826(3) 0.0344(8) Uani 1 1 d . . .
C1B C 0.5806(5) 0.2190(3) 0.5215(4) 0.0328(11) Uani 1 1 d . . .
C2B C 0.6152(5) 0.1448(3) 0.5345(4) 0.0334(11) Uani 1 1 d . . .
C5B C 0.6775(6) 0.0160(3) 0.5736(4) 0.0349(12) Uani 1 1 d . . .
C3A C 1.0606(5) 0.2091(3) 0.7029(5) 0.0419(14) Uani 1 1 d . . .
H3A H 1.1103 0.2426 0.6900 0.050 Uiso 1 1 calc R . .
C4A C 1.0916(5) 0.1426(3) 0.7095(5) 0.0403(14) Uani 1 1 d . . .
H4A H 1.1618 0.1284 0.6976 0.048 Uiso 1 1 calc R . .
C6A C 1.0466(5) 0.0216(3) 0.7510(4) 0.0328(11) Uani 1 1 d . . .
O4A O 1.1343(4) 0.0004(3) 0.7288(5) 0.0582(15) Uani 1 1 d . . .
C6B C 0.7155(6) -0.0561(3) 0.6030(4) 0.0385(13) Uani 1 1 d . . .
O4B O 0.6846(6) -0.1022(2) 0.5487(4) 0.0653(16) Uani 1 1 d . . .
C3B C 0.5981(7) 0.0991(3) 0.4624(4) 0.0497(17) Uani 1 1 d . . .
H3B H 0.5670 0.1130 0.4029 0.060 Uiso 1 1 calc R . .
C4B C 0.6291(7) 0.0318(4) 0.4824(5) 0.0517(18) Uani 1 1 d . . .
H4B H 0.6182 -0.0014 0.4371 0.062 Uiso 1 1 calc R . .
C1C C 0.6497(4) 0.1376(2) 0.8932(3) 0.0261(9) Uani 1 1 d . . .
C2C C 0.6491(4) 0.0874(2) 0.9676(3) 0.0254(9) Uani 1 1 d . . .
C3C C 0.6089(5) 0.1037(3) 1.0450(4) 0.0339(11) Uani 1 1 d . . .
H3C H 0.5823 0.1472 1.0540 0.041 Uiso 1 1 calc R . .
N1C N 0.6911(4) 0.0260(2) 0.9522(3) 0.0270(8) Uani 1 1 d . . .
N2C N 0.6880(4) -0.0247(2) 1.0126(3) 0.0286(9) Uani 1 1 d . . .
C4C C 0.6101(5) 0.0529(3) 1.1077(4) 0.0345(11) Uani 1 1 d . . .
H4C H 0.5881 0.0610 1.1626 0.041 Uiso 1 1 calc R . .
C5C C 0.6461(4) -0.0126(2) 1.0855(4) 0.0275(10) Uani 1 1 d . . .
C6C C 0.6370(4) -0.0738(3) 1.1473(4) 0.0297(10) Uani 1 1 d . . .
O3C O 0.6929(4) -0.1256(2) 1.1361(3) 0.0463(11) Uani 1 1 d . . .
O4C O 0.5720(4) -0.0670(2) 1.2017(3) 0.0399(10) Uani 1 1 d . . .
O7H O 0.2829(8) 0.2353(9) 0.6005(10) 0.107(7) Uani 0.50 1 d P . .
O8H O 0.3615(8) 0.3594(5) 0.7525(9) 0.062(3) Uani 0.50 1 d P . .
O9H O 0.6221(4) 0.3754(2) 0.4419(3) 0.0375(9) Uani 1 1 d . . .
O10H O 0.4096(7) 0.3630(5) 0.5794(6) 0.116(4) 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'
Gd Gd -0.1653 3.9035 '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 Gd1 O1C 135.14(13) . . ?
O6H Gd1 O3B 77.48(13) . . ?
O1C Gd1 O3B 134.06(13) . . ?
O6H Gd1 O3A 79.95(14) . . ?
O1C Gd1 O3A 134.04(13) . . ?
O3B Gd1 O3A 71.15(15) . . ?
O6H Gd1 O5H 84.28(14) . . ?
O1C Gd1 O5H 81.30(15) . . ?
O3B Gd1 O5H 142.08(15) . . ?
O3A Gd1 O5H 73.11(16) . . ?
O6H Gd1 O4H 82.67(14) . . ?
O1C Gd1 O4H 80.75(13) . . ?
O3B Gd1 O4H 71.83(14) . . ?
O3A Gd1 O4H 141.65(15) . . ?
O5H Gd1 O4H 138.50(15) . . ?
O6H Gd1 N2A 140.89(14) . . ?
O1C Gd1 N2A 74.08(12) . . ?
O3B Gd1 N2A 99.56(14) . . ?
O3A Gd1 N2A 62.72(13) . . ?
O5H Gd1 N2A 74.53(14) . . ?
O4H Gd1 N2A 134.14(14) . . ?
O6H Gd1 N2B 136.82(13) . . ?
O1C Gd1 N2B 73.54(13) . . ?
O3B Gd1 N2B 62.81(13) . . ?
O3A Gd1 N2B 101.19(15) . . ?
O5H Gd1 N2B 137.91(15) . . ?
O4H Gd1 N2B 69.92(14) . . ?
N2A Gd1 N2B 66.49(13) . . ?
O6H Gd1 N1C 73.03(13) . . ?
O1C Gd1 N1C 62.18(12) . . ?
O3B Gd1 N1C 134.72(14) . . ?
O3A Gd1 N1C 133.77(15) . . ?
O5H Gd1 N1C 67.54(14) . . ?
O4H Gd1 N1C 70.98(14) . . ?
N2A Gd1 N1C 124.92(13) . . ?
N2B Gd1 N1C 124.21(14) . . ?
O1A Gd2 O2H 80.81(14) . . ?
O1A Gd2 O1B 72.55(15) . . ?
O2H Gd2 O1B 83.87(15) . . ?
O1A Gd2 O1C 133.87(13) . . ?
O2H Gd2 O1C 129.98(14) . . ?
O1B Gd2 O1C 134.11(14) . . ?
O1A Gd2 O1H 143.80(15) . . ?
O2H Gd2 O1H 84.03(16) . . ?
O1B Gd2 O1H 73.28(15) . . ?
O1C Gd2 O1H 80.05(14) . . ?
O1A Gd2 O3H 72.73(17) . . ?
O2H Gd2 O3H 76.61(15) . . ?
O1B Gd2 O3H 142.33(16) . . ?
O1C Gd2 O3H 81.81(15) . . ?
O1H Gd2 O3H 134.64(17) . . ?
O1A Gd2 O2C 137.51(16) . . ?
O2H Gd2 O2C 77.76(13) . . ?
O1B Gd2 O2C 139.47(14) . . ?
O1C Gd2 O2C 52.25(11) . . ?
O1H Gd2 O2C 69.15(15) . . ?
O3H Gd2 O2C 66.84(16) . . ?
O1A Gd2 N1A 62.85(13) . . ?
O2H Gd2 N1A 137.72(14) . . ?
O1B Gd2 N1A 103.53(14) . . ?
O1C Gd2 N1A 73.19(12) . . ?
O1H Gd2 N1A 138.18(16) . . ?
O3H Gd2 N1A 72.65(14) . . ?
O2C Gd2 N1A 114.40(13) . . ?
O1A Gd2 N1B 100.24(15) . . ?
O2H Gd2 N1B 144.82(14) . . ?
O1B Gd2 N1B 63.54(14) . . ?
O1C Gd2 N1B 73.81(12) . . ?
O1H Gd2 N1B 74.58(16) . . ?
O3H Gd2 N1B 137.69(14) . . ?
O2C Gd2 N1B 118.23(13) . . ?
N1A Gd2 N1B 67.49(13) . . ?
O1A Gd2 C1C 142.27(15) . . ?
O2H Gd2 C1C 103.22(15) . . ?
O1B Gd2 C1C 144.84(15) . . ?
O1C Gd2 C1C 26.77(13) . . ?
O1H Gd2 C1C 73.31(15) . . ?
O3H Gd2 C1C 71.90(16) . . ?
O2C Gd2 C1C 25.50(12) . . ?
N1A Gd2 C1C 94.12(13) . . ?
N1B Gd2 C1C 97.05(14) . . ?
C6A O3A Gd1 128.3(3) . . ?
C5A N2A N1A 119.2(4) . . ?
C5A N2A Gd1 116.4(3) . . ?
N1A N2A Gd1 124.3(3) . . ?
C2A N1A N2A 119.9(4) . . ?
C2A N1A Gd2 115.6(3) . . ?
N2A N1A Gd2 124.5(3) . . ?
C1C O1C Gd1 129.4(3) . . ?
C1C O1C Gd2 96.9(3) . . ?
Gd1 O1C Gd2 133.55(15) . . ?
C2B N1B N2B 119.9(5) . . ?
C2B N1B Gd2 115.4(4) . . ?
N2B N1B Gd2 124.5(3) . . ?
C1C O2C Gd2 89.2(3) . . ?
C1B O1B Gd2 128.2(3) . . ?
C1A O1A Gd2 127.5(3) . . ?
C5B N2B N1B 119.8(4) . . ?
C5B N2B Gd1 115.7(3) . . ?
N1B N2B Gd1 124.5(3) . . ?
O2A C1A O1A 126.0(5) . . ?
O2A C1A C2A 119.4(5) . . ?
O1A C1A C2A 114.7(5) . . ?
N1A C2A C3A 122.9(5) . . ?
N1A C2A C1A 115.3(5) . . ?
C3A C2A C1A 121.8(5) . . ?
N2A C5A C4A 122.6(5) . . ?
N2A C5A C6A 115.3(5) . . ?
C4A C5A C6A 122.0(5) . . ?
C6B O3B Gd1 128.1(4) . . ?
O1B C1B O2B 125.9(5) . . ?
O1B C1B C2B 117.3(5) . . ?
O2B C1B C2B 116.8(5) . . ?
N1B C2B C3B 122.7(5) . . ?
N1B C2B C1B 115.1(5) . . ?
C3B C2B C1B 122.2(5) . . ?
N2B C5B C4B 123.0(5) . . ?
N2B C5B C6B 115.6(5) . . ?
C4B C5B C6B 121.5(5) . . ?
C4A C3A C2A 116.9(5) . . ?
C4A C3A H3A 121.5 . . ?
C2A C3A H3A 121.5 . . ?
C3A C4A C5A 118.3(5) . . ?
C3A C4A H4A 120.9 . . ?
C5A C4A H4A 120.9 . . ?
O4A C6A O3A 126.0(5) . . ?
O4A C6A C5A 118.1(5) . . ?
O3A C6A C5A 115.8(5) . . ?
O4B C6B O3B 126.3(6) . . ?
O4B C6B C5B 118.1(6) . . ?
O3B C6B C5B 115.5(5) . . ?
C4B C3B C2B 117.6(6) . . ?
C4B C3B H3B 121.2 . . ?
C2B C3B H3B 121.2 . . ?
C3B C4B C5B 117.1(6) . . ?
C3B C4B H4B 121.5 . . ?
C5B C4B H4B 121.5 . . ?
O2C C1C O1C 121.6(5) . . ?
O2C C1C C2C 120.9(5) . . ?
O1C C1C C2C 117.5(4) . . ?
O2C C1C Gd2 65.3(3) . . ?
O1C C1C Gd2 56.3(2) . . ?
C2C C1C Gd2 173.6(3) . . ?
N1C C2C C3C 124.0(5) . . ?
N1C C2C C1C 113.8(4) . . ?
C3C C2C C1C 122.2(4) . . ?
C4C C3C C2C 116.9(5) . . ?
C4C C3C H3C 121.5 . . ?
C2C C3C H3C 121.5 . . ?
C2C N1C N2C 118.8(4) . . ?
C2C N1C Gd1 116.5(3) . . ?
N2C N1C Gd1 124.5(3) . . ?
C5C N2C N1C 119.6(4) . . ?
C3C C4C C5C 117.3(5) . . ?
C3C C4C H4C 121.3 . . ?
C5C C4C H4C 121.3 . . ?
N2C C5C C4C 123.1(5) . . ?
N2C C5C C6C 116.6(4) . . ?
C4C C5C C6C 120.3(5) . . ?
O3C C6C O4C 126.8(5) . . ?
O3C C6C C5C 116.7(5) . . ?
O4C C6C C5C 116.5(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
Gd1 O6H 2.322(3) . ?
Gd1 O1C 2.361(3) . ?
Gd1 O3B 2.378(4) . ?
Gd1 O3A 2.384(4) . ?
Gd1 O5H 2.385(4) . ?
Gd1 O4H 2.456(4) . ?
Gd1 N2A 2.666(4) . ?
Gd1 N2B 2.670(4) . ?
Gd1 N1C 2.707(4) . ?
Gd2 O1A 2.354(4) . ?
Gd2 O2H 2.356(4) . ?
Gd2 O1B 2.368(4) . ?
Gd2 O1C 2.394(3) . ?
Gd2 O1H 2.399(4) . ?
Gd2 O3H 2.474(5) . ?
Gd2 O2C 2.595(4) . ?
Gd2 N1A 2.662(4) . ?
Gd2 N1B 2.662(4) . ?
Gd2 C1C 2.856(5) . ?
O3A C6A 1.264(7) . ?
N2A C5A 1.324(7) . ?
N2A N1A 1.344(6) . ?
N1A C2A 1.320(6) . ?
O1C C1C 1.296(6) . ?
N1B C2B 1.335(7) . ?
N1B N2B 1.343(6) . ?
O2C C1C 1.230(6) . ?
O1B C1B 1.248(7) . ?
O1A C1A 1.269(7) . ?
N2B C5B 1.323(7) . ?
O2A C1A 1.223(7) . ?
C1A C2A 1.509(7) . ?
C2A C3A 1.396(8) . ?
C5A C4A 1.392(7) . ?
C5A C6A 1.514(7) . ?
O2B C1B 1.250(7) . ?
O3B C6B 1.253(7) . ?
C1B C2B 1.516(8) . ?
C2B C3B 1.387(9) . ?
C5B C4B 1.400(9) . ?
C5B C6B 1.522(8) . ?
C3A C4A 1.356(8) . ?
C3A H3A 0.9300 . ?
C4A H4A 0.9300 . ?
C6A O4A 1.230(7) . ?
C6B O4B 1.221(7) . ?
C3B C4B 1.386(9) . ?
C3B H3B 0.9300 . ?
C4B H4B 0.9300 . ?
C1C C2C 1.490(7) . ?
C2C N1C 1.344(6) . ?
C2C C3C 1.384(7) . ?
C3C C4C 1.369(7) . ?
C3C H3C 0.9300 . ?
N1C N2C 1.351(6) . ?
N2C C5C 1.317(7) . ?
C4C C5C 1.417(7) . ?
C4C H4C 0.9300 . ?
C5C C6C 1.536(7) . ?
C6C O3C 1.245(7) . ?
C6C O4C 1.245(6) . ?
