#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180381 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/50/7205091.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_7205091
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(Tb 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)'
;
_chemical_formula_sum            'C18 H24 N6 O21 Tb2'
_chemical_formula_weight         978.13
_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                 102.750(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8076(6)
_cell_length_b                   19.6020(10)
_cell_length_c                   14.9743(7)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.412
_cell_measurement_theta_min      2.502
_cell_volume                     3380.4(3)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART/SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0212
_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       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            115552
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    4.237
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6006
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.090
_refine_diff_density_max         3.338
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         10305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0816P)²+10.1305P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1359
_reflns_number_gt                8618
_reflns_number_total             10305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00013B.TXT
_cod_data_source_block           770968
_cod_database_code               7205091
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
Tb1 Tb 0.790002(19) 0.015469(10) 0.806350(15) 0.02657(7) Uani 1 1 d . . .
Tb2 Tb 0.669600(18) 0.223388(10) 0.744419(16) 0.02770(7) Uani 1 1 d . . .
O5H O 0.9220(4) 0.0550(2) 0.9397(3) 0.0425(9) Uani 1 1 d . . .
O6H O 0.8135(3) -0.08847(17) 0.8806(3) 0.0349(7) Uani 1 1 d . . .
O4H O 0.5885(3) -0.02188(19) 0.7625(3) 0.0387(8) Uani 1 1 d . . .
O3A O 0.9786(4) -0.01380(18) 0.7890(3) 0.0436(10) Uani 1 1 d . . .
N2A N 0.9120(4) 0.1130(2) 0.7493(3) 0.0312(8) Uani 1 1 d . . .
N1A N 0.8784(4) 0.1784(2) 0.7382(3) 0.0307(8) Uani 1 1 d . . .
O1C O 0.6966(3) 0.11858(17) 0.8262(2) 0.0316(7) Uani 1 1 d . . .
N1B N 0.6617(4) 0.1268(2) 0.6206(3) 0.0333(8) Uani 1 1 d . . .
O2C O 0.6039(4) 0.19424(19) 0.8935(3) 0.0424(9) Uani 1 1 d . . .
O1H O 0.4744(4) 0.1821(2) 0.7109(3) 0.0509(11) Uani 1 1 d . . .
O3H O 0.8045(4) 0.2640(2) 0.8835(3) 0.0479(10) Uani 1 1 d . . .
O1B O 0.5875(4) 0.25387(19) 0.5920(3) 0.0408(8) Uani 1 1 d . . .
O1A O 0.7949(3) 0.3017(2) 0.6982(3) 0.0442(9) Uani 1 1 d . . .
O2H O 0.5851(4) 0.32549(19) 0.7772(3) 0.0434(9) Uani 1 1 d . . .
N2B N 0.6939(4) 0.0615(2) 0.6402(3) 0.0337(9) Uani 1 1 d . . .
O2A O 0.9720(4) 0.3443(2) 0.7105(4) 0.0578(13) Uani 1 1 d . . .
C1A C 0.9041(4) 0.2967(3) 0.7090(4) 0.0376(11) Uani 1 1 d . . .
C2A C 0.9497(4) 0.2247(2) 0.7170(4) 0.0353(11) Uani 1 1 d . . .
C5A C 1.0146(4) 0.0951(3) 0.7348(4) 0.0355(10) Uani 1 1 d . . .
O2B O 0.5448(5) 0.2386(2) 0.4409(3) 0.0516(11) Uani 1 1 d . . .
O3B O 0.7743(4) -0.06285(19) 0.6842(3) 0.0397(8) Uani 1 1 d . . .
C1B C 0.5791(5) 0.2187(3) 0.5217(4) 0.0380(12) Uani 1 1 d . . .
C2B C 0.6149(5) 0.1448(3) 0.5352(4) 0.0391(11) Uani 1 1 d . . .
C5B C 0.6778(6) 0.0152(3) 0.5742(4) 0.0418(13) Uani 1 1 d . . .
C3A C 1.0602(5) 0.2086(3) 0.7030(5) 0.0476(14) Uani 1 1 d . . .
H3A H 1.1102 0.2421 0.6905 0.057 Uiso 1 1 calc R . .
C4A C 1.0905(5) 0.1417(3) 0.7086(5) 0.0474(14) Uani 1 1 d . . .
H4A H 1.1600 0.1273 0.6954 0.057 Uiso 1 1 calc R . .
C6A C 1.0453(5) 0.0203(3) 0.7507(5) 0.0413(12) Uani 1 1 d . . .
O4A O 1.1333(5) -0.0007(3) 0.7292(5) 0.0675(16) Uani 1 1 d . . .
C6B C 0.7164(6) -0.0569(3) 0.6043(4) 0.0428(12) Uani 1 1 d . . .
O4B O 0.6855(6) -0.1033(2) 0.5488(4) 0.0713(17) Uani 1 1 d . . .
C3B C 0.5981(7) 0.0981(3) 0.4623(4) 0.0565(18) Uani 1 1 d . . .
H3B H 0.5675 0.1119 0.4024 0.068 Uiso 1 1 calc R . .
C4B C 0.6289(8) 0.0309(3) 0.4830(5) 0.0578(18) Uani 1 1 d . . .
H4B H 0.6174 -0.0025 0.4378 0.069 Uiso 1 1 calc R . .
C1C C 0.6494(4) 0.1372(2) 0.8930(4) 0.0325(9) Uani 1 1 d . . .
C2C C 0.6487(4) 0.0869(2) 0.9670(3) 0.0316(9) Uani 1 1 d . . .
C3C C 0.6084(5) 0.1039(3) 1.0447(4) 0.0415(12) Uani 1 1 d . . .
H3C H 0.5815 0.1475 1.0532 0.050 Uiso 1 1 calc R . .
N1C N 0.6919(4) 0.0262(2) 0.9524(3) 0.0325(8) Uani 1 1 d . . .
N2C N 0.6886(4) -0.0244(2) 1.0135(3) 0.0361(9) Uani 1 1 d . . .
C4C C 0.6104(5) 0.0534(3) 1.1079(4) 0.0421(12) Uani 1 1 d . . .
H4C H 0.5884 0.0618 1.1629 0.050 Uiso 1 1 calc R . .
C5C C 0.6470(5) -0.0121(2) 1.0869(4) 0.0338(10) Uani 1 1 d . . .
C6C C 0.6380(5) -0.0735(3) 1.1486(4) 0.0383(11) Uani 1 1 d . . .
O3C O 0.6949(4) -0.1252(2) 1.1384(4) 0.0571(12) Uani 1 1 d . . .
O4C O 0.5741(4) -0.0666(2) 1.2028(3) 0.0468(10) Uani 1 1 d . . .
O7H O 0.2833(8) 0.2368(10) 0.5997(9) 0.112(7) Uani 0.50 1 d P . .
O8H O 0.3613(8) 0.3584(5) 0.7535(11) 0.077(4) Uani 0.50 1 d P . .
O9H O 0.6210(4) 0.3751(2) 0.4415(3) 0.0442(9) Uani 1 1 d . . .
O10H O 0.4094(7) 0.3637(5) 0.5792(6) 0.116(3) 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'
Tb Tb -0.1723 4.1537 '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 Tb1 O1C 135.01(13) . . ?
O6H Tb1 O3B 77.31(13) . . ?
O1C Tb1 O3B 134.18(13) . . ?
O6H Tb1 O3A 79.81(13) . . ?
O1C Tb1 O3A 134.44(13) . . ?
O3B Tb1 O3A 70.91(15) . . ?
O6H Tb1 O5H 84.02(14) . . ?
O1C Tb1 O5H 81.52(14) . . ?
O3B Tb1 O5H 141.92(14) . . ?
O3A Tb1 O5H 73.31(16) . . ?
O6H Tb1 O4H 82.60(13) . . ?
O1C Tb1 O4H 80.52(13) . . ?
O3B Tb1 O4H 72.00(14) . . ?
O3A Tb1 O4H 141.55(15) . . ?
O5H Tb1 O4H 138.16(14) . . ?
O6H Tb1 N2A 140.97(13) . . ?
O1C Tb1 N2A 73.98(12) . . ?
O3B Tb1 N2A 100.06(14) . . ?
O3A Tb1 N2A 63.09(12) . . ?
O5H Tb1 N2A 74.50(14) . . ?
O4H Tb1 N2A 134.34(13) . . ?
O6H Tb1 N2B 137.13(13) . . ?
O1C Tb1 N2B 73.21(13) . . ?
O3B Tb1 N2B 63.33(13) . . ?
O3A Tb1 N2B 101.36(16) . . ?
O5H Tb1 N2B 137.94(14) . . ?
O4H Tb1 N2B 70.11(14) . . ?
N2A Tb1 N2B 66.57(13) . . ?
O6H Tb1 N1C 72.92(13) . . ?
O1C Tb1 N1C 62.18(12) . . ?
O3B Tb1 N1C 134.68(14) . . ?
O3A Tb1 N1C 133.63(15) . . ?
O5H Tb1 N1C 67.24(14) . . ?
O4H Tb1 N1C 70.95(14) . . ?
N2A Tb1 N1C 124.52(13) . . ?
N2B Tb1 N1C 124.16(14) . . ?
O2H Tb2 O1A 80.06(14) . . ?
O2H Tb2 O1B 83.25(15) . . ?
O1A Tb2 O1B 72.47(15) . . ?
O2H Tb2 O1C 130.33(14) . . ?
O1A Tb2 O1C 134.21(13) . . ?
O1B Tb2 O1C 134.39(13) . . ?
O2H Tb2 O1H 84.11(16) . . ?
O1A Tb2 O1H 143.48(15) . . ?
O1B Tb2 O1H 73.14(15) . . ?
O1C Tb2 O1H 80.17(14) . . ?
O2H Tb2 O3H 76.78(15) . . ?
O1A Tb2 O3H 72.80(17) . . ?
O1B Tb2 O3H 142.30(15) . . ?
O1C Tb2 O3H 81.67(14) . . ?
O1H Tb2 O3H 134.61(17) . . ?
O2H Tb2 O2C 77.55(13) . . ?
O1A Tb2 O2C 136.92(16) . . ?
O1B Tb2 O2C 139.17(15) . . ?
O1C Tb2 O2C 52.80(12) . . ?
O1H Tb2 O2C 69.34(16) . . ?
O3H Tb2 O2C 66.52(16) . . ?
O2H Tb2 N1B 144.32(15) . . ?
O1A Tb2 N1B 100.92(15) . . ?
O1B Tb2 N1B 63.71(13) . . ?
O1C Tb2 N1B 73.85(12) . . ?
O1H Tb2 N1B 74.12(16) . . ?
O3H Tb2 N1B 138.07(14) . . ?
O2C Tb2 N1B 118.56(13) . . ?
O2H Tb2 N1A 137.65(14) . . ?
O1A Tb2 N1A 63.38(13) . . ?
O1B Tb2 N1A 103.84(14) . . ?
O1C Tb2 N1A 73.09(12) . . ?
O1H Tb2 N1A 138.15(15) . . ?
O3H Tb2 N1A 72.69(14) . . ?
O2C Tb2 N1A 114.67(13) . . ?
N1B Tb2 N1A 67.90(13) . . ?
O2H Tb2 C1C 103.37(15) . . ?
O1A Tb2 C1C 142.01(15) . . ?
O1B Tb2 C1C 145.29(15) . . ?
O1C Tb2 C1C 26.96(13) . . ?
O1H Tb2 C1C 73.74(15) . . ?
O3H Tb2 C1C 71.36(16) . . ?
O2C Tb2 C1C 25.87(12) . . ?
N1B Tb2 C1C 97.32(13) . . ?
N1A Tb2 C1C 93.96(13) . . ?
C6A O3A Tb1 128.1(3) . . ?
C5A N2A N1A 119.2(4) . . ?
C5A N2A Tb1 116.4(3) . . ?
N1A N2A Tb1 124.3(3) . . ?
C2A N1A N2A 119.9(4) . . ?
C2A N1A Tb2 115.4(3) . . ?
N2A N1A Tb2 124.6(3) . . ?
C1C O1C Tb1 129.1(3) . . ?
C1C O1C Tb2 97.1(3) . . ?
Tb1 O1C Tb2 133.69(15) . . ?
C2B N1B N2B 120.0(4) . . ?
C2B N1B Tb2 115.5(3) . . ?
N2B N1B Tb2 124.3(3) . . ?
C1C O2C Tb2 88.9(3) . . ?
C1B O1B Tb2 128.3(3) . . ?
C1A O1A Tb2 127.2(3) . . ?
C5B N2B N1B 120.1(4) . . ?
C5B N2B Tb1 115.3(3) . . ?
N1B N2B Tb1 124.6(3) . . ?
O2A C1A O1A 125.9(5) . . ?
O2A C1A C2A 119.4(5) . . ?
O1A C1A C2A 114.7(4) . . ?
N1A C2A C3A 123.0(5) . . ?
N1A C2A C1A 115.2(4) . . ?
C3A C2A C1A 121.8(5) . . ?
N2A C5A C4A 122.8(5) . . ?
N2A C5A C6A 115.2(5) . . ?
C4A C5A C6A 122.0(5) . . ?
C6B O3B Tb1 127.9(3) . . ?
O1B C1B O2B 126.5(5) . . ?
O1B C1B C2B 116.7(5) . . ?
O2B C1B C2B 116.7(5) . . ?
N1B C2B C3B 122.3(5) . . ?
N1B C2B C1B 115.4(5) . . ?
C3B C2B C1B 122.2(5) . . ?
N2B C5B C4B 122.6(5) . . ?
N2B C5B C6B 115.5(5) . . ?
C4B C5B C6B 121.9(5) . . ?
C4A C3A C2A 116.7(5) . . ?
C3A C4A C5A 118.2(5) . . ?
O4A C6A O3A 126.2(5) . . ?
O4A C6A C5A 118.1(5) . . ?
O3A C6A C5A 115.6(5) . . ?
O4B C6B O3B 126.6(5) . . ?
O4B C6B C5B 117.4(5) . . ?
O3B C6B C5B 115.9(5) . . ?
C4B C3B C2B 117.5(6) . . ?
C3B C4B C5B 117.5(6) . . ?
O2C C1C O1C 121.1(4) . . ?
O2C C1C C2C 121.3(5) . . ?
O1C C1C C2C 117.5(4) . . ?
O2C C1C Tb2 65.2(3) . . ?
O1C C1C Tb2 56.0(2) . . ?
C2C C1C Tb2 173.3(3) . . ?
N1C C2C C3C 124.4(5) . . ?
N1C C2C C1C 113.9(4) . . ?
C3C C2C C1C 121.6(4) . . ?
C4C C3C C2C 116.7(5) . . ?
C2C N1C N2C 118.3(4) . . ?
C2C N1C Tb1 116.8(3) . . ?
N2C N1C Tb1 124.8(3) . . ?
C5C N2C N1C 119.9(4) . . ?
C3C C4C C5C 117.6(5) . . ?
N2C C5C C4C 122.8(5) . . ?
N2C C5C C6C 116.4(4) . . ?
C4C C5C C6C 120.9(5) . . ?
O4C C6C O3C 126.6(5) . . ?
O4C C6C C5C 116.4(5) . . ?
O3C C6C C5C 117.0(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
Tb1 O6H 2.308(3) . ?
Tb1 O1C 2.352(3) . ?
Tb1 O3B 2.364(4) . ?
Tb1 O3A 2.369(4) . ?
Tb1 O5H 2.375(4) . ?
Tb1 O4H 2.437(4) . ?
Tb1 N2A 2.646(4) . ?
Tb1 N2B 2.655(4) . ?
Tb1 N1C 2.699(4) . ?
Tb2 O2H 2.336(4) . ?
Tb2 O1A 2.339(4) . ?
Tb2 O1B 2.351(4) . ?
Tb2 O1C 2.377(3) . ?
Tb2 O1H 2.389(4) . ?
Tb2 O3H 2.459(4) . ?
Tb2 O2C 2.584(4) . ?
Tb2 N1B 2.637(4) . ?
Tb2 N1A 2.640(4) . ?
Tb2 C1C 2.846(5) . ?
O3A C6A 1.263(7) . ?
N2A C5A 1.323(6) . ?
N2A N1A 1.342(5) . ?
N1A C2A 1.323(6) . ?
O1C C1C 1.300(6) . ?
N1B C2B 1.323(7) . ?
N1B N2B 1.349(6) . ?
O2C C1C 1.242(6) . ?
O1B C1B 1.245(7) . ?
O1A C1A 1.267(6) . ?
N2B C5B 1.325(7) . ?
O2A C1A 1.227(6) . ?
C1A C2A 1.507(7) . ?
C2A C3A 1.401(7) . ?
C5A C4A 1.395(8) . ?
C5A C6A 1.516(7) . ?
O2B C1B 1.250(7) . ?
O3B C6B 1.245(7) . ?
C1B C2B 1.511(7) . ?
C2B C3B 1.404(9) . ?
C5B C4B 1.395(8) . ?
C5B C6B 1.521(8) . ?
C3A C4A 1.358(8) . ?
C6A O4A 1.226(7) . ?
C6B O4B 1.233(7) . ?
C3B C4B 1.382(9) . ?
C1C C2C 1.483(7) . ?
C2C N1C 1.330(6) . ?
C2C C3C 1.391(7) . ?
C3C C4C 1.367(8) . ?
N1C N2C 1.358(6) . ?
N2C C5C 1.320(7) . ?
C4C C5C 1.411(7) . ?
C5C C6C 1.536(7) . ?
C6C O4C 1.232(7) . ?
C6C O3C 1.244(7) . ?
