#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180381 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/50/7205094.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_7205094
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(Lu 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)'
;
_chemical_formula_sum            'C18 H24 Lu2 N6 O21'
_chemical_formula_weight         1010.35
_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                 103.041(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7980(7)
_cell_length_b                   19.4168(12)
_cell_length_c                   14.8932(10)
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.554
_cell_measurement_theta_min      2.255
_cell_volume                     3323.7(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_ambient_temperature      296(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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            122645
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    5.996
_exptl_absorpt_correction_T_max  0.5339
_exptl_absorpt_correction_T_min  0.1137
_exptl_absorpt_correction_type   'empirical (SADABS)'
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2290
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.413
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.432
_refine_ls_extinction_coef       0.00170(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         10139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0336
_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)+(0.0688P)²+12.1299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                8908
_reflns_number_total             10139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00013B.TXT
_cod_data_source_block           770971
_cod_database_code               7205094
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
Lu1 Lu 0.789080(16) 0.016114(9) 0.805557(13) 0.02459(7) Uani 1 1 d . . .
Lu2 Lu 0.671339(16) 0.222099(9) 0.742938(14) 0.02486(7) Uani 1 1 d . . .
O5H O 0.9183(3) 0.0537(2) 0.9358(3) 0.0373(8) Uani 1 1 d . . .
O6H O 0.8129(3) -0.08530(17) 0.8792(2) 0.0300(7) Uani 1 1 d . . .
O4H O 0.5930(3) -0.02006(19) 0.7641(3) 0.0340(8) Uani 1 1 d . . .
O3A O 0.9737(4) -0.01551(19) 0.7894(3) 0.0402(9) Uani 1 1 d . . .
N2A N 0.9086(4) 0.1120(2) 0.7495(3) 0.0288(8) Uani 1 1 d . . .
N1A N 0.8745(4) 0.1781(2) 0.7370(3) 0.0281(8) Uani 1 1 d . . .
O1C O 0.6989(3) 0.11847(17) 0.8237(2) 0.0263(6) Uani 1 1 d . . .
N1B N 0.6622(4) 0.1270(2) 0.6220(3) 0.0305(8) Uani 1 1 d . . .
O2C O 0.6051(4) 0.1954(2) 0.8899(3) 0.0385(8) Uani 1 1 d . . .
O1H O 0.4810(3) 0.1822(2) 0.7101(3) 0.0434(10) Uani 1 1 d . . .
O3H O 0.8041(4) 0.2610(2) 0.8804(3) 0.0417(9) Uani 1 1 d . . .
O1B O 0.5894(4) 0.2547(2) 0.5938(3) 0.0373(8) Uani 1 1 d . . .
O1A O 0.7903(3) 0.3015(2) 0.6980(3) 0.0405(9) Uani 1 1 d . . .
O2H O 0.5888(4) 0.32190(19) 0.7744(3) 0.0384(8) Uani 1 1 d . . .
N2B N 0.6954(4) 0.0612(2) 0.6424(3) 0.0306(8) Uani 1 1 d . . .
O2A O 0.9674(4) 0.3450(2) 0.7086(4) 0.0552(13) Uani 1 1 d . . .
C1A C 0.8995(5) 0.2969(3) 0.7072(4) 0.0356(11) Uani 1 1 d . . .
C2A C 0.9464(5) 0.2245(3) 0.7164(4) 0.0332(10) Uani 1 1 d . . .
C5A C 1.0109(5) 0.0940(3) 0.7346(4) 0.0324(10) Uani 1 1 d . . .
O2B O 0.5438(4) 0.2402(2) 0.4415(3) 0.0467(10) Uani 1 1 d . . .
O3B O 0.7728(4) -0.0634(2) 0.6882(3) 0.0372(8) Uani 1 1 d . . .
C1B C 0.5794(5) 0.2194(3) 0.5226(4) 0.0327(10) Uani 1 1 d . . .
C2B C 0.6150(5) 0.1447(3) 0.5358(4) 0.0352(10) Uani 1 1 d . . .
C5B C 0.6780(6) 0.0145(3) 0.5754(4) 0.0372(12) Uani 1 1 d . . .
C3A C 1.0570(5) 0.2082(3) 0.7021(5) 0.0448(15) Uani 1 1 d . . .
H3A H 1.1066 0.2420 0.6887 0.054 Uiso 1 1 calc R . .
C4A C 1.0881(5) 0.1404(3) 0.7087(5) 0.0430(13) Uani 1 1 d . . .
H4A H 1.1581 0.1256 0.6965 0.052 Uiso 1 1 calc R . .
C6A C 1.0417(5) 0.0187(3) 0.7517(5) 0.0386(12) Uani 1 1 d . . .
O4A O 1.1303(5) -0.0030(3) 0.7310(5) 0.0627(16) Uani 1 1 d . . .
C6B C 0.7156(6) -0.0581(3) 0.6066(4) 0.0384(11) Uani 1 1 d . . .
O4B O 0.6868(6) -0.1055(2) 0.5514(3) 0.0645(16) Uani 1 1 d . . .
C3B C 0.5971(7) 0.0978(3) 0.4624(4) 0.0489(16) Uani 1 1 d . . .
H3B H 0.5652 0.1117 0.4023 0.059 Uiso 1 1 calc R . .
C4B C 0.6287(8) 0.0302(3) 0.4832(4) 0.0527(17) Uani 1 1 d . . .
H4B H 0.6177 -0.0035 0.4377 0.063 Uiso 1 1 calc R . .
C1C C 0.6506(4) 0.1378(2) 0.8906(4) 0.0293(9) Uani 1 1 d . . .
C2C C 0.6496(4) 0.0873(2) 0.9654(4) 0.0295(9) Uani 1 1 d . . .
C3C C 0.6076(5) 0.1047(3) 1.0426(4) 0.0381(11) Uani 1 1 d . . .
H3C H 0.5797 0.1487 1.0502 0.046 Uiso 1 1 calc R . .
N1C N 0.6932(4) 0.0260(2) 0.9510(3) 0.0305(8) Uani 1 1 d . . .
N2C N 0.6893(4) -0.0251(2) 1.0127(3) 0.0340(9) Uani 1 1 d . . .
C4C C 0.6094(6) 0.0539(3) 1.1071(4) 0.0400(12) Uani 1 1 d . . .
H4C H 0.5875 0.0626 1.1622 0.048 Uiso 1 1 calc R . .
C5C C 0.6461(5) -0.0122(3) 1.0858(4) 0.0315(10) Uani 1 1 d . . .
O3C O 0.6942(5) -0.1263(2) 1.1375(4) 0.0528(12) Uani 1 1 d . . .
O4C O 0.5729(4) -0.0671(2) 1.2027(3) 0.0444(10) Uani 1 1 d . . .
O7H O 0.2862(8) 0.2393(10) 0.6035(10) 0.103(7) Uani 0.50 1 d P . .
O8H O 0.3635(8) 0.3541(5) 0.7554(11) 0.071(4) Uani 0.50 1 d P . .
O9H O 0.6195(4) 0.3770(2) 0.4412(3) 0.0409(9) Uani 1 1 d . . .
O10H O 0.4140(6) 0.3664(5) 0.5797(5) 0.097(3) Uani 1 1 d . . .
C6C C 0.6377(5) -0.0742(3) 1.1485(4) 0.0356(11) 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'
Lu Lu -0.4720 5.8584 '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 Lu1 O1C 135.46(13) . . ?
O6H Lu1 O5H 83.10(14) . . ?
O1C Lu1 O5H 82.13(14) . . ?
O6H Lu1 O3B 76.23(13) . . ?
O1C Lu1 O3B 134.92(13) . . ?
O5H Lu1 O3B 141.01(15) . . ?
O6H Lu1 O3A 78.57(14) . . ?
O1C Lu1 O3A 135.15(13) . . ?
O5H Lu1 O3A 73.31(16) . . ?
O3B Lu1 O3A 70.43(16) . . ?
O6H Lu1 O4H 82.73(14) . . ?
O1C Lu1 O4H 80.56(13) . . ?
O5H Lu1 O4H 137.60(15) . . ?
O3B Lu1 O4H 72.19(15) . . ?
O3A Lu1 O4H 141.15(15) . . ?
O6H Lu1 N2B 137.53(13) . . ?
O1C Lu1 N2B 72.93(13) . . ?
O5H Lu1 N2B 138.36(15) . . ?
O3B Lu1 N2B 64.54(13) . . ?
O3A Lu1 N2B 101.76(16) . . ?
O4H Lu1 N2B 70.71(14) . . ?
O6H Lu1 N2A 140.70(14) . . ?
O1C Lu1 N2A 73.48(12) . . ?
O5H Lu1 N2A 74.80(15) . . ?
O3B Lu1 N2A 101.30(15) . . ?
O3A Lu1 N2A 64.22(13) . . ?
O4H Lu1 N2A 134.69(14) . . ?
N2B Lu1 N2A 66.49(14) . . ?
O6H Lu1 N1C 72.26(13) . . ?
O1C Lu1 N1C 63.26(12) . . ?
O5H Lu1 N1C 67.28(14) . . ?
O3B Lu1 N1C 133.25(15) . . ?
O3A Lu1 N1C 132.94(16) . . ?
O4H Lu1 N1C 70.35(14) . . ?
N2B Lu1 N1C 124.71(14) . . ?
N2A Lu1 N1C 124.92(13) . . ?
O2H Lu2 O1A 78.70(14) . . ?
O2H Lu2 O1B 81.80(16) . . ?
O1A Lu2 O1B 71.58(16) . . ?
O2H Lu2 O1H 83.59(16) . . ?
O1A Lu2 O1H 142.44(15) . . ?
O1B Lu2 O1H 73.29(15) . . ?
O2H Lu2 O1C 130.48(14) . . ?
O1A Lu2 O1C 135.31(13) . . ?
O1B Lu2 O1C 135.65(13) . . ?
O1H Lu2 O1C 80.58(13) . . ?
O2H Lu2 O3H 77.43(16) . . ?
O1A Lu2 O3H 73.25(17) . . ?
O1B Lu2 O3H 141.91(15) . . ?
O1H Lu2 O3H 134.30(17) . . ?
O1C Lu2 O3H 81.00(14) . . ?
O2H Lu2 O2C 76.50(14) . . ?
O1A Lu2 O2C 136.02(16) . . ?
O1B Lu2 O2C 138.09(15) . . ?
O1H Lu2 O2C 69.03(15) . . ?
O1C Lu2 O2C 54.01(12) . . ?
O3H Lu2 O2C 66.27(15) . . ?
O2H Lu2 N1B 144.04(15) . . ?
O1A Lu2 N1B 102.22(16) . . ?
O1B Lu2 N1B 65.08(14) . . ?
O1H Lu2 N1B 74.13(16) . . ?
O1C Lu2 N1B 73.70(12) . . ?
O3H Lu2 N1B 137.84(14) . . ?
O2C Lu2 N1B 119.07(13) . . ?
O2H Lu2 N1A 137.82(14) . . ?
O1A Lu2 N1A 64.81(13) . . ?
O1B Lu2 N1A 104.53(15) . . ?
O1H Lu2 N1A 138.49(16) . . ?
O1C Lu2 N1A 72.96(12) . . ?
O3H Lu2 N1A 72.53(15) . . ?
O2C Lu2 N1A 115.67(13) . . ?
N1B Lu2 N1A 68.12(14) . . ?
O2H Lu2 C1C 102.73(15) . . ?
O1A Lu2 C1C 142.57(16) . . ?
O1B Lu2 C1C 145.84(15) . . ?
O1H Lu2 C1C 73.62(15) . . ?
O1C Lu2 C1C 27.75(13) . . ?
O3H Lu2 C1C 70.72(15) . . ?
O2C Lu2 C1C 26.28(13) . . ?
N1B Lu2 C1C 97.67(14) . . ?
N1A Lu2 C1C 94.61(14) . . ?
C6A O3A Lu1 127.5(3) . . ?
C5A N2A N1A 119.0(4) . . ?
C5A N2A Lu1 116.7(3) . . ?
N1A N2A Lu1 124.3(3) . . ?
C2A N1A N2A 119.7(4) . . ?
C2A N1A Lu2 115.8(3) . . ?
N2A N1A Lu2 124.5(3) . . ?
C1C O1C Lu1 129.0(3) . . ?
C1C O1C Lu2 96.4(3) . . ?
Lu1 O1C Lu2 134.50(15) . . ?
C2B N1B N2B 120.1(4) . . ?
C2B N1B Lu2 115.8(3) . . ?
N2B N1B Lu2 124.0(3) . . ?
C1C O2C Lu2 88.6(3) . . ?
C1B O1B Lu2 127.5(3) . . ?
C1A O1A Lu2 126.7(3) . . ?
C5B N2B N1B 119.3(4) . . ?
C5B N2B Lu1 115.8(3) . . ?
N1B N2B Lu1 125.0(3) . . ?
O2A C1A O1A 126.3(5) . . ?
O2A C1A C2A 118.9(5) . . ?
O1A C1A C2A 114.8(5) . . ?
N1A C2A C3A 123.3(5) . . ?
N1A C2A C1A 114.6(4) . . ?
C3A C2A C1A 122.1(5) . . ?
N2A C5A C4A 123.6(5) . . ?
N2A C5A C6A 114.9(5) . . ?
C4A C5A C6A 121.5(5) . . ?
C6B O3B Lu1 127.8(3) . . ?
O1B C1B O2B 126.2(5) . . ?
O1B C1B C2B 116.6(5) . . ?
O2B C1B C2B 117.2(5) . . ?
N1B C2B C3B 122.9(5) . . ?
N1B C2B C1B 114.8(5) . . ?
C3B C2B C1B 122.2(5) . . ?
N2B C5B C4B 123.2(5) . . ?
N2B C5B C6B 114.8(5) . . ?
C4B C5B C6B 122.1(5) . . ?
C4A C3A C2A 116.8(5) . . ?
C4A C3A H3A 121.6 . . ?
C2A C3A H3A 121.6 . . ?
C3A C4A C5A 117.4(5) . . ?
C3A C4A H4A 121.3 . . ?
C5A C4A H4A 121.3 . . ?
O4A C6A O3A 126.2(5) . . ?
O4A C6A C5A 118.3(5) . . ?
O3A C6A C5A 115.5(5) . . ?
O4B C6B O3B 126.4(5) . . ?
O4B C6B C5B 118.2(5) . . ?
O3B C6B C5B 115.4(5) . . ?
C4B C3B C2B 117.2(5) . . ?
C4B C3B H3B 121.4 . . ?
C2B C3B H3B 121.4 . . ?
C3B C4B C5B 117.3(6) . . ?
C3B C4B H4B 121.4 . . ?
C5B C4B H4B 121.4 . . ?
O2C C1C O1C 120.8(5) . . ?
O2C C1C C2C 121.7(5) . . ?
O1C C1C C2C 117.4(4) . . ?
O2C C1C Lu2 65.1(3) . . ?
O1C C1C Lu2 55.8(2) . . ?
C2C C1C Lu2 173.1(3) . . ?
N1C C2C C3C 124.9(5) . . ?
N1C C2C C1C 113.6(4) . . ?
C3C C2C C1C 121.6(4) . . ?
C4C C3C C2C 116.8(5) . . ?
C4C C3C H3C 121.6 . . ?
C2C C3C H3C 121.6 . . ?
C2C N1C N2C 118.0(4) . . ?
C2C N1C Lu1 116.4(3) . . ?
N2C N1C Lu1 125.5(3) . . ?
C5C N2C N1C 119.6(4) . . ?
C3C C4C C5C 116.9(5) . . ?
C3C C4C H4C 121.5 . . ?
C5C C4C H4C 121.5 . . ?
N2C C5C C4C 123.3(5) . . ?
N2C C5C C6C 116.1(5) . . ?
C4C C5C C6C 120.6(5) . . ?
O4C C6C O3C 127.1(5) . . ?
O4C C6C C5C 116.3(5) . . ?
O3C C6C C5C 116.6(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
Lu1 O6H 2.240(3) . ?
Lu1 O1C 2.299(3) . ?
Lu1 O5H 2.299(4) . ?
Lu1 O3B 2.307(4) . ?
Lu1 O3A 2.328(4) . ?
Lu1 O4H 2.362(4) . ?
Lu1 N2B 2.585(4) . ?
Lu1 N2A 2.586(4) . ?
Lu1 N1C 2.668(4) . ?
Lu2 O2H 2.265(4) . ?
Lu2 O1A 2.284(4) . ?
Lu2 O1B 2.302(4) . ?
Lu2 O1H 2.320(4) . ?
Lu2 O1C 2.329(3) . ?
Lu2 O3H 2.402(4) . ?
Lu2 O2C 2.538(4) . ?
Lu2 N1B 2.566(4) . ?
Lu2 N1A 2.565(4) . ?
Lu2 C1C 2.797(5) . ?
O3A C6A 1.266(7) . ?
N2A C5A 1.322(6) . ?
N2A N1A 1.345(5) . ?
N1A C2A 1.321(6) . ?
O1C C1C 1.311(6) . ?
N1B C2B 1.324(7) . ?
N1B N2B 1.349(6) . ?
O2C C1C 1.239(6) . ?
O1B C1B 1.246(7) . ?
O1A C1A 1.268(7) . ?
N2B C5B 1.330(7) . ?
O2A C1A 1.227(7) . ?
C1A C2A 1.506(7) . ?
C2A C3A 1.404(7) . ?
C5A C4A 1.395(7) . ?
C5A C6A 1.514(7) . ?
O2B C1B 1.253(6) . ?
O3B C6B 1.255(7) . ?
C1B C2B 1.511(7) . ?
C2B C3B 1.401(8) . ?
C5B C4B 1.399(8) . ?
C5B C6B 1.519(7) . ?
C3A C4A 1.365(8) . ?
C3A H3A 0.9300 . ?
C4A H4A 0.9300 . ?
C6A O4A 1.231(7) . ?
C6B O4B 1.229(7) . ?
C3B C4B 1.381(9) . ?
C3B H3B 0.9300 . ?
C4B H4B 0.9300 . ?
C1C C2C 1.485(7) . ?
C2C N1C 1.333(6) . ?
C2C C3C 1.393(7) . ?
C3C C4C 1.373(8) . ?
C3C H3C 0.9300 . ?
N1C N2C 1.360(6) . ?
N2C C5C 1.326(7) . ?
C4C C5C 1.414(8) . ?
C4C H4C 0.9300 . ?
C5C C6C 1.540(7) . ?
O3C C6C 1.243(7) . ?
O4C C6C 1.239(7) . ?
