#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:15:50 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180384 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/53/7205383.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_7205383
loop_
_publ_author_name
'Karmakar, Anirban'
'Goldberg, Israel'
_publ_section_title
;
 Coordination polymers of flexible tetracarboxylic acids with metal
 ions. I. Synthesis of CH2- and (CH2)2-spaced bis(oxy)isophthalic acid
 ligands, and structural characterization of their polymeric adducts
 with lanthanoid ions
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              339
_journal_paper_doi               10.1039/c0ce00474j
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         '2(C18 H15 Nd O12), 4(H2 O), 3(O)'
_chemical_formula_sum            'C36 H38 Nd2 O31'
_chemical_formula_weight         1255.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.5960(15)
_cell_angle_beta                 94.8827(14)
_cell_angle_gamma                93.4052(16)
_cell_formula_units_Z            1
_cell_length_a                   8.5679(3)
_cell_length_b                   9.9939(3)
_cell_length_c                   12.5472(5)
_cell_measurement_reflns_used    3561
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.39
_cell_volume                     1068.00(7)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. ω scans'
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10107
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.514
_exptl_absorpt_correction_T_max  0.7043
_exptl_absorpt_correction_T_min  0.5193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             622
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.068
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0815P)²+1.1382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                4113
_reflns_number_total             4997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00474J.TXT
_cod_data_source_block           9
_cod_database_code               7205383
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Nd Nd 0.40284(3) 0.60355(3) -0.32267(2) 0.01608(12) Uani 1 1 d . . .
O1 O 0.3606(5) 0.7364(4) -0.1512(3) 0.0249(9) Uani 1 1 d . . .
O2 O 0.4736(5) 0.8404(4) -0.2797(3) 0.0220(9) Uani 1 1 d . . .
C3 C 0.4074(6) 0.8437(5) -0.1938(4) 0.0165(11) Uani 1 1 d . . .
C4 C 0.3791(6) 0.9766(5) -0.1429(4) 0.0166(11) Uani 1 1 d . . .
C5 C 0.4200(6) 1.0912(5) -0.1985(4) 0.0166(11) Uani 1 1 d . . .
H5 H 0.4685 1.0844 -0.2636 0.020 Uiso 1 1 calc R . .
C6 C 0.3872(6) 1.2166(5) -0.1551(4) 0.0169(11) Uani 1 1 d . . .
C7 C 0.4155(7) 1.3422(5) -0.2153(4) 0.0173(11) Uani 1 1 d . . .
O8 O 0.5051(5) 1.3488(4) -0.2905(3) 0.0177(8) Uani 1 1 d . . .
O9 O 0.3420(5) 1.4428(4) -0.1876(3) 0.0208(8) Uani 1 1 d . . .
C10 C 0.3183(6) 1.2250(5) -0.0598(5) 0.0174(11) Uani 1 1 d . . .
H10 H 0.2970 1.3101 -0.0309 0.021 Uiso 1 1 calc R . .
C11 C 0.2795(6) 1.1085(6) -0.0056(4) 0.0181(11) Uani 1 1 d . . .
C12 C 0.3100(6) 0.9834(5) -0.0473(4) 0.0174(11) Uani 1 1 d . . .
H12 H 0.2839 0.9041 -0.0109 0.021 Uiso 1 1 calc R . .
O13 O 0.2120(5) 1.1297(4) 0.0893(3) 0.0228(9) Uani 1 1 d . . .
C14 C 0.1574(7) 1.0121(6) 0.1407(5) 0.0210(12) Uani 1 1 d . . .
H14A H 0.2475 0.9627 0.1697 0.025 Uiso 1 1 calc R . .
H14B H 0.0912 0.9522 0.0888 0.025 Uiso 1 1 calc R . .
C15 C 0.0636(7) 1.0563(5) 0.2296(5) 0.0194(11) Uani 1 1 d . . .
H15A H 0.1295 1.1134 0.2837 0.023 Uiso 1 1 calc R . .
H15B H -0.0266 1.1064 0.2018 0.023 Uiso 1 1 calc R . .
O16 O 0.0117(5) 0.9316(4) 0.2739(3) 0.0218(8) Uani 1 1 d . . .
C17 C -0.0865(6) 0.9348(5) 0.3542(4) 0.0167(11) Uani 1 1 d . . .
C18 C -0.1359(6) 0.8085(5) 0.3881(4) 0.0170(11) Uani 1 1 d . . .
H18 H -0.0991 0.7300 0.3568 0.020 Uiso 1 1 calc R . .
C19 C -0.2385(6) 0.7974(5) 0.4677(4) 0.0143(10) Uani 1 1 d . . .
C20 C -0.2988(6) 0.6578(5) 0.4958(4) 0.0147(10) Uani 1 1 d . . .
O21 O -0.2564(5) 0.5590(4) 0.4439(3) 0.0178(8) Uani 1 1 d . . .
O22 O -0.3889(5) 0.6474(4) 0.5694(3) 0.0213(8) Uani 1 1 d . . .
C23 C -0.2918(6) 0.9122(5) 0.5161(4) 0.0160(10) Uani 1 1 d . . .
H23 H -0.3600 0.9050 0.5718 0.019 Uiso 1 1 calc R . .
C24 C -0.2419(6) 1.0374(5) 0.4802(4) 0.0146(10) Uani 1 1 d . . .
C25 C -0.2959(6) 1.1641(5) 0.5273(4) 0.0165(11) Uani 1 1 d . . .
O26 O -0.2879(5) 1.2708(4) 0.4820(3) 0.0200(8) Uani 1 1 d . . .
O27 O -0.3528(5) 1.1500(4) 0.6208(3) 0.0209(8) Uani 1 1 d . . .
H27 H -0.3986 1.2189 0.6366 0.031 Uiso 1 1 calc R . .
C28 C -0.1398(6) 1.0490(5) 0.3993(4) 0.0166(11) Uani 1 1 d . . .
H28 H -0.1074 1.1349 0.3756 0.020 Uiso 1 1 calc R . .
O29 O 0.1188(5) 0.6319(4) -0.2962(3) 0.0219(9) Uani 1 1 d . . .
H29A H 0.1037 0.6455 -0.2266 0.033 Uiso 1 1 d R . .
H29B H 0.0372 0.5855 -0.3329 0.033 Uiso 1 1 d R . .
O30 O 0.6592(5) 0.6015(4) -0.2027(3) 0.0226(9) Uani 1 1 d . . .
H30A H 0.7077 0.6820 -0.1841 0.034 Uiso 1 1 d R . .
H30B H 0.6497 0.5482 -0.1468 0.034 Uiso 1 1 d R . .
O31 O 0.3264(7) 0.5686(5) 0.0385(4) 0.0450(13) Uani 1 1 d . . .
H31A H 0.4086 0.6153 0.0157 0.068 Uiso 1 1 d R . .
H31B H 0.2430 0.5515 -0.0096 0.068 Uiso 1 1 d R . .
O32 O 0.1382(5) 0.5459(4) 0.3399(4) 0.0281(10) Uani 1 1 d . . .
H32A H 0.1823 0.4780 0.3075 0.042 Uiso 1 1 d R . .
H32B H 0.0646 0.5832 0.2968 0.042 Uiso 1 1 d R . .
O33A O 0.0516(13) 0.5723(11) 0.9185(9) 0.046(3) Uiso 0.75 1 d P A 1
O33B O -0.0698(17) 0.3143(15) 0.8487(12) 0.050(3) Uiso 0.75 1 d P B 2
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'
Nd Nd -0.1943 3.0179 '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'
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
O22 Nd O21 96.48(14) 1_654 2_565 ?
O22 Nd O9 136.20(13) 1_654 1_545 ?
O21 Nd O9 83.75(13) 2_565 1_545 ?
O22 Nd O2 78.05(13) 1_654 . ?
O21 Nd O2 146.81(13) 2_565 . ?
O9 Nd O2 122.85(13) 1_545 . ?
O22 Nd O29 146.71(13) 1_654 . ?
O21 Nd O29 74.50(13) 2_565 . ?
O9 Nd O29 75.63(13) 1_545 . ?
O2 Nd O29 92.10(13) . . ?
O22 Nd O26 74.01(13) 1_654 2_575 ?
O21 Nd O26 72.42(12) 2_565 2_575 ?
O9 Nd O26 144.35(14) 1_545 2_575 ?
O2 Nd O26 74.63(13) . 2_575 ?
O29 Nd O26 72.72(13) . 2_575 ?
O22 Nd O30 72.42(14) 1_654 . ?
O21 Nd O30 134.06(13) 2_565 . ?
O9 Nd O30 76.38(14) 1_545 . ?
O2 Nd O30 75.99(13) . . ?
O29 Nd O30 136.35(13) . . ?
O26 Nd O30 139.01(13) 2_575 . ?
O22 Nd O1 124.90(14) 1_654 . ?
O21 Nd O1 137.77(13) 2_565 . ?
O9 Nd O1 72.35(12) 1_545 . ?
O2 Nd O1 52.21(12) . . ?
O29 Nd O1 66.22(14) . . ?
O26 Nd O1 108.37(13) 2_575 . ?
O30 Nd O1 73.73(14) . . ?
O22 Nd O8 89.25(12) 1_654 1_545 ?
O21 Nd O8 69.10(12) 2_565 1_545 ?
O9 Nd O8 49.80(11) 1_545 1_545 ?
O2 Nd O8 142.37(13) . 1_545 ?
O29 Nd O8 115.71(12) . 1_545 ?
O26 Nd O8 135.71(12) 2_575 1_545 ?
O30 Nd O8 66.39(12) . 1_545 ?
O1 Nd O8 114.69(12) . 1_545 ?
O22 Nd C3 102.84(15) 1_654 . ?
O21 Nd C3 148.54(14) 2_565 . ?
O9 Nd C3 98.56(14) 1_545 . ?
O2 Nd C3 26.09(14) . . ?
O29 Nd C3 75.74(15) . . ?
O26 Nd C3 89.22(14) 2_575 . ?
O30 Nd C3 76.11(14) . . ?
O1 Nd C3 26.44(13) . . ?
O8 Nd C3 134.88(13) 1_545 . ?
O22 Nd C7 113.59(14) 1_654 1_545 ?
O21 Nd C7 73.97(14) 2_565 1_545 ?
O9 Nd C7 24.72(13) 1_545 1_545 ?
O2 Nd C7 138.41(14) . 1_545 ?
O29 Nd C7 94.96(14) . 1_545 ?
O26 Nd C7 146.20(14) 2_575 1_545 ?
O30 Nd C7 70.78(14) . 1_545 ?
O1 Nd C7 94.10(13) . 1_545 ?
O8 Nd C7 25.14(13) 1_545 1_545 ?
C3 Nd C7 118.79(15) . 1_545 ?
C3 O1 Nd 89.7(3) . . ?
C3 O2 Nd 95.5(3) . . ?
O2 C3 O1 121.1(5) . . ?
O2 C3 C4 119.4(5) . . ?
O1 C3 C4 119.5(5) . . ?
O2 C3 Nd 58.5(3) . . ?
O1 C3 Nd 63.8(3) . . ?
C4 C3 Nd 167.2(4) . . ?
C12 C4 C5 122.3(5) . . ?
C12 C4 C3 120.7(5) . . ?
C5 C4 C3 117.0(5) . . ?
C4 C5 C6 118.1(5) . . ?
C4 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
C10 C6 C5 120.3(5) . . ?
C10 C6 C7 118.9(5) . . ?
C5 C6 C7 120.6(5) . . ?
O8 C7 O9 121.2(5) . . ?
O8 C7 C6 122.7(5) . . ?
O9 C7 C6 116.1(5) . . ?
O8 C7 Nd 68.3(3) . 1_565 ?
O9 C7 Nd 53.1(3) . 1_565 ?
C6 C7 Nd 167.7(4) . 1_565 ?
C7 O8 Nd 86.5(3) . 1_565 ?
C7 O9 Nd 102.2(3) . 1_565 ?
C6 C10 C11 120.4(5) . . ?
C6 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
O13 C11 C12 124.7(5) . . ?
O13 C11 C10 115.1(5) . . ?
C12 C11 C10 120.2(5) . . ?
C4 C12 C11 118.7(5) . . ?
C4 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C11 O13 C14 116.0(4) . . ?
O13 C14 C15 107.6(4) . . ?
O13 C14 H14A 110.2 . . ?
C15 C14 H14A 110.2 . . ?
O13 C14 H14B 110.2 . . ?
C15 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O16 C15 C14 103.1(4) . . ?
O16 C15 H15A 111.1 . . ?
C14 C15 H15A 111.1 . . ?
O16 C15 H15B 111.1 . . ?
C14 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C17 O16 C15 118.7(4) . . ?
O16 C17 C28 125.6(5) . . ?
O16 C17 C18 114.2(5) . . ?
C28 C17 C18 120.2(5) . . ?
C19 C18 C17 120.1(5) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C23 120.7(5) . . ?
C18 C19 C20 118.1(5) . . ?
C23 C19 C20 121.1(5) . . ?
O22 C20 O21 123.5(5) . . ?
O22 C20 C19 118.2(5) . . ?
O21 C20 C19 118.3(5) . . ?
C20 O21 Nd 131.4(3) . 2_565 ?
C20 O22 Nd 167.1(4) . 1_456 ?
C24 C23 C19 118.2(5) . . ?
C24 C23 H23 120.9 . . ?
C19 C23 H23 120.9 . . ?
C23 C24 C28 121.3(5) . . ?
C23 C24 C25 121.1(5) . . ?
C28 C24 C25 117.6(4) . . ?
O26 C25 O27 123.4(5) . . ?
O26 C25 C24 122.5(5) . . ?
O27 C25 C24 114.1(4) . . ?
C25 O26 Nd 143.5(4) . 2_575 ?
C25 O27 H27 109.5 . . ?
C17 C28 C24 119.5(5) . . ?
C17 C28 H28 120.2 . . ?
C24 C28 H28 120.2 . . ?
Nd O29 H29A 111.8 . . ?
Nd O29 H29B 124.8 . . ?
H29A O29 H29B 112.6 . . ?
Nd O30 H30A 116.2 . . ?
Nd O30 H30B 112.0 . . ?
H30A O30 H30B 113.1 . . ?
H31A O31 H31B 116.4 . . ?
H32A O32 H32B 113.0 . . ?
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
Nd O22 2.359(4) 1_654 ?
Nd O21 2.413(4) 2_565 ?
Nd O9 2.434(4) 1_545 ?
Nd O2 2.442(4) . ?
Nd O29 2.515(4) . ?
Nd O26 2.549(4) 2_575 ?
Nd O30 2.556(4) . ?
Nd O1 2.560(4) . ?
Nd O8 2.770(4) 1_545 ?
Nd C3 2.852(5) . ?
Nd C7 2.975(5) 1_545 ?
O1 C3 1.270(6) . ?
O2 C3 1.260(7) . ?
C3 C4 1.499(7) . ?
C4 C12 1.385(8) . ?
C4 C5 1.399(7) . ?
C5 C6 1.406(7) . ?
C5 H5 0.9500 . ?
C6 C10 1.381(8) . ?
C6 C7 1.501(7) . ?
C7 O8 1.266(7) . ?
C7 O9 1.273(6) . ?
C7 Nd 2.975(5) 1_565 ?
O8 Nd 2.770(4) 1_565 ?
O9 Nd 2.434(4) 1_565 ?
C10 C11 1.402(7) . ?
C10 H10 0.9500 . ?
C11 O13 1.384(7) . ?
C11 C12 1.390(8) . ?
C12 H12 0.9500 . ?
O13 C14 1.429(6) . ?
C14 C15 1.501(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 O16 1.441(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
O16 C17 1.367(7) . ?
C17 C28 1.379(7) . ?
C17 C18 1.397(7) . ?
C18 C19 1.388(8) . ?
C18 H18 0.9500 . ?
C19 C23 1.401(7) . ?
C19 C20 1.520(7) . ?
C20 O22 1.256(6) . ?
C20 O21 1.256(6) . ?
O21 Nd 2.413(4) 2_565 ?
O22 Nd 2.359(4) 1_456 ?
C23 C24 1.397(7) . ?
C23 H23 0.9500 . ?
C24 C28 1.398(8) . ?
C24 C25 1.497(7) . ?
C25 O26 1.224(6) . ?
C25 O27 1.316(7) . ?
O26 Nd 2.549(4) 2_575 ?
O27 H27 0.8400 . ?
C28 H28 0.9500 . ?
O29 H29A 0.9011 . ?
O29 H29B 0.9008 . ?
O30 H30A 0.8989 . ?
O30 H30B 0.8991 . ?
O31 H31A 0.8934 . ?
O31 H31B 0.8999 . ?
O32 H32A 0.8998 . ?
O32 H32B 0.8998 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O27 H27 O8 0.84 1.84 2.658(5) 163 1_456
O29 H29A O33A 0.90 2.05 2.873(12) 150 1_554
O29 H29B O32 0.90 1.93 2.754(6) 151 2_565
O30 H30A O13 0.90 2.24 3.103(6) 161 2_675
O30 H30B O31 0.90 1.82 2.707(6) 168 2_665
O31 H31A O1 0.89 2.46 2.974(6) 117 .
O31 H31B O33A 0.90 1.83 2.688(6) 159 1_554
O32 H32A O30 0.90 2.14 2.970(6) 153 2_665
O32 H32B O33B 0.90 2.12 2.817(7) 134 2_566
