#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:15:50 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180384 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/53/7205382.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_7205382
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         'C18 H17 La O13, H2 O'
_chemical_formula_sum            'C18 H19 La O14'
_chemical_formula_weight         598.24
_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                68.4154(10)
_cell_angle_beta                 89.3378(11)
_cell_angle_gamma                72.780(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5147(2)
_cell_length_b                   10.2584(2)
_cell_length_c                   12.4540(5)
_cell_measurement_reflns_used    4226
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.27
_cell_volume                     960.38(5)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo and Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. φ anf 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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0528
_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            16654
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_T_max  0.8022
_exptl_absorpt_correction_T_min  0.5963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.932
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0531P)²+2.6625P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                3924
_reflns_number_total             4565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00474J.TXT
_cod_data_source_block           8
_cod_original_cell_volume        960.37(5)
_cod_database_code               7205382
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
La La 0.84466(3) 1.17822(2) 0.263756(18) 0.01304(8) Uani 1 1 d . . .
O1 O 0.6548(4) 1.0446(3) 0.2267(2) 0.0183(6) Uani 1 1 d . . .
O2 O 0.8755(4) 1.0299(3) 0.1320(2) 0.0180(6) Uani 1 1 d . . .
C3 C 0.7444(5) 0.9991(4) 0.1572(3) 0.0130(7) Uani 1 1 d . . .
C4 C 0.6935(5) 0.9040(4) 0.1064(3) 0.0128(7) Uani 1 1 d . . .
C5 C 0.7834(5) 0.8606(4) 0.0252(3) 0.0139(7) Uani 1 1 d . . .
H5 H 0.8752 0.8937 -0.0010 0.017 Uiso 1 1 calc R . .
C6 C 0.7371(5) 0.7671(4) -0.0177(3) 0.0149(8) Uani 1 1 d . . .
C7 C 0.8331(6) 0.7168(5) -0.1041(4) 0.0198(9) Uani 1 1 d . . .
O8 O 0.8996(3) 0.8014(3) -0.1754(2) 0.0181(6) Uani 1 1 d . . .
O9A O 0.8033(10) 0.6086(8) -0.1189(6) 0.0171(14) Uani 0.50 1 d P . .
O9B O 0.8815(10) 0.5753(8) -0.0852(7) 0.0201(15) Uani 0.50 1 d P . .
C10 C 0.6026(5) 0.7192(4) 0.0206(3) 0.0154(8) Uani 1 1 d . . .
H10 H 0.5741 0.6532 -0.0067 0.018 Uiso 1 1 calc R . .
C11 C 0.5100(5) 0.7679(4) 0.0987(3) 0.0140(7) Uani 1 1 d . . .
C12 C 0.5544(5) 0.8589(4) 0.1428(3) 0.0140(7) Uani 1 1 d . . .
H12 H 0.4917 0.8907 0.1972 0.017 Uiso 1 1 calc R . .
O13 O 0.3759(4) 0.7173(3) 0.1269(2) 0.0171(6) Uani 1 1 d . . .
C14 C 0.2674(5) 0.7667(5) 0.2039(3) 0.0176(8) Uani 1 1 d . . .
H14A H 0.1592 0.7531 0.1931 0.021 Uiso 1 1 calc R . .
H14B H 0.2487 0.8734 0.1830 0.021 Uiso 1 1 calc R . .
C15 C 0.3364(5) 0.6848(4) 0.3292(3) 0.0176(8) Uani 1 1 d . . .
H15A H 0.4414 0.7028 0.3419 0.021 Uiso 1 1 calc R . .
H15B H 0.2574 0.7210 0.3786 0.021 Uiso 1 1 calc R . .
O16 O 0.3659(4) 0.5279(3) 0.3612(2) 0.0185(6) Uani 1 1 d . . .
C17 C 0.2886(5) 0.4584(4) 0.4531(3) 0.0144(8) Uani 1 1 d . . .
C18 C 0.2592(5) 0.4993(4) 0.5484(3) 0.0151(8) Uani 1 1 d . . .
H18 H 0.2989 0.5735 0.5552 0.018 Uiso 1 1 calc R . .
C19 C 0.1709(5) 0.4297(4) 0.6335(3) 0.0146(8) Uani 1 1 d . . .
C20 C 0.1231(5) 0.4872(4) 0.7266(3) 0.0165(8) Uani 1 1 d . . .
O21 O 0.1930(4) 0.5655(3) 0.7488(2) 0.0211(6) Uani 1 1 d . . .
O22 O -0.0018(4) 0.4535(3) 0.7788(2) 0.0204(6) Uani 1 1 d . . .
H22 H -0.0582 0.5181 0.8210 0.025 Uiso 1 1 d R . .
C23 C 0.1149(5) 0.3183(4) 0.6253(3) 0.0143(8) Uani 1 1 d . . .
H23 H 0.0539 0.2719 0.6832 0.017 Uiso 1 1 calc R . .
C24 C 0.1494(5) 0.2764(4) 0.5314(3) 0.0149(8) Uani 1 1 d . . .
C25 C 0.0709(5) 0.1708(4) 0.5138(3) 0.0176(8) Uani 1 1 d . . .
O26 O 0.0208(4) 0.0879(3) 0.6018(2) 0.0172(6) Uani 1 1 d . . .
O27 O 0.0522(4) 0.1760(3) 0.4126(2) 0.0215(6) Uani 1 1 d . . .
C28 C 0.2373(5) 0.3454(4) 0.4458(3) 0.0173(8) Uani 1 1 d . . .
H28 H 0.2620 0.3150 0.3825 0.021 Uiso 1 1 calc R . .
O29 O 0.7602(4) 1.3514(3) 0.0481(2) 0.0191(6) Uani 1 1 d . . .
H29A H 0.7690 1.4426 0.0036 0.023 Uiso 1 1 d R . .
H29B H 0.7353 1.3091 -0.0109 0.023 Uiso 1 1 d R . .
O30 O 0.5313(4) 1.3318(3) 0.2401(3) 0.0229(6) Uani 1 1 d . . .
H30A H 0.4868 1.4322 0.2245 0.028 Uiso 1 1 d R . .
H30B H 0.4463 1.3007 0.2227 0.028 Uiso 1 1 d R . .
O31 O 0.7302(4) 1.1434(4) 0.4614(3) 0.0275(7) Uani 1 1 d . . .
H31A H 0.8104 1.1129 0.5219 0.033 Uiso 1 1 d R . .
H31B H 0.6418 1.1120 0.4892 0.033 Uiso 1 1 d R . .
O32A O 0.3999(12) 1.0601(10) 0.3563(9) 0.034(2) Uani 0.56 1 d P . .
O32B O 0.402(2) 0.9958(13) 0.3639(14) 0.049(4) Uani 0.44 1 d P . .
H32A H 0.4784 1.0405 0.3151 0.074 Uiso 1 1 d R . .
H32B H 0.2919 1.1368 0.3242 0.074 Uiso 1 1 d R . .
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'
La La -0.2871 2.4523 '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
O8 La O21 84.20(10) 2_775 2_676 ?
O8 La O26 93.20(9) 2_775 2_666 ?
O21 La O26 140.68(9) 2_676 2_666 ?
O8 La O1 126.80(9) 2_775 . ?
O21 La O1 135.01(10) 2_676 . ?
O26 La O1 76.17(9) 2_666 . ?
O8 La O27 70.81(9) 2_775 1_665 ?
O21 La O27 69.49(9) 2_676 1_665 ?
O26 La O27 72.63(9) 2_666 1_665 ?
O1 La O27 145.07(9) . 1_665 ?
O8 La O31 139.13(10) 2_775 . ?
O21 La O31 84.13(10) 2_676 . ?
O26 La O31 72.41(10) 2_666 . ?
O1 La O31 87.59(10) . . ?
O27 La O31 68.41(10) 1_665 . ?
O8 La O29 72.79(9) 2_775 . ?
O21 La O29 72.83(9) 2_676 . ?
O26 La O29 143.44(9) 2_666 . ?
O1 La O29 85.51(9) . . ?
O27 La O29 129.28(9) 1_665 . ?
O31 La O29 138.85(10) . . ?
O8 La O2 75.94(9) 2_775 . ?
O21 La O2 140.45(9) 2_676 . ?
O26 La O2 75.17(9) 2_666 . ?
O1 La O2 50.87(9) . . ?
O27 La O2 131.55(10) 1_665 . ?
O31 La O2 132.28(10) . . ?
O29 La O2 68.76(9) . . ?
O8 La O30 140.05(10) 2_775 . ?
O21 La O30 68.05(10) 2_676 . ?
O26 La O30 126.53(9) 2_666 . ?
O1 La O30 67.86(9) . . ?
O27 La O30 120.76(10) 1_665 . ?
O31 La O30 67.97(10) . . ?
O29 La O30 71.87(9) . . ?
O2 La O30 107.42(9) . . ?
O8 La C3 101.19(10) 2_775 . ?
O21 La C3 145.07(10) 2_676 . ?
O26 La C3 73.97(9) 2_666 . ?
O1 La C3 25.62(10) . . ?
O27 La C3 145.03(10) 1_665 . ?
O31 La C3 110.55(10) . . ?
O29 La C3 75.93(9) . . ?
O2 La C3 25.25(10) . . ?
O30 La C3 87.76(10) . . ?
C3 O1 La 94.4(2) . . ?
C3 O2 La 93.3(2) . . ?
O2 C3 O1 121.4(3) . . ?
O2 C3 C4 119.4(3) . . ?
O1 C3 C4 119.1(3) . . ?
O2 C3 La 61.42(19) . . ?
O1 C3 La 60.00(19) . . ?
C4 C3 La 178.2(2) . . ?
C5 C4 C12 120.6(3) . . ?
C5 C4 C3 120.2(3) . . ?
C12 C4 C3 119.2(3) . . ?
C4 C5 C6 119.1(4) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C10 C6 C5 120.4(4) . . ?
C10 C6 C7 119.3(3) . . ?
C5 C6 C7 120.3(4) . . ?
O8 C7 O9A 123.5(5) . . ?
O8 C7 O9B 120.1(5) . . ?
O8 C7 C6 118.8(3) . . ?
O9A C7 C6 115.0(5) . . ?
O9B C7 C6 118.8(4) . . ?
C7 O8 La 145.3(3) . 2_775 ?
O9B O9A C7 76.6(10) . . ?
O9A O9B C7 71.8(10) . . ?
C11 C10 C6 119.9(3) . . ?
C11 C10 H10 120.0 . . ?
C6 C10 H10 120.0 . . ?
O13 C11 C12 124.8(4) . . ?
O13 C11 C10 114.7(3) . . ?
C12 C11 C10 120.6(4) . . ?
C11 C12 C4 119.3(4) . . ?
C11 C12 H12 120.3 . . ?
C4 C12 H12 120.3 . . ?
C11 O13 C14 119.0(3) . . ?
O13 C14 C15 112.5(3) . . ?
O13 C14 H14A 109.1 . . ?
C15 C14 H14A 109.1 . . ?
O13 C14 H14B 109.1 . . ?
C15 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
O16 C15 C14 109.8(3) . . ?
O16 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
O16 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 O16 C15 117.2(3) . . ?
O16 C17 C28 116.7(3) . . ?
O16 C17 C18 122.9(3) . . ?
C28 C17 C18 120.4(4) . . ?
C19 C18 C17 119.1(4) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C23 C19 C18 120.8(4) . . ?
C23 C19 C20 120.7(4) . . ?
C18 C19 C20 118.2(3) . . ?
O21 C20 O22 123.3(4) . . ?
O21 C20 C19 121.8(4) . . ?
O22 C20 C19 114.8(3) . . ?
C20 O21 La 143.6(3) . 2_676 ?
C20 O22 H22 114.6 . . ?
C24 C23 C19 119.2(4) . . ?
C24 C23 H23 120.4 . . ?
C19 C23 H23 120.4 . . ?
C23 C24 C28 120.4(4) . . ?
C23 C24 C25 119.3(4) . . ?
C28 C24 C25 119.7(3) . . ?
O27 C25 O26 124.6(4) . . ?
O27 C25 C24 117.6(4) . . ?
O26 C25 C24 117.8(3) . . ?
C25 O26 La 130.8(3) . 2_666 ?
C25 O27 La 143.2(3) . 1_445 ?
C17 C28 C24 120.0(4) . . ?
C17 C28 H28 120.0 . . ?
C24 C28 H28 120.0 . . ?
La O29 H29A 134.1 . . ?
La O29 H29B 119.1 . . ?
H29A O29 H29B 105.1 . . ?
La O30 H30A 127.4 . . ?
La O30 H30B 122.9 . . ?
H30A O30 H30B 107.1 . . ?
La O31 H31A 113.6 . . ?
La O31 H31B 129.6 . . ?
H31A O31 H31B 109.4 . . ?
H32A O32A H32B 124.0 . . ?
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
La O8 2.457(3) 2_775 ?
La O21 2.498(3) 2_676 ?
La O26 2.530(3) 2_666 ?
La O1 2.549(3) . ?
La O27 2.566(3) 1_665 ?
La O31 2.577(3) . ?
La O29 2.582(3) . ?
La O2 2.582(3) . ?
La O30 2.622(3) . ?
La C3 2.935(4) . ?
O1 C3 1.273(5) . ?
O2 C3 1.254(5) . ?
C3 C4 1.501(5) . ?
C4 C5 1.384(5) . ?
C4 C12 1.407(5) . ?
C5 C6 1.402(5) . ?
C5 H5 0.9500 . ?
C6 C10 1.388(6) . ?
C6 C7 1.494(5) . ?
C7 O8 1.255(5) . ?
C7 O9A 1.284(8) . ?
C7 O9B 1.315(8) . ?
O8 La 2.457(3) 2_775 ?
O9A O9B 0.708(7) . ?
C10 C11 1.387(6) . ?
C10 H10 0.9500 . ?
C11 O13 1.380(5) . ?
C11 C12 1.382(5) . ?
C12 H12 0.9500 . ?
O13 C14 1.446(5) . ?
C14 C15 1.500(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 O16 1.450(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
O16 C17 1.382(5) . ?
C17 C28 1.386(5) . ?
C17 C18 1.395(5) . ?
C18 C19 1.393(6) . ?
C18 H18 0.9500 . ?
C19 C23 1.397(5) . ?
C19 C20 1.486(5) . ?
C20 O21 1.236(5) . ?
C20 O22 1.307(5) . ?
O21 La 2.498(3) 2_676 ?
O22 H22 1.0042 . ?
C23 C24 1.387(5) . ?
C23 H23 0.9500 . ?
C24 C28 1.392(6) . ?
C24 C25 1.508(5) . ?
C25 O27 1.252(5) . ?
C25 O26 1.274(5) . ?
O26 La 2.530(3) 2_666 ?
O27 La 2.566(3) 1_445 ?
C28 H28 0.9500 . ?
O29 H29A 0.9202 . ?
O29 H29B 1.0325 . ?
O30 H30A 0.9307 . ?
O30 H30B 0.9296 . ?
O31 H31A 0.9193 . ?
O31 H31B 0.9191 . ?
O32A O32B 0.625(11) . ?
O32A H32A 0.8595 . ?
O32A H32B 0.9862 . ?
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
O22 H22 O9B 1.00 1.51 2.491(8) 163 1_456
O22 H22 O9A 1.00 1.63 2.606(8) 163 1_456
O29 H29A O9B 0.92 1.91 2.767(8) 155 1_565
O29 H29A O9A 0.92 1.92 2.818(8) 165 1_565
O29 H29B O13 1.03 1.88 2.874(4) 161 2_675
O30 H30A O16 0.93 2.35 2.968(4) 124 1_565
O30 H30B O9A 0.93 2.25 3.026(8) 141 2_675
O31 H31A O26 0.92 1.96 2.836(4) 158 1_665
O31 H31B O32B 0.92 1.86 2.580(15) 134 2_676
O31 H31B O32A 0.92 2.19 2.927(10) 136 2_676
O32A H32A O1 0.86 1.85 2.691(10) 164 .
O32A H32B O8 0.99 2.26 3.038(11) 135 2_675
O32A H32B O27 0.99 2.31 3.025(10) 129 1_565
