#------------------------------------------------------------------------------
#$Date: 2019-02-23 05:43:31 +0200 (Sat, 23 Feb 2019) $
#$Revision: 213810 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242857.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2242857
loop_
_publ_author_name
'Camara, Magatte'
'Badiane, Insa'
'Diallo, Mamoudou'
'Daiguebonne, Carole'
'Guillou, Olivier'
_publ_section_title
;
 Synthesis and crystal structure of a new coordination polymer based on
 lanthanum and 1,4-phenylenediacetate ligands
;
_journal_coeditor_code           VN2143
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              378
_journal_page_last               382
_journal_paper_doi               10.1107/S2056989019002378
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[La2 (C10 H8 O4)3 (H2 O1)4], 8H2 O'
_chemical_formula_moiety         'C30 H32 La2 O16, 8(H2 O)'
_chemical_formula_sum            'C30 H48 La2 O24'
_chemical_formula_weight         1070.05
_chemical_name_systematic
;
Poly[[tetraaquatris(μ-1,4-phenylenediacetato)dilanthanum(III)] octahydrate]
;
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.0490(10)
_cell_angle_beta                 107.7290(10)
_cell_angle_gamma                106.6220(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1197(2)
_cell_length_b                   11.1231(2)
_cell_length_c                   11.9434(2)
_cell_measurement_reflns_used    15558
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1005.21(4)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Bruker, 2004)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2001)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4588
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         3.611
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.759
_refine_diff_density_min         -0.646
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0308P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                3751
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            vn2143sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1005.21(3)
_cod_database_code               2242857
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
La La1 0.75090(2) 0.52031(2) 0.47969(2) 0.02048(7) Uani d 1
O O5 0.4472(3) 0.3677(2) 0.4069(2) 0.0332(6) Uani d 1
O O3 1.0575(3) 0.5881(3) 0.6253(2) 0.0323(6) Uani d 1
O O1 0.7627(3) 0.3041(3) 0.5311(2) 0.0336(6) Uani d 1
O O6 0.8146(3) 0.7579(3) 0.6435(3) 0.0362(6) Uani d 1
O O2 0.7422(3) 0.4674(3) 0.6736(2) 0.0351(6) Uani d 1
O O4 0.6840(3) 0.3616(3) 0.2490(2) 0.0415(7) Uani d 1
O O7 0.5690(4) 0.5882(4) 0.3233(3) 0.0486(8) Uani d 1
H H7A 0.468(3) 0.558(4) 0.307(5) 0.058 Uiso d 1
H H7B 0.591(5) 0.651(4) 0.302(5) 0.058 Uiso d 1
O O8 0.9316(4) 0.7051(3) 0.4326(4) 0.0503(8) Uani d 1
H H8A 0.947(6) 0.785(3) 0.470(4) 0.060 Uiso d 1
H H8B 1.026(4) 0.712(4) 0.435(5) 0.060 Uiso d 1
C C6 0.6834(4) 0.7426(3) 0.6621(3) 0.0260(7) Uani d 1
C C11 0.8165(4) 0.3436(3) 0.2659(3) 0.0261(7) Uani d 1
C C1 0.7640(4) 0.3589(4) 0.6405(4) 0.0315(8) Uani d 1
C C13 0.6579(5) 0.1147(4) 0.0739(4) 0.0340(9) Uani d 1
C C12 0.8247(5) 0.2382(4) 0.1565(4) 0.0390(9) Uani d 1
H H12A 0.857342 0.281262 0.102898 0.058 Uiso calc 1
H H12B 0.910563 0.207990 0.192279 0.058 Uiso calc 1
C C14 0.6017(5) 0.0190(4) 0.1196(4) 0.0427(10) Uani d 1
H H14 0.669560 0.030195 0.201149 0.051 Uiso calc 1
C C8 0.8472(5) 0.9325(4) 0.8881(4) 0.0340(9) Uani d 1
C C10 0.9564(5) 1.0646(4) 0.9217(4) 0.0433(10) Uani d 1
H H10 0.928413 1.109955 0.869797 0.052 Uiso calc 1
C C15 0.5547(5) 0.0946(4) -0.0469(4) 0.0412(10) Uani d 1
H H15 0.589046 0.157191 -0.080797 0.049 Uiso calc 1
C C7 0.6832(5) 0.8578(4) 0.7675(4) 0.0445(11) Uani d 1
H H7C 0.660724 0.923722 0.734480 0.067 Uiso calc 1
H H7D 0.592152 0.819798 0.789973 0.067 Uiso calc 1
C C9 0.8927(6) 0.8687(4) 0.9685(4) 0.0461(11) Uani d 1
H H9 0.820475 0.779508 0.948162 0.055 Uiso calc 1
C C3 0.8997(5) 0.3972(4) 0.8732(4) 0.0392(9) Uani d 1
C C4 1.0738(6) 0.4427(5) 0.9267(4) 0.0514(11) Uani d 1
H H4 1.125405 0.405378 0.878263 0.062 Uiso calc 1
C C5 0.8281(6) 0.4561(5) 0.9477(4) 0.0501(11) Uani d 1
H H5 0.711419 0.427472 0.913133 0.060 Uiso calc 1
C C2 0.7931(6) 0.2928(4) 0.7347(4) 0.0460(10) Uani d 1
H H2A 0.684726 0.235879 0.727251 0.069 Uiso calc 1
H H2B 0.848359 0.233001 0.711571 0.069 Uiso calc 1
O OW1 0.6313(10) 0.0072(5) 0.4440(6) 0.1327(17) Uani d 1
H HW1A 0.589(11) -0.025(9) 0.491(8) 0.159 Uiso d 1
H HW1B 0.639(13) -0.072(6) 0.411(8) 0.159 Uiso d 1
O OW2 0.5351(5) 0.6185(4) 0.9718(4) 0.0741(11) Uani d 1
H HW2A 0.476(7) 0.639(6) 0.920(5) 0.111 Uiso d 1
H HW2B 0.622(6) 0.678(5) 1.033(5) 0.111 Uiso d 1
O OW3 0.0357(9) 0.0056(6) 0.3870(6) 0.1327(17) Uani d 1
H HW3A 0.059(10) 0.059(7) 0.354(7) 0.159 Uiso d 1
H HW3B 0.122(7) 0.023(10) 0.447(6) 0.159 Uiso d 1
O OW4 0.7105(10) 0.7873(7) 0.2433(6) 0.154(3) Uani d 1
H HW4A 0.649(10) 0.805(11) 0.192(8) 0.185 Uiso d 1
H HW4B 0.810(5) 0.831(11) 0.255(10) 0.185 Uiso d 1
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -5 4 0.034
-1 4 -3 0.04
2 1 0 0.093
-12 -5 -1 0.081
1 -2 1 0.07
-1 3 -2 0.045
1 4 1 0.052
-1 -3 -1 0.081
-1 1 14 0.085
1 -2 -18 0.067
-5 10 -4 0.062
5 -1 -5 0.094
0 -1 2 0.047
-3 1 2 0.085
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O5 La1 O5 . 2_666 61.48(9)
O5 La1 O3 . . 146.45(9)
O5 La1 O3 . 2_766 118.58(7)
O5 La1 O1 . . 75.87(8)
O5 La1 O6 . . 107.86(8)
O5 La1 O2 . . 75.29(8)
O5 La1 O4 . . 80.33(8)
O5 La1 O7 . . 71.93(9)
O5 La1 O8 . . 140.13(9)
O5 La1 C11 2_666 . 156.28(8)
O5 La1 C11 . . 98.48(8)
O5 La1 C1 . . 75.84(9)
O5 La1 C1 2_666 . 88.69(9)
O3 La1 O5 . 2_666 118.22(7)
O3 La1 O5 2_766 2_666 179.00(7)
O3 La1 O3 . 2_766 61.11(8)
O3 La1 O1 . . 73.20(8)
O3 La1 O6 . . 80.93(8)
O3 La1 O2 . . 74.87(8)
O3 La1 O4 . . 108.82(8)
O3 La1 O8 . . 73.39(9)
O3 La1 C11 2_766 . 24.36(8)
O3 La1 C11 . . 85.47(8)
O3 La1 C1 . . 70.64(9)
O3 La1 C1 2_766 . 90.37(9)
O1 La1 O5 . 2_666 109.68(7)
O1 La1 O3 . 2_766 69.49(8)
O1 La1 C11 . . 74.29(9)
O1 La1 C1 . . 25.01(9)
O6 La1 O5 . 2_666 46.41(7)
O6 La1 O3 . 2_766 133.56(8)
O6 La1 O1 . . 126.21(9)
O6 La1 O2 . . 78.86(9)
O6 La1 O4 . . 149.49(10)
O6 La1 O8 . . 71.55(10)
O6 La1 C11 . . 149.62(9)
O6 La1 C1 . . 101.90(10)
O2 La1 O5 . 2_666 66.57(8)
O2 La1 O3 . 2_766 112.44(8)
O2 La1 O1 . . 49.39(8)
O2 La1 C11 . . 123.42(9)
O2 La1 C1 . . 24.50(9)
O4 La1 O5 . 2_666 132.95(7)
O4 La1 O3 . 2_766 47.75(7)
O4 La1 O1 . . 84.13(9)
O4 La1 O2 . . 131.27(9)
O4 La1 C11 . . 23.49(8)
O4 La1 C1 . . 108.61(10)
O7 La1 O5 . 2_666 70.81(9)
O7 La1 O3 . . 141.53(10)
O7 La1 O3 . 2_766 110.19(9)
O7 La1 O1 . . 142.43(10)
O7 La1 O6 . . 82.59(10)
O7 La1 O2 . . 134.87(9)
O7 La1 O4 . . 71.95(10)
O7 La1 O8 . . 68.46(10)
O7 La1 C11 . . 91.69(10)
O7 La1 C1 . . 147.21(10)
O8 La1 O5 . 2_666 108.04(8)
O8 La1 O3 . 2_766 72.59(9)
O8 La1 O1 . . 138.11(8)
O8 La1 O2 . . 139.28(10)
O8 La1 O4 . . 83.41(11)
O8 La1 C11 . . 78.57(10)
O8 La1 C1 . . 144.03(10)
C1 La1 C11 . . 98.95(10)
La1 O5 La1 . 2_666 118.52(9)
C6 O5 La1 2_666 2_666 88.1(2)
C6 O5 La1 2_666 . 153.4(2)
La1 O3 La1 . 2_766 118.89(8)
C11 O3 La1 2_766 . 150.5(2)
C11 O3 La1 2_766 2_766 90.56(19)
C1 O1 La1 . . 91.6(2)
C6 O6 La1 . . 104.8(2)
C1 O2 La1 . . 96.9(2)
C11 O4 La1 . . 101.3(2)
La1 O7 H7A . . 116(3)
La1 O7 H7B . . 133(3)
H7A O7 H7B . . 109(3)
La1 O8 H8A . . 118(3)
La1 O8 H8B . . 122(3)
H8A O8 H8B . . 104(3)
O5 C6 La1 2_666 . 68.28(18)
O5 C6 O6 2_666 . 120.2(3)
O5 C6 C7 2_666 . 120.1(3)
O6 C6 La1 . . 52.33(16)
O6 C6 C7 . . 119.7(3)
C7 C6 La1 . . 169.6(2)
O3 C11 La1 2_766 . 65.08(17)
O3 C11 C12 2_766 . 120.3(3)
O4 C11 La1 . . 55.16(17)
O4 C11 O3 . 2_766 119.9(3)
O4 C11 C12 . . 119.8(3)
C12 C11 La1 . . 171.2(2)
O1 C1 La1 . . 63.39(19)
O1 C1 C2 . . 119.8(3)
O2 C1 La1 . . 58.58(18)
O2 C1 O1 . . 121.5(3)
O2 C1 C2 . . 118.7(3)
C2 C1 La1 . . 172.4(3)
C14 C13 C12 . . 120.5(4)
C15 C13 C12 . . 122.1(4)
C15 C13 C14 . . 117.4(4)
C11 C12 H12A . . 109.2
C11 C12 H12B . . 109.2
C13 C12 C11 . . 112.0(3)
C13 C12 H12A . . 109.2
C13 C12 H12B . . 109.2
H12A C12 H12B . . 107.9
C13 C14 H14 . . 119.1
C13 C14 C15 . 2_655 121.8(4)
C15 C14 H14 2_655 . 119.1
C10 C8 C7 . . 121.6(4)
C10 C8 C9 . . 117.8(4)
C9 C8 C7 . . 120.6(4)
C8 C10 H10 . . 119.5
C8 C10 C9 . 2_777 121.1(4)
C9 C10 H10 2_777 . 119.5
C13 C15 C14 . 2_655 120.7(4)
C13 C15 H15 . . 119.6
C14 C15 H15 2_655 . 119.6
C6 C7 H7C . . 108.9
C6 C7 H7D . . 108.9
C8 C7 C6 . . 113.4(3)
C8 C7 H7C . . 108.9
C8 C7 H7D . . 108.9
H7C C7 H7D . . 107.7
C8 C9 H9 . . 119.4
C10 C9 C8 2_777 . 121.1(4)
C10 C9 H9 2_777 . 119.4
C4 C3 C2 . . 120.7(4)
C5 C3 C4 . . 118.0(4)
C5 C3 C2 . . 121.2(4)
C3 C4 H4 . . 119.8
C3 C4 C5 . 2_767 120.4(4)
C5 C4 H4 2_767 . 119.8
C3 C5 C4 . 2_767 121.6(4)
C3 C5 H5 . . 119.2
C4 C5 H5 2_767 . 119.2
C1 C2 H2A . . 109.0
C1 C2 H2B . . 109.0
C3 C2 C1 . . 112.8(3)
C3 C2 H2A . . 109.0
C3 C2 H2B . . 109.0
H2A C2 H2B . . 107.8
HW1A OW1 HW1B . . 88(7)
HW2A OW2 HW2B . . 121(5)
HW3A OW3 HW3B . . 108(4)
HW4A OW4 HW4B . . 107(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
La1 O5 . 2.507(2) y
La1 O5 2_666 2.905(3) y
La1 O3 2_766 2.781(2) y
La1 O3 . 2.545(2) y
La1 O1 . 2.673(2) y
La1 O6 . 2.559(2) y
La1 O2 . 2.569(2) y
La1 O4 . 2.566(2) y
La1 O7 . 2.543(3) y
La1 O8 . 2.562(3) y
La1 C11 . 3.066(3) y
La1 C1 . 2.988(4) y
O5 C6 2_666 1.255(4) ?
O3 C11 2_766 1.264(4) ?
O1 C1 . 1.264(4) ?
O6 C6 . 1.256(4) ?
O2 C1 . 1.248(4) ?
O4 C11 . 1.246(4) ?
O7 H7A . 0.824(19) ?
O7 H7B . 0.806(18) ?
O8 H8A . 0.815(19) ?
O8 H8B . 0.833(19) ?
C6 C7 . 1.512(5) ?
C11 C12 . 1.516(5) ?
C1 C2 . 1.514(5) ?
C13 C12 . 1.507(5) ?
C13 C14 . 1.376(6) ?
C13 C15 . 1.371(5) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C14 H14 . 0.9300 ?
C14 C15 2_655 1.399(6) ?
C8 C10 . 1.373(6) ?
C8 C7 . 1.509(5) ?
C8 C9 . 1.388(6) ?
C10 H10 . 0.9300 ?
C10 C9 2_777 1.382(6) ?
C15 H15 . 0.9300 ?
C7 H7C . 0.9700 ?
C7 H7D . 0.9700 ?
C9 H9 . 0.9300 ?
C3 C4 . 1.385(6) ?
C3 C5 . 1.381(6) ?
C3 C2 . 1.509(6) ?
C4 H4 . 0.9300 ?
C4 C5 2_767 1.391(6) ?
C5 H5 . 0.9300 ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
OW1 HW1A . 0.87(2) ?
OW1 HW1B . 0.88(2) ?
OW2 HW2A . 0.821(19) ?
OW2 HW2B . 0.81(2) ?
OW3 HW3A . 0.82(2) ?
OW3 HW3B . 0.81(2) ?
OW4 HW4A . 0.81(2) ?
OW4 HW4B . 0.84(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
OW1 HW1A OW1 2_656 0.87(9) 2.40(11) 3.067(13) 133(9)
OW1 HW1B OW4 1_545 0.89(9) 2.54(10) 3.298(11) 145(7)
OW2 HW2A O4 2_666 0.82(6) 2.10(6) 2.895(5) 164(6)
OW2 HW2B OW4 1_556 0.82(6) 2.20(5) 2.855(8) 137(5)
OW3 HW3A O6 2_666 0.82(8) 2.02(8) 2.780(8) 154(7)
OW3 HW3B OW1 2_656 0.81(7) 2.40(8) 3.162(11) 156(8)
OW4 HW4A OW2 1_554 0.81(10) 2.49(9) 2.855(8) 109(9)
O7 H7A O2 2_666 0.82(4) 1.95(4) 2.741(5) 161(5)
O7 H7B OW4 1_555 0.81(5) 2.03(5) 2.800(9) 160(5)
OW4 HW4B OW3 1_665 0.84(9) 2.11(10) 2.824(11) 143(8)
O8 H8A OW3 2_666 0.82(4) 2.38(4) 3.175(8) 165(4)
O8 H8B O1 2_766 0.83(4) 1.92(4) 2.725(5) 163(5)
C7 H7D O4 2_666 0.97 2.54 3.442(6) 154
C12 H12B O6 2_766 0.97 2.51 3.406(6) 154

_cod_database_fobs_code 2242857
