#------------------------------------------------------------------------------
#$Date: 2025-07-01 16:04:19 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1352 $
#$URL: svn://crystallography.net/testcod/cif/4/00/00/4000086.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_4000086
loop_
_publ_author_name
'Colodrero, Rosario M. P.'
'Papathanasiou, Konstantinos E.'
'Stavgianoudaki, Nikoleta'
'Olivera-Pastor, Pascual'
'Losilla, Enrique R.'
'Aranda, Miguel A. G.'
'León-Reina, Laura'
'Sanz, Jesús'
'Sobrados, Isabel'
'Choquesillo-Lazarte, Duane'
'García-Ruiz, Juan M.'
'Atienzar, Pedro'
'Rey, Fernando'
'Demadis, Konstantinos D.'
'Cabeza, Aurelio'
_publ_section_title
;
 Multifunctional Luminescent and Proton-Conducting Lanthanide
 Carboxyphosphonate Open-Framework Hybrids Exhibiting
 Crystalline-to-Amorphous-to-Crystalline Transformations
;
_journal_issue                   19
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3780
_journal_page_last               3792
_journal_paper_doi               10.1021/cm302381k
_journal_volume                  24
_journal_year                    2012
_chemical_formula_moiety         'C8 H28 Gd3 O32 P4, 4(H2 O)'
_chemical_formula_sum            'C8 H36 Gd3 O36 P4'
_chemical_formula_weight         1304.00
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2c'
_space_group_name_H-M_alt        'P c a n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0433(2)
_cell_length_b                   25.7014(3)
_cell_length_c                   11.07570(10)
_cell_measurement_reflns_used    10904
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1651
_cell_measurement_theta_min      2.8809
_cell_volume                     3712.92(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16585
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    5.583
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_correction_T_min  0.8075
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains 16 water molecules which 
have been treated as a diffuse contribution 
to the overall scattering without specific 
atom positions by SQUEEZE/PLATON
;
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0248P)²+21.0704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                3059
_reflns_number_total             3274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm302381k_si_002.cif
_cod_data_source_block           GdHPA-II
_cod_original_sg_symbol_H-M      Pcan
_cod_database_code               4000086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x, y, z-1/2'
'x-1/2, -y-1/2, 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
Gd2 Gd 0.342968(16) 0.781217(8) 1.020585(19) 0.00612(8) Uani 1 1 d . . .
P1 P 0.18856(9) 0.69604(4) 0.84725(10) 0.0080(2) Uani 1 1 d . . .
O2 O 0.2911(2) 0.71915(11) 0.8785(3) 0.0084(6) Uani 1 1 d . . .
O3 O 0.1724(3) 0.64054(12) 0.9013(3) 0.0142(7) Uani 1 1 d . . .
O1 O 0.1622(2) 0.69278(12) 0.7167(3) 0.0107(7) Uani 1 1 d . . .
C1 C 0.0927(3) 0.73830(18) 0.9182(4) 0.0102(9) Uani 1 1 d . . .
H1 H 0.1094 0.7754 0.8994 0.012 Uiso 1 1 calc R . .
O4 O -0.0086(2) 0.72726(12) 0.8779(3) 0.0109(7) Uani 1 1 d . . .
H4 H -0.0084 0.7251 0.8048 0.016 Uiso 1 1 d R . .
C2 C 0.0983(4) 0.73011(17) 1.0549(4) 0.0104(10) Uani 1 1 d . . .
O5 O 0.1853(2) 0.73552(12) 1.1027(3) 0.0103(7) Uani 1 1 d . . .
O6 O 0.0173(2) 0.71891(11) 1.1107(3) 0.0093(7) Uani 1 1 d . . .
Gd1 Gd 0.50787(3) 1.0000 0.7500 0.01077(9) Uani 1 2 d S . .
P2 P 0.29826(10) 0.91835(5) 0.68901(10) 0.0115(3) Uani 1 1 d . . .
O9 O 0.3822(3) 0.95379(11) 0.6419(3) 0.0126(7) Uani 1 1 d . . .
O8 O 0.2205(3) 0.94952(13) 0.7656(3) 0.0172(7) Uani 1 1 d . . .
O7 O 0.2422(3) 0.88759(12) 0.5920(3) 0.0130(7) Uani 1 1 d . . .
C3 C 0.3652(4) 0.87055(17) 0.7842(4) 0.0104(9) Uani 1 1 d . . .
H3 H 0.4263 0.8585 0.7374 0.012 Uiso 1 1 calc R . .
O10 O 0.3073(3) 0.82488(12) 0.8145(3) 0.0108(7) Uani 1 1 d . . .
H10 H 0.3141 0.8077 0.7520 0.016 Uiso 1 1 d R . .
C4 C 0.4059(4) 0.89520(17) 0.9011(4) 0.0113(10) Uani 1 1 d . . .
O12 O 0.4423(3) 0.93961(12) 0.8956(3) 0.0153(7) Uani 1 1 d . . .
O11 O 0.3989(3) 0.86844(12) 0.9965(3) 0.0114(7) Uani 1 1 d . . .
O1W O 0.3905(3) 0.69734(12) 1.1065(3) 0.0157(7) Uani 1 1 d . . .
O4W O 0.1910(3) 0.83909(14) 1.0340(3) 0.0176(7) Uani 1 1 d . . .
O5W O 0.5952(3) 0.92009(13) 0.7101(3) 0.0197(8) Uani 1 1 d . . .
O6W O 0.6324(3) 0.98844(13) 0.9085(3) 0.0204(8) 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'
Gd Gd -0.1653 3.9035 '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'
P P 0.1023 0.0942 '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
O1 Gd2 O2 146.52(11) 2_565 . ?
O1 Gd2 O11 80.71(11) 2_565 . ?
O2 Gd2 O11 131.09(10) . . ?
O1 Gd2 O1W 83.97(11) 2_565 . ?
O2 Gd2 O1W 74.53(11) . . ?
O11 Gd2 O1W 143.27(11) . . ?
O1 Gd2 O4W 75.11(11) 2_565 . ?
O2 Gd2 O4W 102.56(11) . . ?
O11 Gd2 O4W 71.72(12) . . ?
O1W Gd2 O4W 135.23(12) . . ?
O1 Gd2 O6 69.14(11) 2_565 8_675 ?
O2 Gd2 O6 122.28(10) . 8_675 ?
O11 Gd2 O6 76.38(11) . 8_675 ?
O1W Gd2 O6 66.98(10) . 8_675 ?
O4W Gd2 O6 135.08(11) . 8_675 ?
O1 Gd2 O4 130.57(11) 2_565 8_675 ?
O2 Gd2 O4 74.96(10) . 8_675 ?
O11 Gd2 O4 76.93(11) . 8_675 ?
O1W Gd2 O4 88.43(11) . 8_675 ?
O4W Gd2 O4 134.90(11) . 8_675 ?
O6 Gd2 O4 63.01(10) 8_675 8_675 ?
O1 Gd2 O5 76.66(10) 2_565 . ?
O2 Gd2 O5 72.02(10) . . ?
O11 Gd2 O5 136.64(11) . . ?
O1W Gd2 O5 69.93(11) . . ?
O4W Gd2 O5 66.95(11) . . ?
O6 Gd2 O5 126.71(10) 8_675 . ?
O4 Gd2 O5 144.23(10) 8_675 . ?
O1 Gd2 O10 135.27(10) 2_565 . ?
O2 Gd2 O10 69.52(10) . . ?
O11 Gd2 O10 63.01(10) . . ?
O1W Gd2 O10 140.74(10) . . ?
O4W Gd2 O10 69.46(10) . . ?
O6 Gd2 O10 121.32(10) 8_675 . ?
O4 Gd2 O10 67.68(10) 8_675 . ?
O5 Gd2 O10 111.83(10) . . ?
O1 P1 O2 116.79(18) . . ?
O1 P1 O3 106.85(18) . . ?
O2 P1 O3 113.12(18) . . ?
O1 P1 C1 107.0(2) . . ?
O2 P1 C1 105.92(19) . . ?
O3 P1 C1 106.6(2) . . ?
P1 O2 Gd2 132.93(18) . . ?
P1 O1 Gd2 156.7(2) . 2_564 ?
O4 C1 C2 109.1(4) . . ?
O4 C1 P1 112.4(3) . . ?
C2 C1 P1 108.0(3) . . ?
C1 O4 Gd2 122.4(2) . 8_575 ?
O6 C2 O5 125.1(4) . . ?
O6 C2 C1 118.5(4) . . ?
O5 C2 C1 116.4(4) . . ?
C2 O5 Gd2 129.0(3) . . ?
C2 O6 Gd2 124.9(3) . 8_575 ?
O9 Gd1 O9 91.61(16) . 3_576 ?
O9 Gd1 O5W 149.34(11) . 3_576 ?
O9 Gd1 O5W 78.71(12) 3_576 3_576 ?
O9 Gd1 O5W 78.71(12) . . ?
O9 Gd1 O5W 149.34(11) 3_576 . ?
O5W Gd1 O5W 123.08(18) 3_576 . ?
O9 Gd1 O12 74.67(11) . 3_576 ?
O9 Gd1 O12 76.50(11) 3_576 3_576 ?
O5W Gd1 O12 74.79(11) 3_576 3_576 ?
O5W Gd1 O12 127.06(11) . 3_576 ?
O9 Gd1 O12 76.50(11) . . ?
O9 Gd1 O12 74.67(11) 3_576 . ?
O5W Gd1 O12 127.06(11) 3_576 . ?
O5W Gd1 O12 74.79(12) . . ?
O12 Gd1 O12 138.16(17) 3_576 . ?
O9 Gd1 O6W 99.28(12) . 3_576 ?
O9 Gd1 O6W 141.12(11) 3_576 3_576 ?
O5W Gd1 O6W 72.99(12) 3_576 3_576 ?
O5W Gd1 O6W 69.52(12) . 3_576 ?
O12 Gd1 O6W 70.78(12) 3_576 3_576 ?
O12 Gd1 O6W 144.16(12) . 3_576 ?
O9 Gd1 O6W 141.12(11) . . ?
O9 Gd1 O6W 99.28(12) 3_576 . ?
O5W Gd1 O6W 69.52(12) 3_576 . ?
O5W Gd1 O6W 72.99(12) . . ?
O12 Gd1 O6W 144.16(12) 3_576 . ?
O12 Gd1 O6W 70.77(12) . . ?
O6W Gd1 O6W 95.24(18) 3_576 . ?
O9 P2 O7 114.60(18) . . ?
O9 P2 O8 110.54(18) . . ?
O7 P2 O8 109.97(19) . . ?
O9 P2 C3 104.8(2) . . ?
O7 P2 C3 106.59(19) . . ?
O8 P2 C3 110.1(2) . . ?
P2 O9 Gd1 129.13(17) . . ?
O10 C3 C4 108.8(4) . . ?
O10 C3 P2 115.5(3) . . ?
C4 C3 P2 111.8(3) . . ?
C3 O10 Gd2 117.9(2) . . ?
O12 C4 O11 124.8(4) . . ?
O12 C4 C3 118.1(4) . . ?
O11 C4 C3 117.1(4) . . ?
C4 O12 Gd1 140.1(3) . . ?
C4 O11 Gd2 129.0(3) . . ?
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
Gd2 O1 2.273(3) 2_565 ?
Gd2 O2 2.341(3) . ?
Gd2 O11 2.373(3) . ?
Gd2 O1W 2.436(3) . ?
Gd2 O4W 2.483(3) . ?
Gd2 O6 2.484(3) 8_675 ?
Gd2 O4 2.509(3) 8_675 ?
Gd2 O5 2.537(3) . ?
Gd2 O10 2.586(3) . ?
P1 O1 1.489(3) . ?
P1 O2 1.503(3) . ?
P1 O3 1.561(3) . ?
P1 C1 1.834(5) . ?
O1 Gd2 2.273(3) 2_564 ?
C1 O4 1.422(5) . ?
C1 C2 1.530(6) . ?
O4 Gd2 2.509(3) 8_575 ?
C2 O6 1.257(6) . ?
C2 O5 1.260(6) . ?
O6 Gd2 2.484(3) 8_575 ?
Gd1 O9 2.352(3) . ?
Gd1 O9 2.352(3) 3_576 ?
Gd1 O5W 2.390(3) 3_576 ?
Gd1 O5W 2.390(3) . ?
Gd1 O12 2.396(3) 3_576 ?
Gd1 O12 2.396(3) . ?
Gd1 O6W 2.410(3) 3_576 ?
Gd1 O6W 2.410(3) . ?
P2 O9 1.516(3) . ?
P2 O7 1.521(3) . ?
P2 O8 1.546(3) . ?
P2 C3 1.839(5) . ?
C3 O10 1.435(5) . ?
C3 C4 1.536(6) . ?
C4 O12 1.238(5) . ?
C4 O11 1.265(5) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.014 489 107 ' '
2 0.500 0.500 0.012 489 107 ' '
