#------------------------------------------------------------------------------
#$Date: 2018-05-30 18:52:24 +0300 (Wed, 30 May 2018) $
#$Revision: 208051 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/11/2021141.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_2021141
loop_
_publ_author_name
'Mendes, Ricardo F.'
'Firmino, Ana D. G.'
'Tomé, João P. C.'
'Almeida Paz, Filipe A.'
_publ_section_title
;
 Metal--organic framework assembled from erbium and a tetrapodal
 polyphosphonic acid organic linker
;
_journal_coeditor_code           LG3220
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618007374
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Er (C12 H11 O12 P4)], 2.5H2 O'
_chemical_formula_moiety         'C12 H11 O12 P4 Er, 2.5(H2 O)'
_chemical_formula_sum            'C12 H16 Er O14.5 P4'
_chemical_formula_weight         1366.77
_chemical_name_systematic
;
Poly[[μ₆-pentahydrogen
[1,1'-biphenyl]-3,3',5,5'-tetrayltetrakis(phosphonato)]erbium(III)]
2.5-hydrate]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'SSHELXL-2014/6, manual editing plus enCIFer'
_cell_angle_alpha                90
_cell_angle_beta                 115.261(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1557(11)
_cell_length_b                   23.753(3)
_cell_length_c                   10.3790(13)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.60
_cell_volume                     2041.3(4)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST '
_diffrn_measurement_method       'ω/φ scans'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            37649
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         3.560
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_description       Block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.811
_refine_diff_density_min         -1.691
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3726
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+38.9895P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                2799
_reflns_number_total             3726
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lg3220sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C12 H16 Er1 O14.5 P4'
_cod_database_code               2021141
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Er Er1 0.27760(6) 0.04946(2) 1.04347(6) 0.01629(16) Uani d 1
P P1 0.3811(4) 0.17420(12) 0.9026(4) 0.0175(7) Uani d 1
P P2 0.8544(4) 0.06748(12) 0.8092(4) 0.0167(7) Uani d 1
P P3 0.6971(3) 0.45502(13) 0.7233(3) 0.0180(7) Uani d 1
P P4 1.2091(4) 0.33477(14) 0.7346(5) 0.0314(10) Uani d 1
O O1 0.3695(9) 0.1160(3) 0.9503(9) 0.0186(19) Uani d 1
O O2 0.3873(12) 0.2208(4) 1.0061(12) 0.045(3) Uani d 1
H H2 0.3211 0.2136 1.0402 0.068 Uiso calc 1
O O3 0.2340(10) 0.1835(4) 0.7581(11) 0.035(2) Uani d 1
H H3 0.2438 0.2144 0.7233 0.053 Uiso calc 1
O O4 0.7740(10) 0.0190(3) 0.8426(9) 0.0198(19) Uani d 1
O O5 1.0329(10) 0.0707(3) 0.8943(10) 0.030(2) Uani d 1
O O6 0.8288(11) 0.0663(4) 0.6507(9) 0.030(2) Uani d 1
H H6 0.7319 0.0585 0.5979 0.044 Uiso calc 1
O O7 0.5307(9) 0.4486(3) 0.7153(8) 0.0207(18) Uani d 1
O O8 0.8084(11) 0.4822(4) 0.8666(9) 0.031(2) Uani d 1
H H8 0.8205 0.5165 0.8540 0.047 Uiso calc 1
O O9 0.7021(10) 0.4865(3) 0.6034(9) 0.024(2) Uani d 1
O O10 1.2402(10) 0.3913(3) 0.6898(9) 0.025(2) Uani d 1
O O11 1.2029(15) 0.2869(4) 0.6343(15) 0.071(4) Uani d 1
O O12 1.3410(11) 0.3235(5) 0.8888(14) 0.071(4) Uani d 1
H H12 1.3157 0.2949 0.9223 0.107 Uiso calc 1
C C1 0.5587(13) 0.1795(5) 0.8717(12) 0.015(2) Uani d 1
C C2 0.6163(14) 0.2305(5) 0.8479(13) 0.019(2) Uani d 1
H H2A 0.5645 0.2644 0.8542 0.022 Uiso calc 1
C C3 0.7484(14) 0.2334(4) 0.8149(13) 0.017(2) Uani d 1
C C4 0.8146(14) 0.1826(5) 0.8010(13) 0.019(2) Uani d 1
H H4 0.9008 0.1830 0.7729 0.023 Uiso calc 1
C C5 0.7608(13) 0.1316(4) 0.8262(13) 0.016(2) Uani d 1
C C6 0.6307(13) 0.1306(5) 0.8601(13) 0.017(2) Uani d 1
H H6A 0.5907 0.0955 0.8756 0.021 Uiso calc 1
C C7 0.8102(14) 0.2875(5) 0.7856(13) 0.018(2) Uani d 1
C C8 0.7300(14) 0.3382(5) 0.7679(13) 0.018(2) Uani d 1
H H8A 0.6307 0.3393 0.7763 0.022 Uiso calc 1
C C9 0.7908(14) 0.3874(5) 0.7383(14) 0.020(2) Uani d 1
C C10 0.9345(14) 0.3861(5) 0.7234(14) 0.023(2) Uani d 1
H H10 0.9740 0.4196 0.6994 0.028 Uiso calc 1
C C11 1.0206(15) 0.3364(5) 0.7433(14) 0.024(2) Uani d 1
C C12 0.9572(15) 0.2881(5) 0.7747(14) 0.023(2) Uani d 1
H H12A 1.0161 0.2540 0.7893 0.027 Uiso calc 1
O O1W 0.538(2) 0.4262(9) 0.976(2) 0.039(2) Uiso d 0.5
O O2W 0.525(2) 0.4604(9) 0.971(2) 0.039(2) Uiso d 0.5
O O3W 0.094(2) 0.4158(6) 0.0882(18) 0.039(2) Uiso d 0.7
O O4W 0.093(5) 0.3959(14) 0.108(4) 0.039(2) Uiso d 0.3
O O5W 0.352(4) 0.3820(13) 0.028(3) 0.039(2) Uiso d 0.3
O O6W 0.256(5) 0.443(2) -0.017(5) 0.039(2) Uiso d 0.2
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'
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'
Er Er -0.2586 4.9576 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Er1 O9 . 2_646 91.3(3) yes
O1 Er1 O7 . 4_566 82.8(3) yes
O1 Er1 O10 . 4_466 92.6(3) yes
O4 Er1 O1 3_657 . 171.1(3) yes
O4 Er1 O7 3_657 4_566 88.5(3) yes
O4 Er1 O9 3_657 2_646 88.3(3) yes
O4 Er1 O10 3_657 4_466 88.3(3) yes
O5 Er1 O1 1_455 . 89.5(3) yes
O5 Er1 O4 1_455 3_657 99.4(3) yes
O5 Er1 O7 1_455 4_566 164.7(3) yes
O5 Er1 O9 1_455 2_646 91.8(3) yes
O5 Er1 O10 1_455 4_466 85.8(3) yes
O9 Er1 O7 2_646 4_566 101.6(3) yes
O9 Er1 O10 2_646 4_466 175.4(3) yes
O10 Er1 O7 4_466 4_566 81.4(3) yes
O1 P1 O2 . . 115.2(5) ?
O1 P1 O3 . . 107.4(5) ?
O2 P1 O3 . . 109.5(6) ?
O1 P1 C1 . . 109.0(5) ?
O2 P1 C1 . . 108.1(5) ?
O3 P1 C1 . . 107.4(5) ?
O4 P2 O5 . . 115.4(5) ?
O4 P2 O6 . . 111.5(5) ?
O5 P2 O6 . . 105.0(5) ?
O4 P2 C5 . . 109.3(5) ?
O5 P2 C5 . . 110.3(5) ?
O6 P2 C5 . . 104.8(5) ?
O9 P3 O7 . . 113.8(5) ?
O9 P3 O8 . . 111.0(5) ?
O7 P3 O8 . . 109.5(5) ?
O9 P3 C9 . . 110.0(5) ?
O7 P3 C9 . . 110.5(5) ?
O8 P3 C9 . . 101.3(6) ?
O10 P4 O11 . . 114.6(6) ?
O10 P4 O12 . . 107.9(6) ?
O11 P4 O12 . . 111.0(7) ?
O10 P4 C11 . . 108.5(5) ?
O11 P4 C11 . . 107.4(6) ?
O12 P4 C11 . . 107.2(6) ?
P1 O1 Er1 . . 155.5(5) ?
P1 O2 H2 . . 109.5 ?
P1 O3 H3 . . 109.5 ?
P2 O4 Er1 . 3_657 161.8(6) ?
P2 O5 Er1 . 1_655 161.2(5) ?
P2 O6 H6 . . 109.5 ?
P3 O7 Er1 . 4_565 136.3(5) ?
P3 O8 H8 . . 109.5 ?
P3 O9 Er1 . 2_656 167.3(6) ?
P4 O10 Er1 . 4_665 154.1(6) ?
P4 O12 H12 . . 109.5 ?
C6 C1 C2 . . 119.6(10) ?
C6 C1 P1 . . 117.7(8) ?
C2 C1 P1 . . 122.5(8) ?
C1 C2 C3 . . 121.6(10) ?
C1 C2 H2A . . 119.2 ?
C3 C2 H2A . . 119.2 ?
C4 C3 C2 . . 116.6(10) ?
C4 C3 C7 . . 120.7(9) ?
C2 C3 C7 . . 122.5(10) ?
C5 C4 C3 . . 122.6(10) ?
C5 C4 H4 . . 118.7 ?
C3 C4 H4 . . 118.7 ?
C4 C5 C6 . . 118.9(10) ?
C4 C5 P2 . . 120.3(8) ?
C6 C5 P2 . . 120.8(8) ?
C1 C6 C5 . . 120.6(10) ?
C1 C6 H6A . . 119.7 ?
C5 C6 H6A . . 119.7 ?
C8 C7 C12 . . 117.2(10) ?
C8 C7 C3 . . 123.6(10) ?
C12 C7 C3 . . 119.2(10) ?
C7 C8 C9 . . 121.6(10) ?
C7 C8 H8A . . 119.2 ?
C9 C8 H8A . . 119.2 ?
C8 C9 C10 . . 119.6(10) ?
C8 C9 P3 . . 123.5(8) ?
C10 C9 P3 . . 116.8(8) ?
C11 C10 C9 . . 120.6(10) ?
C11 C10 H10 . . 119.7 ?
C9 C10 H10 . . 119.7 ?
C10 C11 C12 . . 118.1(10) ?
C10 C11 P4 . . 121.2(8) ?
C12 C11 P4 . . 120.6(9) ?
C11 C12 C7 . . 122.8(11) ?
C11 C12 H12A . . 118.6 ?
C7 C12 H12A . . 118.6 ?
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
Er1 O1 . 2.199(7) yes
Er1 O4 3_657 2.179(8) yes
Er1 O5 1_455 2.171(8) yes
Er1 O7 4_566 2.242(8) yes
Er1 O9 2_646 2.200(8) yes
Er1 O10 4_466 2.202(8) yes
P1 O1 . 1.487(8) no
P1 O2 . 1.526(9) no
P1 O3 . 1.546(10) no
P1 C1 . 1.791(11) no
P2 O4 . 1.484(8) no
P2 O5 . 1.491(9) no
P2 O6 . 1.560(9) no
P2 C5 . 1.793(11) no
P3 O9 . 1.468(9) no
P3 O7 . 1.498(7) no
P3 O8 . 1.541(9) no
P3 C9 . 1.796(11) no
P4 O10 . 1.487(8) no
P4 O11 . 1.527(11) no
P4 O12 . 1.562(12) no
P4 C11 . 1.767(11) no
O2 H2 . 0.8400 ?
O3 H3 . 0.8400 ?
O4 Er1 3_657 2.179(8) no
O5 Er1 1_655 2.171(8) no
O6 H6 . 0.8400 ?
O7 Er1 4_565 2.242(8) no
O8 H8 . 0.8400 ?
O9 Er1 2_656 2.200(8) no
O10 Er1 4_665 2.202(8) no
O12 H12 . 0.8400 ?
C1 C6 . 1.367(15) ?
C1 C2 . 1.385(15) ?
C2 C3 . 1.392(15) ?
C2 H2A . 0.9500 ?
C3 C4 . 1.385(15) ?
C3 C7 . 1.488(15) ?
C4 C5 . 1.374(15) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.379(15) ?
C6 H6A . 0.9500 ?
C7 C8 . 1.380(15) ?
C7 C12 . 1.398(15) ?
C8 C9 . 1.385(15) ?
C8 H8A . 0.9500 ?
C9 C10 . 1.389(15) ?
C10 C11 . 1.384(15) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.385(15) ?
C12 H12A . 0.9500 ?
O1W O2W . 0.82(2) ?
O3W O4W . 0.52(4) ?
O5W O6W . 1.66(5) ?
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
O2 H2 O11 4_466 0.84 1.74 2.564(12) 166.4
O3 H3 O11 1_455 0.84 1.91 2.728(13) 163.6
O6 H6 O1W 4_565 0.84 1.73 2.51(2) 154.5
O6 H6 O2W 4_565 0.84 1.85 2.68(2) 175.3
O8 H8 O3W 3_666 0.84 1.78 2.556(17) 153.3
O8 H8 O4W 3_666 0.84 2.20 3.01(3) 161.8
O12 H12 O2 1_655 0.84 1.95 2.679(14) 144.7
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
O2 P1 O1 Er1 . 44.2(14)
O3 P1 O1 Er1 . -78.1(13)
C1 P1 O1 Er1 . 165.9(12)
O5 P2 O4 Er1 3_657 26.4(17)
O6 P2 O4 Er1 3_657 146.0(15)
C5 P2 O4 Er1 3_657 -98.6(16)
O4 P2 O5 Er1 1_655 5(2)
O6 P2 O5 Er1 1_655 -118.4(18)
C5 P2 O5 Er1 1_655 129.2(18)
O9 P3 O7 Er1 4_565 22.9(9)
O8 P3 O7 Er1 4_565 147.8(6)
C9 P3 O7 Er1 4_565 -101.4(8)
O7 P3 O9 Er1 2_656 96(2)
O8 P3 O9 Er1 2_656 -28(3)
C9 P3 O9 Er1 2_656 -139(2)
O11 P4 O10 Er1 4_665 4.4(15)
O12 P4 O10 Er1 4_665 128.6(13)
C11 P4 O10 Er1 4_665 -115.5(13)
O1 P1 C1 C6 . 15.7(11)
O2 P1 C1 C6 . 141.6(10)
O3 P1 C1 C6 . -100.3(10)
O1 P1 C1 C2 . -169.7(10)
O2 P1 C1 C2 . -43.8(12)
O3 P1 C1 C2 . 74.3(11)
C6 C1 C2 C3 . -1.3(19)
P1 C1 C2 C3 . -175.7(10)
C1 C2 C3 C4 . 2.8(19)
C1 C2 C3 C7 . 178.6(11)
C2 C3 C4 C5 . -3.7(19)
C7 C3 C4 C5 . -179.7(12)
C3 C4 C5 C6 . 3.1(19)
C3 C4 C5 P2 . -178.9(10)
O4 P2 C5 C4 . 179.8(10)
O5 P2 C5 C4 . 51.9(12)
O6 P2 C5 C4 . -60.7(11)
O4 P2 C5 C6 . -2.3(12)
O5 P2 C5 C6 . -130.1(10)
O6 P2 C5 C6 . 117.3(10)
C2 C1 C6 C5 . 0.6(18)
P1 C1 C6 C5 . 175.3(9)
C4 C5 C6 C1 . -1.4(19)
P2 C5 C6 C1 . -179.4(9)
C4 C3 C7 C8 . 165.8(13)
C2 C3 C7 C8 . -9.8(19)
C4 C3 C7 C12 . -14.0(18)
C2 C3 C7 C12 . 170.4(12)
C12 C7 C8 C9 . 1.0(19)
C3 C7 C8 C9 . -178.8(12)
C7 C8 C9 C10 . 1(2)
C7 C8 C9 P3 . -176.7(10)
O9 P3 C9 C8 . -138.8(11)
O7 P3 C9 C8 . -12.3(13)
O8 P3 C9 C8 . 103.7(12)
O9 P3 C9 C10 . 43.3(12)
O7 P3 C9 C10 . 169.8(10)
O8 P3 C9 C10 . -74.1(11)
C8 C9 C10 C11 . -2(2)
P3 C9 C10 C11 . 175.5(11)
C9 C10 C11 C12 . 2(2)
C9 C10 C11 P4 . -176.4(11)
O10 P4 C11 C10 . -5.7(14)
O11 P4 C11 C10 . -130.1(12)
O12 P4 C11 C10 . 110.5(12)
O10 P4 C11 C12 . 176.2(11)
O11 P4 C11 C12 . 51.9(13)
O12 P4 C11 C12 . -67.5(13)
C10 C11 C12 C7 . 1(2)
P4 C11 C12 C7 . 178.6(11)
C8 C7 C12 C11 . -1.9(19)
C3 C7 C12 C11 . 177.9(12)

_cod_database_fobs_code 2021141
