#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:47:02 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180276 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/62/7116250.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_7116250
loop_
_publ_author_name
'Zeng, Dai'
'Ren, Min'
'Bao, Song-Song'
'Feng, Jian-Shen'
'Li, Li'
'Zheng, Li-Min'
_publ_section_title
;
 pH-controlled polymorphism in a layered dysprosium phosphonate and its
 impact on the magnetization relaxation.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2649
_journal_page_last               2652
_journal_paper_doi               10.1039/c4cc09341k
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C9 H11 N O9 P S Y'
_chemical_formula_sum            'C9 H11 N O9 P S Y'
_chemical_formula_weight         429.13
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.423(6)
_cell_angle_beta                 93.298(7)
_cell_angle_gamma                102.310(6)
_cell_formula_units_Z            2
_cell_length_a                   6.778(3)
_cell_length_b                   7.572(3)
_cell_length_c                   13.356(5)
_cell_measurement_reflns_used    747
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.344
_cell_measurement_theta_min      2.754
_cell_volume                     668.5(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4878
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.464
_diffrn_reflns_theta_min         1.527
_exptl_absorpt_coefficient_mu    4.687
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_description       sheet-like
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0601
_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)+(0.0785P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2444
_reflns_number_total             3311
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc09341k2.cif
_cod_data_source_block           Y
_cod_depositor_comments          'Adding full bibliography for 7116250.cif.'
_cod_original_cell_volume        668.4(4)
_cod_database_code               7116250
#BEGIN Tags that were not found in dictionaries:
_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   0.651
_shelx_estimated_absorpt_t_max   0.799
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Y1 Y 0.29334(8) 0.76591(7) 0.45639(4) 0.01372(17) Uani 1 1 d . .
P1 P 0.2451(2) 0.38475(19) 0.61875(11) 0.0136(3) Uani 1 1 d . .
S1 S 0.3967(2) 1.07150(19) 0.30800(10) 0.0166(3) Uani 1 1 d . .
C1 C 0.2334(9) 0.3909(8) 0.7566(4) 0.0185(12) Uani 1 1 d . .
C2 C 0.1858(10) 0.2342(9) 0.8126(5) 0.0252(14) Uani 1 1 d . .
H2 H 0.1541 0.1221 0.7798 0.030 Uiso 1 1 calc R U
C3 C 0.1849(10) 0.2425(9) 0.9135(5) 0.0258(14) Uani 1 1 d . .
H3 H 0.1550 0.1361 0.9493 0.031 Uiso 1 1 calc R U
C4 C 0.2289(10) 0.4116(9) 0.9657(4) 0.0230(13) Uani 1 1 d . .
C5 C 0.2294(11) 0.4319(10) 1.0710(5) 0.0282(15) Uani 1 1 d . .
H5 H 0.2013 0.3301 1.1106 0.034 Uiso 1 1 calc R U
C6 C 0.2707(11) 0.5998(10) 1.1147(5) 0.0340(17) Uani 1 1 d . .
H6 H 0.2709 0.6118 1.1841 0.041 Uiso 1 1 calc R U
C7 C 0.3126(11) 0.7536(10) 1.0567(5) 0.0341(17) Uani 1 1 d . .
H7 H 0.3401 0.8668 1.0883 0.041 Uiso 1 1 calc R U
C8 C 0.3145(11) 0.7429(9) 0.9547(5) 0.0292(15) Uani 1 1 d . .
H8 H 0.3411 0.8469 0.9168 0.035 Uiso 1 1 calc R U
C9 C 0.2746(9) 0.5678(9) 0.9077(5) 0.0208(13) Uani 1 1 d . .
N1 N 0.2761(8) 0.5495(7) 0.8053(4) 0.0183(10) Uani 1 1 d . .
H1A H 0.3062 0.6460 0.7708 0.022 Uiso 1 1 calc R U
O1 O 0.2540(7) 0.5781(5) 0.5889(3) 0.0201(9) Uani 1 1 d . .
O2 O 0.4301(6) 0.3140(6) 0.6001(3) 0.0203(9) Uani 1 1 d . .
O3 O 0.0509(6) 0.2572(5) 0.5839(3) 0.0195(9) Uani 1 1 d . .
O4 O 0.2781(7) 0.8866(6) 0.2882(3) 0.0230(10) Uani 1 1 d . .
O5 O 0.4343(6) 1.0808(5) 0.4204(3) 0.0174(9) Uani 1 1 d . .
O6 O 0.2896(8) 1.2075(6) 0.2732(3) 0.0320(11) Uani 1 1 d . .
O7 O 0.5937(7) 1.0974(6) 0.2610(3) 0.0230(10) Uani 1 1 d . .
O1W O 0.1718(7) 0.4791(6) 0.3717(3) 0.0263(10) Uani 1 1 d . .
H1WA H 0.2213 0.4046 0.3372 0.040 Uiso 1 1 d R U
H1WB H 0.0686 0.4227 0.4016 0.040 Uiso 1 1 d R U
O2W O 0.1397(6) 0.9151(6) 0.5810(3) 0.0223(9) Uani 1 1 d . .
H2WA H 0.1042 0.8404 0.6279 0.033 Uiso 1 1 d R U
H2WB H 0.2263 1.0081 0.6050 0.033 Uiso 1 1 d R U
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Y Y -2.7962 3.5667 '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
O2 Y1 O1 97.24(15) 2_666 .
O2 Y1 O3 141.85(15) 2_666 2_566
O1 Y1 O3 96.20(15) . 2_566
O2 Y1 O1W 74.43(15) 2_666 .
O1 Y1 O1W 79.27(15) . .
O3 Y1 O1W 73.29(15) 2_566 .
O2 Y1 O2W 149.63(15) 2_666 .
O1 Y1 O2W 74.09(15) . .
O3 Y1 O2W 68.52(14) 2_566 .
O1W Y1 O2W 129.95(15) . .
O2 Y1 O5 90.14(15) 2_666 .
O1 Y1 O5 139.64(14) . .
O3 Y1 O5 102.11(14) 2_566 .
O1W Y1 O5 140.44(14) . .
O2W Y1 O5 79.66(14) . .
O2 Y1 O4 81.58(15) 2_666 .
O1 Y1 O4 162.87(14) . .
O3 Y1 O4 75.37(15) 2_566 .
O1W Y1 O4 83.99(15) . .
O2W Y1 O4 115.08(15) . .
O5 Y1 O4 57.47(13) . .
O2 Y1 O5 77.56(14) 2_666 2_676
O1 Y1 O5 77.37(14) . 2_676
O3 Y1 O5 140.38(14) 2_566 2_676
O1W Y1 O5 140.60(15) . 2_676
O2W Y1 O5 72.16(14) . 2_676
O5 Y1 O5 65.57(16) . 2_676
O4 Y1 O5 118.66(13) . 2_676
O2 P1 O3 113.5(2) . .
O2 P1 O1 115.2(2) . .
O3 P1 O1 113.6(2) . .
O2 P1 C1 105.3(3) . .
O3 P1 C1 103.5(3) . .
O1 P1 C1 104.0(3) . .
O6 S1 O4 112.4(3) . .
O6 S1 O7 109.7(3) . .
O4 S1 O7 110.5(3) . .
O6 S1 O5 111.5(3) . .
O4 S1 O5 103.6(2) . .
O7 S1 O5 109.0(2) . .
N1 C1 C2 118.2(5) . .
N1 C1 P1 119.3(4) . .
C2 C1 P1 122.4(5) . .
C3 C2 C1 121.2(6) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C2 C3 C4 120.7(6) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C9 C4 C5 118.7(6) . .
C9 C4 C3 117.1(6) . .
C5 C4 C3 124.2(6) . .
C6 C5 C4 120.3(6) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C7 120.7(6) . .
C5 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C8 C7 C6 121.8(7) . .
C8 C7 H7 119.1 . .
C6 C7 H7 119.1 . .
C7 C8 C9 118.3(6) . .
C7 C8 H8 120.9 . .
C9 C8 H8 120.9 . .
N1 C9 C4 119.1(6) . .
N1 C9 C8 120.6(6) . .
C4 C9 C8 120.3(6) . .
C1 N1 C9 123.6(5) . .
C1 N1 H1A 118.2 . .
C9 N1 H1A 118.2 . .
P1 O1 Y1 143.0(2) . .
P1 O2 Y1 169.0(3) . 2_666
P1 O3 Y1 144.4(2) . 2_566
S1 O4 Y1 99.7(2) . .
S1 O5 Y1 98.71(19) . .
S1 O5 Y1 136.9(2) . 2_676
Y1 O5 Y1 114.43(16) . 2_676
Y1 O1W H1WA 137.2 . .
Y1 O1W H1WB 107.7 . .
H1WA O1W H1WB 110.4 . .
Y1 O2W H2WA 108.3 . .
Y1 O2W H2WB 109.2 . .
H2WA O2W H2WB 109.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y1 O2 2.256(4) 2_666
Y1 O1 2.270(4) .
Y1 O3 2.333(4) 2_566
Y1 O1W 2.402(4) .
Y1 O2W 2.409(4) .
Y1 O5 2.435(4) .
Y1 O4 2.436(4) .
Y1 O5 2.484(4) 2_676
P1 O2 1.497(4) .
P1 O3 1.504(4) .
P1 O1 1.510(4) .
P1 C1 1.848(6) .
S1 O6 1.446(5) .
S1 O4 1.472(4) .
S1 O7 1.484(4) .
S1 O5 1.507(4) .
C1 N1 1.330(8) .
C1 C2 1.396(9) .
C2 C3 1.349(9) .
C2 H2 0.9300 .
C3 C4 1.419(9) .
C3 H3 0.9300 .
C4 C9 1.407(9) .
C4 C5 1.414(8) .
C5 C6 1.362(10) .
C5 H5 0.9300 .
C6 C7 1.391(10) .
C6 H6 0.9300 .
C7 C8 1.365(9) .
C7 H7 0.9300 .
C8 C9 1.428(9) .
C8 H8 0.9300 .
C9 N1 1.374(7) .
N1 H1A 0.8600 .
O2 Y1 2.256(4) 2_666
O3 Y1 2.333(4) 2_566
O5 Y1 2.484(4) 2_676
O1W H1WA 0.8584 .
O1W H1WB 0.8594 .
O2W H2WA 0.8569 .
O2W H2WB 0.8612 .
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
O2W H2WB O2 0.86 2.43 3.234(6) 154.7 1_565
O1W H1WB O1 0.86 2.20 2.905(6) 139.7 2_566
O1W H1WA O6 0.86 1.87 2.716(6) 168.6 1_545
N1 H1A O7 0.86 1.97 2.798(6) 160.0 2_676
N1 H1A O1 0.86 2.47 2.898(6) 111.5 .
N1 H1A S1 0.86 2.86 3.630(5) 150.0 2_676
C8 H8 O7 0.93 2.46 3.176(8) 133.5 2_676
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
_geom_torsion_site_symmetry_4
O2 P1 C1 N1 107.8(5) .
O3 P1 C1 N1 -132.8(5) .
O1 P1 C1 N1 -13.8(5) .
O2 P1 C1 C2 -70.7(6) .
O3 P1 C1 C2 48.7(6) .
O1 P1 C1 C2 167.8(5) .
N1 C1 C2 C3 -0.7(10) .
P1 C1 C2 C3 177.8(5) .
C1 C2 C3 C4 1.1(10) .
C2 C3 C4 C9 -0.5(10) .
C2 C3 C4 C5 179.4(7) .
C9 C4 C5 C6 0.8(10) .
C3 C4 C5 C6 -179.1(7) .
C4 C5 C6 C7 0.1(11) .
C5 C6 C7 C8 -0.1(12) .
C6 C7 C8 C9 -0.8(11) .
C5 C4 C9 N1 179.5(6) .
C3 C4 C9 N1 -0.5(9) .
C5 C4 C9 C8 -1.8(10) .
C3 C4 C9 C8 178.1(6) .
C7 C8 C9 N1 -179.6(6) .
C7 C8 C9 C4 1.8(10) .
C2 C1 N1 C9 -0.4(9) .
P1 C1 N1 C9 -179.0(4) .
C4 C9 N1 C1 1.0(9) .
C8 C9 N1 C1 -177.6(6) .
O2 P1 O1 Y1 59.2(5) .
O3 P1 O1 Y1 -74.2(5) .
C1 P1 O1 Y1 173.9(4) .
O3 P1 O2 Y1 90.2(14) 2_666
O1 P1 O2 Y1 -43.3(15) 2_666
C1 P1 O2 Y1 -157.3(13) 2_666
O2 P1 O3 Y1 -162.8(4) 2_566
O1 P1 O3 Y1 -28.6(5) 2_566
C1 P1 O3 Y1 83.6(5) 2_566
O6 S1 O4 Y1 -126.8(2) .
O7 S1 O4 Y1 110.3(2) .
O5 S1 O4 Y1 -6.3(3) .
O6 S1 O5 Y1 127.4(3) .
O4 S1 O5 Y1 6.3(3) .
O7 S1 O5 Y1 -111.4(2) .
O6 S1 O5 Y1 -91.7(4) 2_676
O4 S1 O5 Y1 147.2(3) 2_676
O7 S1 O5 Y1 29.6(4) 2_676
