#------------------------------------------------------------------------------
#$Date: 2025-08-04 10:03:09 +0300 (Mon, 04 Aug 2025) $
#$Revision: 301442 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/64/7056438.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_7056438
loop_
_publ_author_name
'Beyer, Ole'
'Homburg, Thomas'
'Albat, Martin'
'Stock, Norbert'
'Luening, Ulrich'
_publ_section_title
;
 Synthesis of phosphonosulfonic acid building blocks as linkers for
 coordination polymers
;
_journal_issue                   17
_journal_name_full               'New J. Chem.'
_journal_page_first              8870
_journal_page_last               8876
_journal_paper_doi               10.1039/C7NJ01697B
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C15 H26 La2 O22 P3 S3'
_chemical_formula_weight         1025.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-03 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.047(4)
_cell_length_b                   11.357(2)
_cell_length_c                   18.677(4)
_cell_measurement_reflns_used    26130
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      56.01
_cell_measurement_theta_min      4.07
_cell_volume                     3736.6(17)
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19490
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.449
_diffrn_reflns_theta_min         2.036
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  0.8019
_exptl_absorpt_correction_T_min  0.6378
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED and X-SHAPE (STOE, 2008)'
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       prism
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.1333
_exptl_crystal_size_mid          0.1059
_exptl_crystal_size_min          0.0603
_refine_diff_density_max         1.523
_refine_diff_density_min         -1.914
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0667
_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)+(0.0506P)²+130.8599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3990
_reflns_number_total             4470
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj01697b2.cif
_cod_data_source_block           thc1
_cod_original_cell_volume        3736.3(16)
_cod_database_code               7056438
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_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.
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.80074(4) 0.5000 0.69994(4) 0.03173(18) Uani 1 2 d S T P A .
La2 La 0.77987(4) 0.0000 0.68406(4) 0.03557(19) Uani 1 2 d S T P A .
O1 O 0.6987(5) 0.5000 0.5458(5) 0.046(2) Uani 1 2 d S T P . .
O2 O 0.6799(6) 0.0000 0.5264(6) 0.053(2) Uani 1 2 d S T P . .
O3 O 0.7607(10) 0.0000 0.8162(10) 0.096(5) Uani 1 2 d S T P . .
O4 O 0.7811(10) 0.5000 0.8323(9) 0.097(5) Uani 1 2 d S T P . .
S1 S 0.65849(12) 0.25291(19) 0.67967(14) 0.0361(4) Uani 0.5 1 d . . P A 1
P1 P 0.65849(12) 0.25291(19) 0.67967(14) 0.0361(4) Uani 0.5 1 d . . P A 2
O5 O 0.6816(3) 0.1386(6) 0.6590(5) 0.0550(18) Uani 1 1 d . . . . .
O6 O 0.7081(3) 0.3513(6) 0.6857(5) 0.0525(17) Uani 1 1 d . . . . .
O7 O 0.6530(4) 0.2385(8) 0.7571(4) 0.063(2) Uani 1 1 d . . . . .
C1 C 0.5648(4) 0.2822(7) 0.6007(5) 0.0356(17) Uani 1 1 d . . . . .
H1B H 0.5654 0.2909 0.5483 0.043 Uiso 1 1 calc R U . A 1
H1A H 0.5315 0.2148 0.5956 0.043 Uiso 1 1 calc R U . A 1
C2 C 0.5335(4) 0.3918(7) 0.6177(5) 0.0322(16) Uani 1 1 d . . . . .
C3 C 0.5537(6) 0.5000 0.5984(7) 0.034(2) Uani 1 2 d S T P . .
H3 H 0.5829 0.5000 0.5706 0.041 Uiso 1 2 calc R U P . .
C4 C 0.4694(6) 0.5000 0.6783(7) 0.030(2) Uani 1 2 d S T P . .
H4 H 0.4415 0.5000 0.7075 0.036 Uiso 1 2 calc R U P . .
C5 C 0.4895(4) 0.3922(7) 0.6573(5) 0.0313(15) Uani 1 1 d . . . . .
C6 C 0.4602(5) 0.2813(7) 0.6762(5) 0.0372(17) Uani 1 1 d . . . . .
H6B H 0.4665 0.2868 0.7320 0.045 Uiso 1 1 calc R U . B 1
H6A H 0.4907 0.2137 0.6748 0.045 Uiso 1 1 calc R U . B 1
S2 S 0.36183(12) 0.25539(19) 0.60548(13) 0.0366(4) Uani 0.5 1 d . . P C 1
P2 P 0.36183(12) 0.25539(19) 0.60548(13) 0.0366(4) Uani 0.5 1 d . . P C 2
O8 O 0.3398(4) 0.1406(6) 0.6250(4) 0.0499(16) Uani 1 1 d . . . . .
O9 O 0.3172(4) 0.3566(6) 0.6091(4) 0.0497(16) Uani 1 1 d . . . . .
O10 O 0.3574(4) 0.2513(6) 0.5223(4) 0.0499(16) Uani 1 1 d . . . . .
S3 S 0.89193(13) 0.7571(2) 0.84216(14) 0.0419(5) Uani 0.5 1 d . . P A 1
P3 P 0.89193(13) 0.7571(2) 0.84216(14) 0.0419(5) Uani 0.5 1 d . . P A 2
O11 O 0.8875(4) 0.6399(6) 0.8046(4) 0.0562(18) Uani 1 1 d . . . . .
O12 O 0.8485(5) 0.7577(10) 0.8897(5) 0.089(3) Uani 1 1 d . . . . .
O13 O 0.8673(4) 0.8560(6) 0.7835(4) 0.0520(17) Uani 1 1 d . . . . .
C7 C 0.9896(5) 0.7809(8) 0.9139(5) 0.0413(19) Uani 1 1 d . . . . .
H7B H 1.0091 0.7131 0.9517 0.050 Uiso 1 1 calc R U . A 1
H7A H 1.0197 0.7874 0.8848 0.050 Uiso 1 1 calc R U . A 1
C8 C 0.9981(5) 0.8930(8) 0.9620(5) 0.0382(18) Uani 1 1 d . . . . .
C9 C 0.9948(7) 1.0000 0.9242(7) 0.038(3) Uani 1 2 d S T P . .
H9 H 0.9902 1.0000 0.8712 0.046 Uiso 1 2 calc R U P . .
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'
S S 0.1246 0.1234 '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'
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
O6 La1 O6 88.1(3) . 6_565
O6 La1 O11 138.2(3) . .
O6 La1 O11 81.5(2) 6_565 .
O6 La1 O11 81.5(2) . 6_565
O6 La1 O11 138.2(3) 6_565 6_565
O11 La1 O11 79.9(3) . 6_565
O6 La1 O8 85.5(2) . 8
O6 La1 O8 144.6(2) 6_565 8
O11 La1 O8 124.5(2) . 8
O11 La1 O8 75.0(2) 6_565 8
O6 La1 O8 144.6(2) . 3
O6 La1 O8 85.5(2) 6_565 3
O11 La1 O8 75.0(2) . 3
O11 La1 O8 124.5(2) 6_565 3
O8 La1 O8 80.0(3) 8 3
O6 La1 O1 74.0(2) . .
O6 La1 O1 74.0(2) 6_565 .
O11 La1 O1 138.95(17) . .
O11 La1 O1 138.95(17) 6_565 .
O8 La1 O1 70.8(2) 8 .
O8 La1 O1 70.8(2) 3 .
O6 La1 O4 70.1(3) . .
O6 La1 O4 70.1(3) 6_565 .
O11 La1 O4 68.2(3) . .
O11 La1 O4 68.2(3) 6_565 .
O8 La1 O4 138.07(19) 8 .
O8 La1 O4 138.07(19) 3 .
O1 La1 O4 129.2(4) . .
O5 La2 O5 82.5(3) 6 .
O5 La2 O13 143.9(3) 6 6_565
O5 La2 O13 86.2(2) . 6_565
O5 La2 O13 86.2(2) 6 1_545
O5 La2 O13 143.9(3) . 1_545
O13 La2 O13 83.0(3) 6_565 1_545
O5 La2 O9 84.3(2) 6 3_545
O5 La2 O9 139.9(2) . 3_545
O13 La2 O9 124.2(2) 6_565 3_545
O13 La2 O9 72.1(2) 1_545 3_545
O5 La2 O9 139.9(2) 6 8
O5 La2 O9 84.3(2) . 8
O13 La2 O9 72.1(2) 6_565 8
O13 La2 O9 124.2(2) 1_545 8
O9 La2 O9 81.9(3) 3_545 8
O5 La2 O2 70.6(2) 6 .
O5 La2 O2 70.6(2) . .
O13 La2 O2 136.34(18) 6_565 .
O13 La2 O2 136.34(18) 1_545 .
O9 La2 O2 69.3(2) 3_545 .
O9 La2 O2 69.3(2) 8 .
O5 La2 O3 73.3(3) 6 .
O5 La2 O3 73.3(3) . .
O13 La2 O3 70.6(3) 6_565 .
O13 La2 O3 70.6(3) 1_545 .
O9 La2 O3 137.31(19) 3_545 .
O9 La2 O3 137.31(19) 8 .
O2 La2 O3 131.2(4) . .
O6 S1 O5 113.7(4) . .
O6 S1 O7 111.5(5) . .
O5 S1 O7 109.1(5) . .
O6 S1 C1 109.3(4) . .
O5 S1 C1 106.5(4) . .
O7 S1 C1 106.5(4) . .
O6 P1 O5 113.7(4) . .
O6 P1 O7 111.5(5) . .
O5 P1 O7 109.1(5) . .
O6 P1 C1 109.3(4) . .
O5 P1 C1 106.5(4) . .
O7 P1 C1 106.5(4) . .
P1 O5 La2 148.6(4) . .
S1 O5 La2 148.6(4) . .
P1 O6 La1 174.2(4) . .
S1 O6 La1 174.2(4) . .
C2 C1 S1 111.3(6) . .
C2 C1 P1 111.3(6) . .
C3 C2 C5 118.0(8) . .
C3 C2 C1 118.4(7) . .
C5 C2 C1 123.4(7) . .
C2 C3 C2 123.6(10) . 6_565
C5 C4 C5 121.6(10) . 6_565
C2 C5 C4 119.3(8) . .
C2 C5 C6 122.7(7) . .
C4 C5 C6 117.9(7) . .
C5 C6 P2 112.3(6) . .
C5 C6 S2 112.3(6) . .
O8 S2 O9 114.6(4) . .
O8 S2 O10 110.3(4) . .
O9 S2 O10 109.3(4) . .
O8 S2 C6 108.4(4) . .
O9 S2 C6 108.3(4) . .
O10 S2 C6 105.4(4) . .
O8 P2 O9 114.6(4) . .
O8 P2 O10 110.3(4) . .
O9 P2 O10 109.3(4) . .
O8 P2 C6 108.4(4) . .
O9 P2 C6 108.3(4) . .
O10 P2 C6 105.4(4) . .
P2 O8 La1 156.7(4) . 3_445
S2 O8 La1 156.7(4) . 3_445
P2 O9 La2 152.5(4) . 3_455
S2 O9 La2 152.5(4) . 3_455
O13 S3 O11 114.0(4) . .
O13 S3 O12 110.4(6) . .
O11 S3 O12 111.1(5) . .
O13 S3 C7 107.4(4) . .
O11 S3 C7 106.6(4) . .
O12 S3 C7 106.9(5) . .
O13 P3 O11 114.0(4) . .
O13 P3 O12 110.4(6) . .
O11 P3 O12 111.1(5) . .
O13 P3 C7 107.4(4) . .
O11 P3 C7 106.6(4) . .
O12 P3 C7 106.9(5) . .
P3 O11 La1 143.9(4) . .
S3 O11 La1 143.9(4) . .
P3 O13 La2 157.9(4) . 1_565
S3 O13 La2 157.9(4) . 1_565
C8 C7 S3 110.1(6) . .
C8 C7 P3 110.1(6) . .
C8 C8 C9 119.1(6) 2_757 .
C8 C8 C7 122.8(5) 2_757 .
C9 C8 C7 117.8(8) . .
C8 C9 C8 121.7(11) 6_575 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O6 2.429(6) .
La1 O6 2.429(6) 6_565
La1 O11 2.475(7) .
La1 O11 2.475(7) 6_565
La1 O8 2.484(6) 8
La1 O8 2.484(6) 3
La1 O1 2.617(9) .
La1 O4 2.683(13) .
La2 O5 2.387(6) 6
La2 O5 2.387(6) .
La2 O13 2.467(7) 6_565
La2 O13 2.467(6) 1_545
La2 O9 2.485(7) 3_545
La2 O9 2.485(7) 8
La2 O2 2.655(9) .
La2 O3 2.673(15) .
S1 O6 1.464(6) .
S1 O5 1.490(7) .
S1 O7 1.510(7) .
S1 C1 1.781(8) .
P1 O6 1.464(6) .
P1 O5 1.490(7) .
P1 O7 1.510(7) .
P1 C1 1.781(8) .
C1 C2 1.495(11) .
C2 C3 1.394(9) .
C2 C5 1.394(10) .
C3 C2 1.394(9) 6_565
C4 C5 1.403(9) .
C4 C5 1.403(9) 6_565
C5 C6 1.501(11) .
C6 P2 1.798(9) .
C6 S2 1.798(9) .
S2 O8 1.477(7) .
S2 O9 1.477(7) .
S2 O10 1.514(7) .
P2 O8 1.477(7) .
P2 O9 1.477(7) .
P2 O10 1.514(7) .
O8 La1 2.484(6) 3_445
O9 La2 2.485(7) 3_455
S3 O13 1.480(7) .
S3 O11 1.487(7) .
S3 O12 1.512(8) .
S3 C7 1.787(9) .
P3 O13 1.480(7) .
P3 O11 1.487(7) .
P3 O12 1.512(8) .
P3 C7 1.787(9) .
O13 La2 2.467(6) 1_565
C7 C8 1.520(12) .
C8 C8 1.384(17) 2_757
C8 C9 1.391(10) .
C9 C8 1.391(10) 6_575
