#------------------------------------------------------------------------------
#$Date: 2023-04-27 18:28:39 +0300 (Thu, 27 Apr 2023) $
#$Revision: 282882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/13/7201311.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_7201311
loop_
_publ_author_name
'Liao, Wuping'
'Liu, Ce'
'Wang, Xiaofei'
'Zhu, Guangshan'
'Zhao, Xiaojun'
'Zhang, Hongjie'
_publ_section_title
;
 3D metal--organic frameworks incorporating water-soluble
 tetra-p-sulfonatocalix[4]arene
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2282
_journal_paper_doi               10.1039/b908189e
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety
'[(CH3)4N] Nd [C12H8N2]2 [C28H20S4O16] 3.5H2O'
_chemical_formula_sum            'C56 H55 N5 Nd O19.5 S4'
_chemical_formula_weight         1382.53
_chemical_name_common
'[(CH3)4N] Nd [C12H8N2]2 [C28H20S4O16] 3.5H2O'
_chemical_name_systematic
;
?
;
_space_group_IT_number           132
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c 2c'
_symmetry_space_group_name_H-M   'P 42/m c m'
_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                   18.9307(13)
_cell_length_b                   18.9307(13)
_cell_length_c                   20.989(2)
_cell_measurement_temperature    145(2)
_cell_volume                     7521.9(10)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      145(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS Apex CCD diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56661
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.8821
_exptl_absorpt_correction_T_min  0.8235
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ' SADABS, Sheldrick, 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.684
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.386
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.1259
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1804P)²+83.9760P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3533
_refine_ls_wR_factor_ref         0.3685
_reflns_number_gt                2699
_reflns_number_total             3580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B908189E.txt
_cod_data_source_block           Nd-N(CH3)4
_cod_original_formula_sum        'C56 H55 N5 Nd O19.50 S4'
_cod_database_code               7201311
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'y, x, -z'
'-y, -x, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z-1/2'
'-y, x, -z-1/2'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-y, -x, z'
'y, x, 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
Nd1A Nd 0.0000 0.5000 0.2500 0.039(2) Uani 0.88(3) 4 d SP . .
Nd1B Nd 0.0000 0.5000 0.221(3) 0.039(2) Uani 0.059(16) 2 d SP . .
S1 S 0.07249(18) 0.3433(2) 0.16456(14) 0.0716(11) Uani 1 1 d . . .
N1 N 0.1199(5) 0.4540(5) 0.2999(5) 0.055(2) Uani 1 1 d . . .
C1 C 0.3494(8) 0.3494(8) 0.1697(7) 0.061(5) Uani 1 2 d S . .
H1A H 0.3414 0.3414 0.2158 0.073 Uiso 1 2 calc SR . .
H1B H 0.3862 0.3862 0.1653 0.073 Uiso 1 2 calc SR . .
C2 C 0.2817(6) 0.3753(6) 0.1397(4) 0.053(3) Uani 1 1 d . . .
C3 C 0.2160(6) 0.3519(6) 0.1635(5) 0.060(3) Uani 1 1 d . . .
H3 H 0.2145 0.3210 0.1992 0.072 Uiso 1 1 calc R . .
C4 C 0.1541(7) 0.3737(7) 0.1350(5) 0.065(3) Uani 1 1 d . . .
C5 C 0.1563(6) 0.4201(6) 0.0838(5) 0.061(3) Uani 1 1 d . . .
H5 H 0.1134 0.4369 0.0658 0.073 Uiso 1 1 calc R . .
C6 C 0.2185(6) 0.4416(6) 0.0593(4) 0.053(3) Uani 1 1 d . . .
C7 C 0.2818(6) 0.4195(6) 0.0875(4) 0.053(3) Uani 1 1 d . . .
C8 C 0.2178(9) 0.4884(9) 0.0000 0.058(4) Uani 1 2 d S . .
H8A H 0.1750 0.5185 0.0000 0.069 Uiso 1 2 calc SR . .
H8B H 0.2598 0.5196 0.0000 0.069 Uiso 1 2 calc SR . .
C9 C 0.1217(7) 0.4101(7) 0.3485(7) 0.073(4) Uani 1 1 d . . .
H9 H 0.0777 0.3948 0.3653 0.088 Uiso 1 1 calc R . .
C10 C 0.1828(8) 0.3840(7) 0.3776(7) 0.081(4) Uani 1 1 d . . .
H10 H 0.1801 0.3522 0.4125 0.097 Uiso 1 1 calc R . .
C11 C 0.2473(7) 0.4058(7) 0.3540(7) 0.070(4) Uani 1 1 d . . .
H11 H 0.2903 0.3898 0.3723 0.084 Uiso 1 1 calc R . .
C12 C 0.2470(5) 0.4528(6) 0.3017(6) 0.058(3) Uani 1 1 d . . .
C13 C 0.3127(6) 0.4781(7) 0.2740(6) 0.072(4) Uani 1 1 d . . .
H13 H 0.3564 0.4626 0.2913 0.086 Uiso 1 1 calc R . .
C14 C 0.1824(5) 0.4755(5) 0.2766(5) 0.049(2) Uani 1 1 d . . .
O1 O 0.3436(4) 0.4426(5) 0.0635(4) 0.069(2) Uani 1 1 d . . .
O2 O 0.0388(6) 0.3073(6) 0.1128(4) 0.090(3) Uani 1 1 d . . .
O3 O 0.0346(4) 0.4081(5) 0.1813(3) 0.066(2) Uani 1 1 d . . .
O4 O 0.0869(6) 0.2999(6) 0.2192(5) 0.100(4) Uani 1 1 d . . .
N2 N 0.186(3) 0.186(3) 0.0000 0.167(11) Uiso 0.50 4 d SPD . .
C15 C 0.238(3) 0.238(3) 0.0000 0.167(11) Uiso 0.50 4 d SPD . .
C16 C 0.114(2) 0.209(4) 0.0000 0.167(11) Uiso 0.50 2 d SPD . .
C17 C 0.191(3) 0.191(3) 0.0681(12) 0.167(11) Uiso 0.25 2 d SPD . .
N3 N 0.0000 0.0000 0.2500 0.167(11) Uiso 1 8 d SD . .
C18 C -0.0409(11) 0.0409(11) 0.2936(16) 0.167(11) Uiso 1 2 d SD . .
O1W O 0.5000 0.5000 0.2500 0.133(14) Uiso 1 8 d S . .
O2W O -0.0302(19) 0.3589(18) 0.0000 0.209(12) Uiso 1 2 d S . .
O3W O 0.309(2) 0.309(2) 0.5000 0.28(3) Uiso 1 4 d S . .
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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
Nd1B Nd1A Nd1B 179.99(5) 5 . ?
Nd1B Nd1A O3 127.79(19) 5 . ?
Nd1B Nd1A O3 52.21(19) . . ?
Nd1B Nd1A O3 52.21(19) 5 5 ?
Nd1B Nd1A O3 127.79(19) . 5 ?
O3 Nd1A O3 84.6(4) . 5 ?
Nd1B Nd1A O3 127.79(19) 5 2_565 ?
Nd1B Nd1A O3 52.21(19) . 2_565 ?
O3 Nd1A O3 104.4(4) . 2_565 ?
O3 Nd1A O3 147.6(4) 5 2_565 ?
Nd1B Nd1A O3 52.21(19) 5 6_565 ?
Nd1B Nd1A O3 127.79(19) . 6_565 ?
O3 Nd1A O3 147.6(4) . 6_565 ?
O3 Nd1A O3 104.4(4) 5 6_565 ?
O3 Nd1A O3 84.6(4) 2_565 6_565 ?
Nd1B Nd1A N1 113.3(2) 5 5 ?
Nd1B Nd1A N1 66.7(2) . 5 ?
O3 Nd1A N1 75.7(3) . 5 ?
O3 Nd1A N1 76.1(3) 5 5 ?
O3 Nd1A N1 76.2(3) 2_565 5 ?
O3 Nd1A N1 136.4(3) 6_565 5 ?
Nd1B Nd1A N1 66.7(2) 5 2_565 ?
Nd1B Nd1A N1 113.3(2) . 2_565 ?
O3 Nd1A N1 136.4(3) . 2_565 ?
O3 Nd1A N1 76.2(3) 5 2_565 ?
O3 Nd1A N1 76.1(3) 2_565 2_565 ?
O3 Nd1A N1 75.7(3) 6_565 2_565 ?
N1 Nd1A N1 61.9(4) 5 2_565 ?
Nd1B Nd1A N1 113.3(2) 5 6_565 ?
Nd1B Nd1A N1 66.7(2) . 6_565 ?
O3 Nd1A N1 76.2(3) . 6_565 ?
O3 Nd1A N1 136.4(3) 5 6_565 ?
O3 Nd1A N1 75.7(3) 2_565 6_565 ?
O3 Nd1A N1 76.1(3) 6_565 6_565 ?
N1 Nd1A N1 133.4(4) 5 6_565 ?
N1 Nd1A N1 141.6(4) 2_565 6_565 ?
Nd1B Nd1A N1 66.7(2) 5 . ?
Nd1B Nd1A N1 113.3(2) . . ?
O3 Nd1A N1 76.1(3) . . ?
O3 Nd1A N1 75.7(3) 5 . ?
O3 Nd1A N1 136.4(3) 2_565 . ?
O3 Nd1A N1 76.2(3) 6_565 . ?
N1 Nd1A N1 141.6(4) 5 . ?
N1 Nd1A N1 133.4(4) 2_565 . ?
N1 Nd1A N1 61.9(4) 6_565 . ?
Nd1A Nd1B Nd1B 0.003(8) . 5 ?
Nd1A Nd1B O3 114.4(17) . . ?
Nd1B Nd1B O3 114.4(17) 5 . ?
Nd1A Nd1B O3 114.4(17) . 2_565 ?
Nd1B Nd1B O3 114.4(17) 5 2_565 ?
O3 Nd1B O3 131(3) . 2_565 ?
Nd1A Nd1B N1 100.4(15) . 5 ?
Nd1B Nd1B N1 100.4(15) 5 5 ?
O3 Nd1B N1 85.4(9) . 5 ?
O3 Nd1B N1 86.0(10) 2_565 5 ?
Nd1A Nd1B N1 100.4(15) . 6_565 ?
Nd1B Nd1B N1 100.4(15) 5 6_565 ?
O3 Nd1B N1 86.0(10) . 6_565 ?
O3 Nd1B N1 85.4(9) 2_565 6_565 ?
N1 Nd1B N1 159(3) 5 6_565 ?
Nd1A Nd1B O3 42.3(9) . 5 ?
Nd1B Nd1B O3 42.3(9) 5 5 ?
O3 Nd1B O3 81.0(9) . 5 ?
O3 Nd1B O3 140.0(16) 2_565 5 ?
N1 Nd1B O3 72.2(7) 5 5 ?
N1 Nd1B O3 125.0(16) 6_565 5 ?
Nd1A Nd1B O3 42.3(9) . 6_565 ?
Nd1B Nd1B O3 42.3(9) 5 6_565 ?
O3 Nd1B O3 140.0(16) . 6_565 ?
O3 Nd1B O3 81.0(9) 2_565 6_565 ?
N1 Nd1B O3 125.0(16) 5 6_565 ?
N1 Nd1B O3 72.2(7) 6_565 6_565 ?
O3 Nd1B O3 84.7(19) 5 6_565 ?
Nd1A Nd1B N1 55.9(11) . 2_565 ?
Nd1B Nd1B N1 55.9(11) 5 2_565 ?
O3 Nd1B N1 137.1(8) . 2_565 ?
O3 Nd1B N1 74.4(6) 2_565 2_565 ?
N1 Nd1B N1 59.7(6) 5 2_565 ?
N1 Nd1B N1 135.0(14) 6_565 2_565 ?
O3 Nd1B N1 65.7(11) 5 2_565 ?
O3 Nd1B N1 65.3(11) 6_565 2_565 ?
Nd1A Nd1B N1 55.9(11) . . ?
Nd1B Nd1B N1 55.9(11) 5 . ?
O3 Nd1B N1 74.4(6) . . ?
O3 Nd1B N1 137.1(8) 2_565 . ?
N1 Nd1B N1 135.0(14) 5 . ?
N1 Nd1B N1 59.7(6) 6_565 . ?
O3 Nd1B N1 65.3(11) 5 . ?
O3 Nd1B N1 65.7(11) 6_565 . ?
N1 Nd1B N1 112(2) 2_565 . ?
O2 S1 O4 114.7(8) . . ?
O2 S1 O3 111.3(6) . . ?
O4 S1 O3 112.4(6) . . ?
O2 S1 C4 106.2(6) . . ?
O4 S1 C4 107.5(6) . . ?
O3 S1 C4 103.9(6) . . ?
C9 N1 C14 116.8(10) . . ?
C9 N1 Nd1B 112.7(14) . 5 ?
C14 N1 Nd1B 129.5(12) . 5 ?
C9 N1 Nd1A 122.4(8) . . ?
C14 N1 Nd1A 120.8(7) . . ?
Nd1B N1 Nd1A 12.9(15) 5 . ?
C9 N1 Nd1B 129.9(10) . . ?
C14 N1 Nd1B 112.8(10) . . ?
Nd1B N1 Nd1B 24(3) 5 . ?
Nd1A N1 Nd1B 10.8(11) . . ?
C2 C1 C2 112.2(13) . 16 ?
C7 C2 C3 118.3(10) . . ?
C7 C2 C1 121.9(12) . . ?
C3 C2 C1 119.8(11) . . ?
C4 C3 C2 120.0(10) . . ?
C3 C4 C5 119.9(13) . . ?
C3 C4 S1 119.7(10) . . ?
C5 C4 S1 120.4(9) . . ?
C6 C5 C4 120.9(10) . . ?
C5 C6 C7 119.7(10) . . ?
C5 C6 C8 118.6(11) . . ?
C7 C6 C8 121.6(12) . . ?
O1 C7 C2 119.7(9) . . ?
O1 C7 C6 119.3(9) . . ?
C2 C7 C6 121.0(11) . . ?
C6 C8 C6 109.1(13) 10 . ?
N1 C9 C10 125.6(13) . . ?
C11 C10 C9 117.9(12) . . ?
C10 C11 C12 117.7(11) . . ?
C14 C12 C11 119.3(11) . . ?
C14 C12 C13 119.8(12) . . ?
C11 C12 C13 120.9(10) . . ?
C13 C13 C12 121.1(7) 6_565 . ?
N1 C14 C12 122.7(10) . . ?
N1 C14 C14 118.3(6) . 6_565 ?
C12 C14 C14 119.0(7) . 6_565 ?
S1 O3 Nd1B 166.1(14) . . ?
S1 O3 Nd1A 154.6(5) . . ?
Nd1B O3 Nd1A 13.4(17) . . ?
S1 O3 Nd1B 145.3(10) . 5 ?
Nd1B O3 Nd1B 23(3) . 5 ?
Nd1A O3 Nd1B 9.9(9) . 5 ?
C15 N2 C16 117(5) . 7 ?
C15 N2 C16 117(5) . . ?
C16 N2 C16 126(10) 7 . ?
C15 N2 C17 85(4) . 10 ?
C16 N2 C17 92.5(15) 7 10 ?
C16 N2 C17 92.5(15) . 10 ?
C15 N2 C17 85(4) . . ?
C16 N2 C17 92.5(15) 7 . ?
C16 N2 C17 92.5(15) . . ?
C17 N2 C17 169(7) 10 . ?
N2 C15 C17 48.4(17) . 10 ?
N2 C15 C17 48.4(17) . . ?
C17 C15 C17 97(3) 10 . ?
N2 C17 C15 47(2) . . ?
C18 N3 C18 114.3(18) . 12_556 ?
C18 N3 C18 100(3) . 2 ?
C18 N3 C18 114.3(18) 12_556 2 ?
C18 N3 C18 114.3(18) . 11_556 ?
C18 N3 C18 100(3) 12_556 11_556 ?
C18 N3 C18 114.3(18) 2 11_556 ?
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
Nd1A Nd1B 0.60(7) 5 ?
Nd1A Nd1B 0.60(7) . ?
Nd1A O3 2.353(8) . ?
Nd1A O3 2.353(8) 5 ?
Nd1A O3 2.353(8) 2_565 ?
Nd1A O3 2.353(8) 6_565 ?
Nd1A N1 2.647(9) 5 ?
Nd1A N1 2.647(9) 2_565 ?
Nd1A N1 2.647(9) 6_565 ?
Nd1A N1 2.647(9) . ?
Nd1B Nd1B 1.20(13) 5 ?
Nd1B O3 2.04(3) . ?
Nd1B O3 2.04(3) 2_565 ?
Nd1B N1 2.472(15) 5 ?
Nd1B N1 2.472(15) 6_565 ?
Nd1B O3 2.76(5) 5 ?
Nd1B O3 2.76(5) 6_565 ?
Nd1B N1 2.94(4) 2_565 ?
Nd1B N1 2.94(4) . ?
S1 O2 1.432(10) . ?
S1 O4 1.436(10) . ?
S1 O3 1.463(9) . ?
S1 C4 1.761(15) . ?
N1 C9 1.317(15) . ?
N1 C14 1.343(13) . ?
N1 Nd1B 2.472(15) 5 ?
C1 C2 1.511(13) . ?
C1 C2 1.511(13) 16 ?
C2 C7 1.378(15) . ?
C2 C3 1.412(17) . ?
C3 C4 1.379(16) . ?
C4 C5 1.390(16) . ?
C5 C6 1.347(16) . ?
C6 C7 1.402(14) . ?
C6 C8 1.527(14) . ?
C7 O1 1.345(14) . ?
C8 C6 1.527(14) 10 ?
C9 C10 1.399(18) . ?
C10 C11 1.38(2) . ?
C11 C12 1.414(19) . ?
C12 C14 1.398(14) . ?
C12 C13 1.454(17) . ?
C13 C13 1.31(3) 6_565 ?
C14 C14 1.45(2) 6_565 ?
O3 Nd1B 2.76(5) 5 ?
N2 C15 1.40(2) . ?
N2 C16 1.42(2) 7 ?
N2 C16 1.42(2) . ?
N2 C17 1.44(2) 10 ?
N2 C17 1.44(2) . ?
C15 C17 1.91(7) 10 ?
C15 C17 1.91(7) . ?
N3 C18 1.428(18) . ?
N3 C18 1.428(18) 12_556 ?
N3 C18 1.428(18) 2 ?
N3 C18 1.428(18) 11_556 ?
