#------------------------------------------------------------------------------
#$Date: 2021-04-19 12:29:21 +0300 (Mon, 19 Apr 2021) $
#$Revision: 264308 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/19/1561926.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_1561926
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Structural variations in terbium(III) complexes with
 1,3-adamantanedicarboxylate and diverse co-ligands
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              265
_journal_page_last               272
_journal_paper_doi               10.1016/j.jssc.2015.01.036
_journal_volume                  227
_journal_year                    2015
_chemical_formula_sum            'C14 H19 O7 Tb'
_chemical_formula_weight         458.21
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_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                   23.9695(14)
_cell_length_b                   6.7843(5)
_cell_length_c                   9.2303(3)
_cell_measurement_reflns_used    39394
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.37
_cell_volume                     1501.00(15)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and four ω scans with 2° steps (354 frames)'
_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  0.0184
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            39394
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.744
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.721
_refine_diff_density_min         -1.665
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0542
_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)+(0.0582P)²+11.2625P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                1394
_reflns_number_total             1545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2015-227-265.cif
_cod_data_source_block           2
_cod_database_code               1561926
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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
Tb1 Tb 0.53693(2) 0.2500 0.09144(5) 0.0439(3) Uani 1 2 d S . .
O1 O 0.6230(4) 0.3426(19) 0.2133(10) 0.045(3) Uani 0.50 1 d P . .
O2 O 0.5517(3) 0.2500 0.3476(8) 0.0357(17) Uani 1 2 d S . .
O3 O 0.6013(2) 0.4090(10) 0.9251(6) 0.0518(16) Uani 1 1 d . . .
O4 O 0.4824(2) 0.4108(11) -0.1248(6) 0.0509(17) Uani 1 1 d . . .
O5 O 0.4423(3) 0.2500 0.1709(8) 0.0410(19) Uani 1 2 d S . .
H5 H 0.4310 0.1289 0.1454 0.049 Uiso 1 1 d R . .
C1 C 0.6431(4) 0.2500 0.4624(11) 0.044(3) Uani 1 2 d S . .
C2 C 0.6100(4) 0.2500 0.6067(10) 0.029(2) Uani 1 2 d S . .
H2A H 0.5860 0.3680 0.6120 0.035 Uiso 1 1 d R . .
C3 C 0.6517(4) 0.2500 0.7329(10) 0.026(2) Uani 1 2 d S . .
C4 C 0.6886(3) 0.4341(12) 0.7241(8) 0.0362(16) Uani 1 1 d . . .
H4A H 0.6650 0.5537 0.7286 0.043 Uiso 1 1 calc R . .
H4B H 0.7145 0.4369 0.8075 0.043 Uiso 1 1 calc R . .
C5 C 0.7218(3) 0.4338(13) 0.5832(8) 0.0370(17) Uani 1 1 d . . .
H5A H 0.7457 0.5543 0.5789 0.044 Uiso 1 1 calc R . .
C6 C 0.6806(3) 0.4352(17) 0.4556(10) 0.058(3) Uani 1 1 d . . .
H6A H 0.7014 0.4370 0.3630 0.069 Uiso 1 1 calc R . .
H6B H 0.6571 0.5553 0.4601 0.069 Uiso 1 1 calc R . .
C7 C 0.7587(4) 0.2500 0.5741(11) 0.037(3) Uani 1 2 d S . .
H7A H 0.7859 0.2500 0.6547 0.044 Uiso 1 2 calc SR . .
H7B H 0.7796 0.2500 0.4816 0.044 Uiso 1 2 calc SR . .
C8 C 0.6036(5) 0.2500 0.3359(14) 0.078(6) Uani 1 2 d S . .
C9 C 0.6167(4) 0.2500 0.8690(11) 0.030(2) Uani 1 2 d S . .
C10 C 0.4718(4) 0.2500 -0.1896(12) 0.043(3) Uani 1 2 d S . .
C11 C 0.4503(5) 0.2500 -0.3413(14) 0.053(3) Uani 1 2 d S . .
H11A H 0.4103 0.2500 -0.3431 0.079 Uiso 1 2 d SR . .
H11B H 0.4640 0.3653 -0.3898 0.079 Uiso 1 1 d R . .
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'
Tb Tb -0.1723 4.1537 '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
O4 Tb1 O4 152.8(3) 3_645 5_665
O4 Tb1 O5 76.94(13) 3_645 .
O4 Tb1 O5 76.94(13) 5_665 .
O4 Tb1 O2 84.27(13) 3_645 .
O4 Tb1 O2 84.27(13) 5_665 .
O5 Tb1 O2 80.6(2) . .
O4 Tb1 O3 129.6(2) 3_645 1_554
O4 Tb1 O3 77.0(2) 5_665 1_554
O5 Tb1 O3 143.0(2) . 1_554
O2 Tb1 O3 122.1(2) . 1_554
O4 Tb1 O3 77.0(2) 3_645 7_564
O4 Tb1 O3 129.6(2) 5_665 7_564
O5 Tb1 O3 143.0(2) . 7_564
O2 Tb1 O3 122.1(2) . 7_564
O3 Tb1 O3 52.7(3) 1_554 7_564
O4 Tb1 O1 110.9(3) 3_645 .
O4 Tb1 O1 81.6(3) 5_665 .
O5 Tb1 O1 131.6(3) . .
O2 Tb1 O1 54.3(3) . .
O3 Tb1 O1 68.9(3) 1_554 .
O3 Tb1 O1 82.5(3) 7_564 .
O4 Tb1 O4 66.3(2) 3_645 7_565
O4 Tb1 O4 113.94(17) 5_665 7_565
O5 Tb1 O4 76.1(2) . 7_565
O2 Tb1 O4 145.71(19) . 7_565
O3 Tb1 O4 91.1(2) 1_554 7_565
O3 Tb1 O4 69.6(2) 7_564 7_565
O1 Tb1 O4 151.9(3) . 7_565
O4 Tb1 O4 113.94(17) 3_645 .
O4 Tb1 O4 66.3(2) 5_665 .
O5 Tb1 O4 76.1(2) . .
O2 Tb1 O4 145.71(19) . .
O3 Tb1 O4 69.6(2) 1_554 .
O3 Tb1 O4 91.1(2) 7_564 .
O1 Tb1 O4 131.9(3) . .
O4 Tb1 O4 49.1(3) 7_565 .
C8 O1 Tb1 88.6(7) . .
C8 O2 Tb1 93.6(7) . .
C9 O3 Tb1 93.8(5) . 1_556
C10 O4 Tb1 149.0(6) . 5_665
C10 O4 Tb1 95.8(6) . .
Tb1 O4 Tb1 113.7(2) 5_665 .
Tb1 O5 H5 102.0 . .
C8 C1 C6 109.5(6) . 7_565
C8 C1 C6 109.5(6) . .
C6 C1 C6 108.8(9) 7_565 .
C8 C1 C2 110.2(8) . .
C6 C1 C2 109.4(6) 7_565 .
C6 C1 C2 109.4(6) . .
C3 C2 C1 108.6(8) . .
C3 C2 H2A 110.0 . .
C1 C2 H2A 109.9 . .
C9 C3 C4 111.4(5) . 7_565
C9 C3 C4 111.4(5) . .
C4 C3 C4 109.2(8) 7_565 .
C9 C3 C2 105.6(7) . .
C4 C3 C2 109.6(5) 7_565 .
C4 C3 C2 109.6(5) . .
C5 C4 C3 110.2(6) . .
C5 C4 H4A 109.6 . .
C3 C4 H4A 109.6 . .
C5 C4 H4B 109.6 . .
C3 C4 H4B 109.6 . .
H4A C4 H4B 108.1 . .
C4 C5 C7 110.5(7) . .
C4 C5 C6 108.5(6) . .
C7 C5 C6 109.5(7) . .
C4 C5 H5A 109.4 . .
C7 C5 H5A 109.4 . .
C6 C5 H5A 109.4 . .
C5 C6 C1 109.7(7) . .
C5 C6 H6A 109.7 . .
C1 C6 H6A 109.7 . .
C5 C6 H6B 109.7 . .
C1 C6 H6B 109.7 . .
H6A C6 H6B 108.2 . .
C5 C7 C5 109.1(8) . 7_565
C5 C7 H7A 109.9 . .
C5 C7 H7A 109.9 7_565 .
C5 C7 H7B 109.9 . .
C5 C7 H7B 109.9 7_565 .
H7A C7 H7B 108.3 . .
O2 C8 O1 114.1(10) . .
O2 C8 C1 124.1(10) . .
O1 C8 C1 115.2(9) . .
O3 C9 O3 119.0(10) . 7_565
O3 C9 C3 120.5(5) . .
O3 C9 C3 120.5(5) 7_565 .
O4 C10 O4 118.4(10) . 7_565
O4 C10 C11 120.7(5) . .
O4 C10 C11 120.7(5) 7_565 .
C10 C11 H11A 111.2 . .
C10 C11 H11B 108.7 . .
H11A C11 H11B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O4 2.368(8) 3_645
Tb1 O4 2.368(8) 5_665
Tb1 O5 2.383(7) .
Tb1 O2 2.391(7) .
Tb1 O3 2.429(6) 1_554
Tb1 O3 2.429(6) 7_564
Tb1 O1 2.433(9) .
Tb1 O4 2.624(6) 7_565
Tb1 O4 2.624(6) .
O1 C8 1.375(14) .
O2 C8 1.249(14) .
O3 C9 1.252(8) .
O3 Tb1 2.429(6) 1_556
O4 C10 1.269(9) .
O4 Tb1 2.368(8) 5_665
O5 H5 0.8968 .
C1 C8 1.502(16) .
C1 C6 1.546(12) 7_565
C1 C6 1.546(12) .
C1 C2 1.550(13) .
C2 C3 1.535(13) .
C2 H2A 0.9880 .
C3 C9 1.512(13) .
C3 C4 1.532(9) 7_565
C3 C4 1.532(9) .
C4 C5 1.524(10) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C7 1.531(10) .
C5 C6 1.538(11) .
C5 H5A 1.0000 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C5 1.531(10) 7_565
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 O1 1.375(14) 7_565
C9 O3 1.252(8) 7_565
C10 O4 1.269(9) 7_565
C10 C11 1.491(16) .
C11 H11A 0.9587 .
C11 H11B 0.9591 .
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
O5 H5 O3 0.90 1.80 2.689(8) 169.5 3_646
