#------------------------------------------------------------------------------
#$Date: 2017-05-18 04:58:38 +0300 (Thu, 18 May 2017) $
#$Revision: 196712 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/82/7228259.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_7228259
loop_
_publ_author_name
'Anderson, Samantha'
'Gladysiak, Andrzej'
'Boyd, Peter G.'
'Ireland, Christopher'
'Miéville, Pascal'
'tiana, davide'
'Vlaisavljevich, Bess'
'Schouwink, Pascal'
'van Beek, Wouter'
'Gagnon, Kevin J.'
'Smit, Berend'
'Stylianou, Kyriakos'
_publ_section_title
;
 Formation Pathways of Metal Organic Frameworks Proceeding Through Partial
 Dissolution of the Metastable Phase
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00589J
_journal_year                    2017
_chemical_formula_moiety         'C12 H6 O13 Tb, 3(H2 O)'
_chemical_formula_sum            'C12 H12 O16 Tb'
_chemical_formula_weight         571.14
_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   geom
_audit_creation_date             2017-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-05-01 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                113.409(10)
_cell_angle_beta                 101.145(9)
_cell_angle_gamma                105.464(8)
_cell_formula_units_Z            2
_cell_length_a                   9.5715(9)
_cell_length_b                   10.1208(10)
_cell_length_c                   11.6980(13)
_cell_measurement_reflns_used    1984
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.2520
_cell_measurement_theta_min      2.0440
_cell_volume                     943.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.810
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -95.00 140.00   1.00   12.00    --    0.00   0.00   0.00  235
  2  ω    -15.00 130.00   1.00   12.00    --    0.00  40.00   0.00  145
  3  ω    -80.00  60.00   1.00   12.00    --    0.00 -40.00   0.00  140
  4  ω    -90.00  65.00   1.00   12.00    --    0.00  65.00   0.00  155
;
_diffrn_measurement_device_type  'Oxford diffraction, KM 6, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0595590000
_diffrn_orient_matrix_UB_12      -0.0761549000
_diffrn_orient_matrix_UB_13      -0.0340861000
_diffrn_orient_matrix_UB_21      0.0534674000
_diffrn_orient_matrix_UB_22      -0.0325671000
_diffrn_orient_matrix_UB_23      -0.0222671000
_diffrn_orient_matrix_UB_31      0.0195788000
_diffrn_orient_matrix_UB_32      -0.0089948000
_diffrn_orient_matrix_UB_33      0.0579297000
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7153
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_Laue_measured_fraction_full 0.810
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6544
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.416
_diffrn_reflns_theta_max         25.661
_diffrn_reflns_theta_min         2.029
_diffrn_source
;
ESRF, Swiss-Norwegian Beamline BM01
;
_exptl_absorpt_coefficient_mu    3.885
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            beige
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_description       plate
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.565
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.820
_refine_diff_density_min         -4.956
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         2780
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0770
_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)+(0.1547P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2142
_reflns_number_total             2780
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00589j2.cif
_cod_data_source_block           Sion-2_H2O
_cod_original_cell_volume        943.19(18)
_cod_database_code               7228259
_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.
;
_reflns_odcompleteness_completeness 79.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4A), C7(H7), C12(H12)
3.b Tetrahedral OH refined with riding coordinates:
 O4(H4)
3.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.609
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
Tb1 Tb 0.63804(8) 0.58918(8) 0.86884(8) 0.0314(4) Uani 1 1 d . .
O1 O 0.4082(12) 0.5066(14) 0.8896(13) 0.043(3) Uani 1 1 d . .
O2 O 0.2245(13) 0.3443(13) 0.9129(13) 0.047(3) Uani 1 1 d . .
O3 O 0.4407(11) 0.3784(12) 0.6543(12) 0.041(3) Uani 1 1 d . .
O4 O 0.0280(12) 0.0490(11) 0.1973(11) 0.032(3) Uani 1 1 d . U
H4 H -0.0362 0.0002 0.1201 0.048 Uiso 1 1 calc R .
O5 O -0.1894(12) 0.0267(12) 0.2429(11) 0.036(3) Uani 1 1 d . .
O6 O -0.1920(12) 0.1016(14) 0.4763(13) 0.042(3) Uani 1 1 d . .
H6 H -0.2300 0.0816 0.3976 0.062 Uiso 1 1 calc GR .
O7 O 0.7689(11) 0.5130(12) 0.7160(11) 0.035(3) Uani 1 1 d . .
O8 O 0.6070(12) 0.3893(12) 0.5096(13) 0.040(3) Uani 1 1 d . .
O9 O 1.0591(12) 0.6148(13) 0.7687(12) 0.036(3) Uani 1 1 d . .
H9 H 0.9852 0.5654 0.7833 0.055 Uiso 1 1 calc GR .
O10 O 0.6567(14) 0.3532(12) 0.8548(13) 0.041(3) Uani 1 1 d . .
O11 O 0.8821(12) 0.7976(13) 0.9431(12) 0.039(3) Uani 1 1 d . .
O12 O 0.5604(12) 0.7025(13) 0.7399(13) 0.042(3) Uani 1 1 d . .
O13 O 0.6069(14) 0.8218(12) 1.0103(14) 0.051(3) Uani 1 1 d . .
C1 C 0.2838(18) 0.3896(18) 0.8402(18) 0.035(4) Uani 1 1 d . U
C2 C 0.2049(18) 0.3084(17) 0.6992(16) 0.033(4) Uani 1 1 d . .
C3 C 0.2850(17) 0.3046(16) 0.6062(16) 0.026(3) Uani 1 1 d . U
C4 C 0.2019(18) 0.2259(17) 0.4704(17) 0.032(4) Uani 1 1 d . .
H4A H 0.2568 0.2221 0.4104 0.038 Uiso 1 1 calc R .
C5 C 0.0437(17) 0.1538(15) 0.4206(16) 0.029(4) Uani 1 1 d . U
C6 C -0.0341(17) 0.1621(17) 0.5146(17) 0.031(4) Uani 1 1 d . .
C7 C 0.0448(17) 0.2327(17) 0.6446(17) 0.032(4) Uani 1 1 d . .
H7 H -0.0115 0.2311 0.7029 0.038 Uiso 1 1 calc R .
C8 C -0.0432(17) 0.0719(17) 0.2808(17) 0.029(3) Uani 1 1 d . U
C9 C 0.7395(17) 0.4580(16) 0.5901(15) 0.027(4) Uani 1 1 d . .
C10 C 0.8758(16) 0.4771(15) 0.5441(16) 0.027(4) Uani 1 1 d . .
C11 C 1.0272(17) 0.5560(16) 0.6341(16) 0.028(3) Uani 1 1 d . U
C12 C 0.8501(16) 0.4220(15) 0.4103(14) 0.024(3) Uani 1 1 d . U
H12 H 0.7479 0.3690 0.3490 0.029 Uiso 1 1 calc R .
O3W O 0.6818(16) 1.188(2) 1.0150(18) 0.119(9) Uani 1 1 d . .
O1W O 0.7078(13) 0.9960(13) 0.7942(12) 0.041(3) Uani 1 1 d . .
O2W O -0.3804(12) 0.1020(13) 0.6207(12) 0.040(3) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0760 4.2260 '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
O1 Tb1 O2 93.7(4) . 2_667
O1 Tb1 O3 68.3(4) . .
O1 Tb1 O7 139.9(4) . .
O1 Tb1 O10 86.8(4) . .
O1 Tb1 O11 148.6(4) . .
O1 Tb1 O12 94.4(4) . .
O1 Tb1 O13 74.5(4) . .
O2 Tb1 O3 145.5(4) 2_667 .
O2 Tb1 O7 114.1(4) 2_667 .
O2 Tb1 O10 75.2(4) 2_667 .
O2 Tb1 O11 71.5(4) 2_667 .
O2 Tb1 O13 74.3(4) 2_667 .
O7 Tb1 O3 72.7(4) . .
O7 Tb1 O10 74.2(4) . .
O7 Tb1 O11 70.8(4) . .
O7 Tb1 O13 138.8(4) . .
O10 Tb1 O3 74.6(4) . .
O10 Tb1 O11 114.4(4) . .
O10 Tb1 O13 142.8(5) . .
O11 Tb1 O3 137.5(4) . .
O11 Tb1 O13 74.9(4) . .
O12 Tb1 O2 141.3(4) . 2_667
O12 Tb1 O3 71.6(4) . .
O12 Tb1 O7 81.7(4) . .
O12 Tb1 O10 142.9(4) . .
O12 Tb1 O11 82.4(4) . .
O12 Tb1 O13 71.6(4) . .
O13 Tb1 O3 124.3(4) . .
C1 O1 Tb1 142.7(11) . .
C1 O2 Tb1 124.1(11) . 2_667
C3 O3 Tb1 136.5(10) . .
C8 O4 H4 109.5 . .
C6 O6 H6 109.5 . .
C9 O7 Tb1 137.3(9) . .
C11 O9 H9 109.5 . .
O1 C1 O2 121.1(16) . .
O1 C1 C2 119.6(15) . .
O2 C1 C2 119.2(14) . .
C1 C2 C3 122.4(14) . .
C7 C2 C1 121.8(15) . .
C7 C2 C3 115.8(15) . .
O3 C3 C2 118.2(14) . .
O3 C3 C4 121.9(14) . .
C4 C3 C2 119.8(14) . .
C3 C4 H4A 118.8 . .
C5 C4 C3 122.5(15) . .
C5 C4 H4A 118.8 . .
C4 C5 C6 116.9(15) . .
C4 C5 C8 123.0(15) . .
C6 C5 C8 120.1(13) . .
O6 C6 C5 121.7(15) . .
C7 C6 O6 117.2(15) . .
C7 C6 C5 121.1(14) . .
C2 C7 H7 118.1 . .
C6 C7 C2 123.9(16) . .
C6 C7 H7 118.1 . .
O4 C8 C5 119.5(13) . .
O5 C8 O4 121.2(15) . .
O5 C8 C5 119.3(14) . .
O7 C9 C10 116.5(13) . .
O8 C9 O7 122.8(14) . .
O8 C9 C10 120.7(14) . .
C11 C10 C9 121.5(15) . .
C12 C10 C9 118.6(13) . .
C12 C10 C11 119.8(14) . .
O9 C11 C10 122.2(14) . .
C12 C11 O9 117.5(13) 2_766 .
C12 C11 C10 120.3(15) 2_766 .
C10 C12 H12 120.1 . .
C11 C12 C10 119.8(14) 2_766 .
C11 C12 H12 120.1 2_766 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.232(11) .
Tb1 O2 2.359(14) 2_667
Tb1 O3 2.486(11) .
Tb1 O7 2.375(10) .
Tb1 O10 2.385(10) .
Tb1 O11 2.407(10) .
Tb1 O12 2.353(13) .
Tb1 O13 2.417(10) .
O1 C1 1.262(19) .
O2 Tb1 2.359(13) 2_667
O2 C1 1.27(2) .
O3 C3 1.358(17) .
O4 H4 0.8400 .
O4 C8 1.278(18) .
O5 C8 1.274(18) .
O6 H6 0.8400 .
O6 C6 1.373(18) .
O7 C9 1.290(18) .
O8 C9 1.236(18) .
O9 H9 0.8400 .
O9 C11 1.378(19) .
C1 C2 1.44(2) .
C2 C3 1.44(2) .
C2 C7 1.40(2) .
C3 C4 1.40(2) .
C4 H4A 0.9500 .
C4 C5 1.38(2) .
C5 C6 1.43(2) .
C5 C8 1.44(2) .
C6 C7 1.34(2) .
C7 H7 0.9500 .
C9 C10 1.50(2) .
C10 C11 1.40(2) .
C10 C12 1.38(2) .
C11 C12 1.37(2) 2_766
C12 C11 1.37(2) 2_766
C12 H12 0.9500 .
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_1
_geom_torsion_site_symmetry_4
Tb1 O1 C1 O2 132.4(16) . .
Tb1 O1 C1 C2 -50(3) . .
Tb1 O2 C1 O1 -20(2) 2_667 .
Tb1 O2 C1 C2 162.0(11) 2_667 .
Tb1 O3 C3 C2 -22(2) . .
Tb1 O3 C3 C4 158.6(11) . .
Tb1 O7 C9 O8 -21(2) . .
Tb1 O7 C9 C10 160.4(9) . .
O1 C1 C2 C3 28(2) . .
O1 C1 C2 C7 -149.4(16) . .
O2 C1 C2 C3 -153.4(15) . .
O2 C1 C2 C7 29(2) . .
O3 C3 C4 C5 -178.4(13) . .
O6 C6 C7 C2 -175.7(14) . .
O7 C9 C10 C11 -2.4(19) . .
O7 C9 C10 C12 -179.1(12) . .
O8 C9 C10 C11 179.4(13) . .
O8 C9 C10 C12 3(2) . .
C1 C2 C3 O3 1(2) . .
C1 C2 C3 C4 -179.0(14) . .
C1 C2 C7 C6 176.7(15) . .
C2 C3 C4 C5 2(2) . .
C3 C2 C7 C6 -1(2) . .
C3 C4 C5 C6 0(2) . .
C3 C4 C5 C8 -179.8(13) . .
C4 C5 C6 O6 176.5(13) . .
C4 C5 C6 C7 -2(2) . .
C4 C5 C8 O4 8(2) . .
C4 C5 C8 O5 -170.4(13) . .
C5 C6 C7 C2 3(2) . .
C6 C5 C8 O4 -171.6(13) . .
C6 C5 C8 O5 10(2) . .
C7 C2 C3 O3 179.1(13) . .
C7 C2 C3 C4 -1(2) . .
C8 C5 C6 O6 -4(2) . .
C8 C5 C6 C7 177.5(14) . .
C9 C10 C11 O9 3(2) . .
C9 C10 C11 C12 -177.0(13) . 2_766
C9 C10 C12 C11 177.1(13) . 2_766
C11 C10 C12 C11 0(2) . 2_766
C12 C10 C11 O9 179.3(13) . .
C12 C10 C11 C12 0(2) . 2_766
