Guest-dependent negative thermal expansion in a lanthanide-based metal‒organic framework
Gładysiak, Andrzej; Moosavi, Seyed Mohamad; Sarkisov, Lev; Smit, Berend; Stylianou, Kyriakos C.; CrystEngComm 21 (2019) 5292–; doi:10.1039/C9CE00941H

data_7233256
_publ_section_title
;
 Guest-dependent negative thermal expansion in a lanthanide-based
 metal--organic framework
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5292
_journal_paper_doi               10.1039/C9CE00941H
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                98.788(14)
_cell_angle_beta                 113.593(18)
_cell_angle_gamma                99.692(11)
_cell_formula_units_Z            2
_cell_length_a                   10.6786(15)
_cell_length_b                   11.0643(14)
_cell_length_c                   13.078(3)
_cell_measurement_reflns_used    2347
_cell_measurement_temperature    380.0
_cell_measurement_theta_max      25.7430
_cell_measurement_theta_min      1.9210
_cell_volume                     1353.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      380.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.733
_diffrn_measured_fraction_theta_max 0.722
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0673581000
_diffrn_orient_matrix_UB_12      -0.0130799000
_diffrn_orient_matrix_UB_13      0.0268784000
_diffrn_orient_matrix_UB_21      -0.0315185000
_diffrn_orient_matrix_UB_22      -0.0657871000
_diffrn_orient_matrix_UB_23      -0.0264320000
_diffrn_orient_matrix_UB_31      0.0127053000
_diffrn_orient_matrix_UB_32      0.0077512000
_diffrn_orient_matrix_UB_33      -0.0485231000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_Laue_measured_fraction_full 0.733
_diffrn_reflns_Laue_measured_fraction_max 0.722
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7717
_diffrn_reflns_point_group_measured_fraction_full 0.733
_diffrn_reflns_point_group_measured_fraction_max 0.722
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.511
_diffrn_reflns_theta_min         1.935
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.882
_refine_diff_density_min         -3.132
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.1222
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2995
_refine_ls_wR_factor_ref         0.3150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2987
_reflns_number_total             3995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_380K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_original_cell_volume        1353.7(4)
_cod_database_code               7233256
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.618
_reflns_odcompleteness_completeness 72.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O11-C13
 1.21 with sigma of 0.02
 O5-C10
 1.21 with sigma of 0.02
 C10-N1
 1.4 with sigma of 0.02
 C13-N2
 1.4 with sigma of 0.02
 N1-C16
 1.45 with sigma of 0.02
 N1-C15
 1.45 with sigma of 0.02
 N2-C17
 1.45 with sigma of 0.02
 N2-C18
 1.45 with sigma of 0.02
 O11-C13
 1.2 with sigma of 0.04
 O5-C10
 1.2 with sigma of 0.04
 C17-N2 \\sim N2-C18
 with sigma of 0.02
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C15-N1 \\sim N1-C16
 with sigma of 0.02
 C15-C10 \\sim C10-C16
 with sigma of 0.02
3. Restrained planarity
 O11, C13, N2, C17, C18
 with sigma of 0.1
 O5, C10, N1, C15, C16
 with sigma of 0.1
4. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 C2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 O3, C2, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C13 \\sim N2 \\sim C18 \\sim C17: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C10 \\sim N1 \\sim C16 \\sim C15: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C2 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C10, N1, C16, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O1B)=Sof(H1B)=Sof(H12A)=1-FVAR(1)
 Sof(O1A)=Sof(H1A)=Sof(H14)=FVAR(1)
8.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
8.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14)
8.c Tetrahedral OH refined with riding coordinates:
 O9(H9), O12(H12), O1A(H1A), O1B(H1B)
;
_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 2.622
_oxdiff_exptl_absorpt_empirical_full_min 0.442