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_7233255
_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, C3 H7 N O'
_chemical_formula_sum            'C21 H27 N3 O12 Tb'
_chemical_formula_weight         672.37
_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             2018-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-03 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                103.484(5)
_cell_angle_beta                 110.657(6)
_cell_angle_gamma                96.519(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5445(7)
_cell_length_b                   11.0141(6)
_cell_length_c                   12.7860(8)
_cell_measurement_reflns_used    5433
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      31.8680
_cell_measurement_theta_min      1.9350
_cell_volume                     1319.52(16)
_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      300.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.743
_diffrn_measured_fraction_theta_max 0.680
_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      0.0618134000
_diffrn_orient_matrix_UB_12      -0.0147029000
_diffrn_orient_matrix_UB_13      0.0360151000
_diffrn_orient_matrix_UB_21      -0.0298104000
_diffrn_orient_matrix_UB_22      -0.0666789000
_diffrn_orient_matrix_UB_23      -0.0269725000
_diffrn_orient_matrix_UB_31      0.0280095000
_diffrn_orient_matrix_UB_32      0.0003611000
_diffrn_orient_matrix_UB_33      -0.0433120000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.743
_diffrn_reflns_Laue_measured_fraction_max 0.680
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8650
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.680
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.429
_diffrn_reflns_theta_min         1.957
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79544
_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    1.692
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.198
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4443
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4185
_reflns_number_total             4443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_300K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_original_cell_volume        1319.52(15)
_cod_database_code               7233255
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.610
_reflns_odcompleteness_completeness 73.14
_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
 C18A-N2 \\sim N2-C18B
 with sigma of 0.01
 C17B-N2 \\sim N2-C17A
 with sigma of 0.01
 C13B-N2 \\sim N2-C13A
 with sigma of 0.01
 C13B-O11B \\sim O11A-C13A
 with sigma of 0.01
 C18B-C17B \\sim C17A-C18A
 with sigma of 0.01
3. Restrained planarity
 C13B, C17B, C18B, N2, O11B
 with sigma of 0.1
 C13A, C17A, C18A, N2, O11A
 with sigma of 0.1
4. Rigid bond restraints
 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
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 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1A) = Uanis(C1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O11B) = Uanis(O11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C18B) = Uanis(C18A)
Uanis(C17B) = Uanis(C17A)
6. Rigid body (RIGU) restrains
 C1A, C2A, C3A, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C17A, C18A, N2, O11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13B, C17B, C18B, N2, O11B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C1B)=Sof(H1BA)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=FVAR(1)
 Sof(H12)=Sof(O1B)=Sof(H1B)=1-FVAR(2)
 Sof(H14)=Sof(O1A)=Sof(H1A)=FVAR(2)
 Sof(C13B)=Sof(H13B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(O11B)=1-FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O11A)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13A(H13A), C13B(H13B), C14(H14),
 C1A(H1AA), C1B(H1BA)
8.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
8.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C2A(H2AA,H2AB,H2AC),
 C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC)
8.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O9(H9), O12(H12A)
;
_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 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.828