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_7233257
_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            'C19.01 H22.36 N2.34 O11.34 Tb'
_chemical_formula_weight         623.95
_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                100.439(10)
_cell_angle_beta                 112.923(12)
_cell_angle_gamma                98.339(9)
_cell_formula_units_Z            2
_cell_length_a                   10.6610(13)
_cell_length_b                   11.0866(11)
_cell_length_c                   13.1016(15)
_cell_measurement_reflns_used    3370
_cell_measurement_temperature    360.0
_cell_measurement_theta_max      30.7490
_cell_measurement_theta_min      1.9090
_cell_volume                     1362.3(3)
_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      360.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.764
_diffrn_measured_fraction_theta_max 0.752
_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      0.0658365000
_diffrn_orient_matrix_UB_12      -0.0149533000
_diffrn_orient_matrix_UB_13      0.0280517000
_diffrn_orient_matrix_UB_21      -0.0315550000
_diffrn_orient_matrix_UB_22      -0.0653357000
_diffrn_orient_matrix_UB_23      -0.0282740000
_diffrn_orient_matrix_UB_31      0.0166758000
_diffrn_orient_matrix_UB_32      0.0074971000
_diffrn_orient_matrix_UB_33      -0.0466090000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.764
_diffrn_reflns_Laue_measured_fraction_max 0.752
_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            7880
_diffrn_reflns_point_group_measured_fraction_full 0.764
_diffrn_reflns_point_group_measured_fraction_max 0.752
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.510
_diffrn_reflns_theta_min         1.932
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38720
_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    1.521
_exptl_crystal_description       prism
_exptl_crystal_F_000             617
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.370
_refine_diff_density_min         -2.979
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4198
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0996
_refine_ls_shift/su_max          0.001
_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          0.2571
_refine_ls_wR_factor_ref         0.2788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3210
_reflns_number_total             4198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_360K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_database_code               7233257
_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   0.619
_reflns_odcompleteness_completeness 75.27
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 O11, C13, N2, C17, C18
 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
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 2.193
_oxdiff_exptl_absorpt_empirical_full_min 0.543