A reversible pressure-induced bond rearrangement of flexible lanthanide 2,5-bis(allyloxy)terephthalate coordination polymer networks
Hunter, L. R.; Sellars, J. D.; Probert, M. R.; CrystEngComm  (2022) –; doi:10.1039/D2CE00499B

data_7245821
_publ_section_title
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 A reversible pressure-induced bond rearrangement of flexible lanthanide
 2,5-bis(allyloxy)terephthalate coordination polymer networks
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00499B
_journal_year                    2022
_chemical_formula_moiety         'C24 H34 N3 O11 Tb'
_chemical_formula_sum            'C24 H34 N3 O11 Tb'
_chemical_formula_weight         699.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-21 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
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_cell_angle_alpha                83.999(5)
_cell_angle_beta                 71.592(6)
_cell_angle_gamma                89.746(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4991(13)
_cell_length_b                   10.5703(13)
_cell_length_c                   13.8816(17)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    290.0
_cell_measurement_theta_max      66.748
_cell_measurement_theta_min      3.376
_cell_volume                     1453.1(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      290.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15951
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.217
_diffrn_reflns_theta_max         67.217
_diffrn_reflns_theta_min         4.649
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.490
_exptl_absorpt_correction_T_max  0.5060
_exptl_absorpt_correction_T_min  0.2074
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1242 before and 0.0949 after correction.
The Ratio of minimum to maximum transmission is 0.4099.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0824P)^2^+1.9350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4613
_reflns_number_total             5063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00499b2.cif
_cod_data_source_block           022_r39_rt
_cod_database_code               7245821
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.563
_shelx_estimated_absorpt_t_min   0.265
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-C18
 2.5 with sigma of 0.02
 N2_$1-C18_$1 \\sim N2_$1-C16_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16 \\sim C17: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C16(H16A,H16B), C18(H18A,H18B), C21(H21A,H21B),
 C23(H23A,H23B)
5.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C13(H13), C15(H15), C20(H20)
5.d X=CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B)
5.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
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_olex2_submission_special_instructions 'No special instructions were received'