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_7245817
_publ_section_title
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 A reversible pressure-induced bond rearrangement of flexible lanthanide
 2,5-bis(allyloxy)terephthalate coordination polymer networks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00499B
_journal_year                    2022
_chemical_formula_moiety         'C24 H34 Ce N3 O11'
_chemical_formula_sum            'C24 H34 Ce N3 O11'
_chemical_formula_weight         680.66
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-17 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                109.534(4)
_cell_angle_beta                 95.570(4)
_cell_angle_gamma                96.701(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9080(16)
_cell_length_b                   11.1776(18)
_cell_length_c                   13.939(2)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.83
_cell_measurement_theta_min      5.27
_cell_volume                     1429.6(4)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42338
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.833
_diffrn_reflns_theta_min         3.400
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.835
_exptl_absorpt_correction_T_max  0.2956
_exptl_absorpt_correction_T_min  0.1565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1291 before and 0.1056 after correction.
The Ratio of minimum to maximum transmission is 0.5294.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       plate
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.533
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5030
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+2.1343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4909
_reflns_number_total             5030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00499b2.cif
_cod_data_source_block           022_r34
_cod_database_code               7245817
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.183
_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
 N2-C22 \\sim N2-C24
 with sigma of 0.02
 C25-C24 \\sim C22-C23
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C25 \\sim C24 \\sim C22 \\sim C23: 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. Others
 Fixed Sof: C24(0.57544) H24A(0.57544) H24B(0.57544) C25(0.57544)
 H25A(0.57544) H25B(0.57544) H25C(0.57544) C23(0.42456) H23A(0.42456)
 H23B(0.42456) H23C(0.42456) C22(0.42456) H22A(0.42456) H22B(0.42456)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C21(H21A,H21B), C17(H17A,H17B), C16(H16A,H16B),
 C24(H24A,H24B), C22(H22A,H22B)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C4(H4), C6(H6), C20(H20), C15(H15), C13(H13)
6.c X=CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'