Tuning dimensionality between 2D and 1D MOFs by lanthanide contraction and ligand-to-metal ratio
González Chávez, Fernando; Beltrán, Hiram Isaac; New Journal of Chemistry 45 (2021) 6600–6610; doi:10.1039/D0NJ04055J

data_7060377
_publ_section_title
;
 Tuning dimensionality between 2D and 1D MOFs by lanthanide contraction
 and ligand-to-metal ratio
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6600
_journal_page_last               6610
_journal_paper_doi               10.1039/D0NJ04055J
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C22 H24 N5 O13 Tm'
_chemical_formula_sum            'C22 H24 N5 O13 Tm'
_chemical_formula_weight         735.39
_chemical_melting_point          673.15
_chemical_name_common            PBIA-Tm1D
_chemical_name_systematic
'catena Thulium (III) - (2,2'-(1,3,5,7-tetraoxo-5,7-dihydropyrrolo[3,4-f]isoindole-2,6(1H,3H)-diyl)dipropionate)-2-dimethylformamide solvate-1-NO3 solvate'
_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     heavy
_audit_creation_date             2020-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-21 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                64.282(2)
_cell_angle_beta                 76.253(2)
_cell_angle_gamma                84.090(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6753(5)
_cell_length_b                   12.6601(7)
_cell_length_c                   13.8621(7)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.69
_cell_volume                     1332.37(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      177.79
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            236958
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.464
_diffrn_reflns_theta_min         2.417
_exptl_absorpt_coefficient_mu    3.406
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method
'In-Situ Crystallization during the reaction'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.568
_refine_diff_density_min         -1.968
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         13053
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0176P)^2^+1.5669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9928
_reflns_number_total             13053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04055j2.cif
_cod_data_source_block           fer03-tm
_cod_depositor_comments          'Adding full bibliography for 7060377.cif.'
_cod_database_code               7060377
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.564
_exptl_absorpt_special_details   multi-scan
_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
2. Restrained distances
 C11-O22 \\sim C11A-O22A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C11-N10 \\sim C11A-N10A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C5-O24 \\sim C5A-O24A
 with sigma of 0.02
 C5-N4 \\sim C5A-N4A
 with sigma of 0.02
 O23-C15 \\sim O23A-C15A
 with sigma of 0.02
 O21-C9 \\sim O21A-C9A
 with sigma of 0.02
 C2-C3 \\sim C2-C3A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 C12-C8 \\sim C12A-C8A
 with sigma of 0.02
 C17-C16 \\sim C17-C16A
 with sigma of 0.02
 C3-C25A \\sim C3A-C25
 with sigma of 0.02
 C3-N4 \\sim C3A-N4A
 with sigma of 0.02
 C14-C6 \\sim C14A-C6A
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C14-C13 \\sim C14A-C13A
 with sigma of 0.02
 C7-C6 \\sim C7A-C6A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C16-C20A \\sim C16A-C20
 with sigma of 0.02
 C16-N10 \\sim C16A-N10A
 with sigma of 0.02
 C9-C8 \\sim C9A-C8A
 with sigma of 0.02
 C9-N10 \\sim C9A-N10A
 with sigma of 0.02
 C15-N4 \\sim C15A-N4A
 with sigma of 0.02
 C11-C16 \\sim C11A-C16A
 with sigma of 0.04
 C11-C9 \\sim C11A-C9A
 with sigma of 0.04
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
 C11-C8 \\sim C11A-C8A
 with sigma of 0.04
 O22-C12 \\sim O22A-C12A
 with sigma of 0.04
 O22-N10 \\sim O22A-N10A
 with sigma of 0.04
 C5-C3 \\sim C5A-C3A
 with sigma of 0.04
 C5-C14 \\sim C5A-C14A
 with sigma of 0.04
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 C5-C15 \\sim C5A-C15A
 with sigma of 0.04
 O23-C14 \\sim O23A-C14A
 with sigma of 0.04
 O23-N4 \\sim O23A-N4A
 with sigma of 0.04
 O21-C8 \\sim O21A-C8A
 with sigma of 0.04
 O21-N10 \\sim O21A-N10A
 with sigma of 0.04
 C2-C25A \\sim C2-C25
 with sigma of 0.04
 C2-N4 \\sim C2-N4A
 with sigma of 0.04
 C12-C14 \\sim C12A-C14A
 with sigma of 0.04
 C12-C7 \\sim C12A-C7A
 with sigma of 0.04
 C12-C9 \\sim C12A-C9A
 with sigma of 0.04
 C12-N10 \\sim C12A-N10A
 with sigma of 0.04
 C17-C20A \\sim C17-C20
 with sigma of 0.04
 C17-N10 \\sim C17-N10A
 with sigma of 0.04
 C3-C15 \\sim C3A-C15A
 with sigma of 0.04
 C14-C7 \\sim C14A-C7A
 with sigma of 0.04
 C14-N4 \\sim C14A-N4A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C16-C9 \\sim C16A-C9A
 with sigma of 0.04
 C20A-N10 \\sim C20-N10A
 with sigma of 0.04
 C6-C15 \\sim C6A-C15A
 with sigma of 0.04
 C6-C13 \\sim C6A-C13A
 with sigma of 0.04
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 C6-O24 \\sim C6A-O24A
 with sigma of 0.04
 C6-N4 \\sim C6A-N4A
 with sigma of 0.04
 C15-C13 \\sim C15A-C13A
 with sigma of 0.04
 C13-C8 \\sim C13A-C8A
 with sigma of 0.04
 C8-N10 \\sim C8A-N10A
 with sigma of 0.04
 C25A-N4 \\sim C25-N4A
 with sigma of 0.04
 O24-N4 \\sim O24A-N4A
 with sigma of 0.04
 Tm1-O32A \\sim Tm1-O32
 with sigma of 0.02
 N34-C36 \\sim N34-C35A
 with sigma of 0.02
 N34-C33 \\sim N34-C33A
 with sigma of 0.02
 N34-C35 \\sim N34-C36A
 with sigma of 0.02
 C33-O32A \\sim C33A-O32
 with sigma of 0.02
 Tm1-C33 \\sim Tm1-C33A
 with sigma of 0.04
 N34-O32A \\sim N34-O32
 with sigma of 0.04
 Tm1-O27 \\sim Tm1-O27A
 with sigma of 0.02
 O27-C28 \\sim O27A-C28A
 with sigma of 0.02
 C31-N29 \\sim C30A-N29A
 with sigma of 0.02
 N29-C28 \\sim N29A-C28A
 with sigma of 0.02
 Tm1-C28 \\sim Tm1-C28A
 with sigma of 0.04
 O27-N29 \\sim O27A-N29A
 with sigma of 0.04
 C31-C28 \\sim C30A-C28A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O27) \\sim Ueq, Uanis(O27A) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(N29) \\sim Ueq, Uanis(N29A) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O39) \\sim Ueq, Uanis(N38) \\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O40)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) = Uanis(C28A)
Uanis(O27) = Uanis(C30A) = Uanis(C31) = Uanis(C30) = Uanis(C31A)
4. Others
 Fixed Sof: O27A(0.5) O21(0.5) O21A(0.5) O23(0.5) O23A(0.5) O22(0.5) O22A(0.5)
 O32A(0.5) O32(0.5) O24(0.5) O24A(0.5) O27(0.5) N29(0.5) N29A(0.5) N10(0.5)
 N10A(0.5) N4(0.5) N4A(0.5) C33A(0.5) H33A(0.5) C3A(0.5) H3A(0.5) C25(0.5)
 H25A(0.5) H25B(0.5) H25C(0.5) C6(0.5) C12(0.5) C12A(0.5) C8(0.5) C14(0.5)
 C15(0.5) C28(0.5) H28(0.5) C7(0.5) H7(0.5) C25A(0.5) H25D(0.5) H25E(0.5)
 H25F(0.5) C9(0.5) C13(0.5) H13(0.5) C20A(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 C3(0.5) H3(0.5) C16(0.5) H16(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C30A(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C11(0.5) C11A(0.5) C14A(0.5) C28A(0.5)
 H28A(0.5) C5(0.5) C5A(0.5) C7A(0.5) H7A(0.5) C31A(0.5) H31D(0.5) H31E(0.5)
 H31F(0.5) C35A(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C16A(0.5) H16A(0.5)
 C36A(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C20(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
 C6A(0.5) C9A(0.5) C30(0.5) H30D(0.5) H30E(0.5) H30F(0.5) C15A(0.5) C13A(0.5)
 H13A(0.5) C8A(0.5) C36(0.5) H36D(0.5) H36E(0.5) H36F(0.5) C33(0.5) H33(0.5)
 C35(0.5) H35D(0.5) H35E(0.5) H35F(0.5)
5.a Ternary CH refined with riding coordinates:
 C3A(H3A), C3(H3), C16(H16), C16A(H16A)
5.b Aromatic/amide H refined with riding coordinates:
 C33A(H33A), C28(H28), C7(H7), C13(H13), C28A(H28A), C7A(H7A), C13A(H13A),
 C33(H33)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C20A(H20A,H20B,H20C), C31(H31A,
 H31B,H31C), C30A(H30A,H30B,H30C), C31A(H31D,H31E,H31F), C35A(H35A,H35B,H35C),
 C36A(H36A,H36B,H36C), C20(H20D,H20E,H20F), C30(H30D,H30E,H30F), C36(H36D,H36E,
 H36F), C35(H35D,H35E,H35F)
;
_shelx_res_checksum              19915
_shelx_hkl_checksum              3712
_olex2_submission_original_sample_id PBIA-Tm1D
_olex2_submission_special_instructions 'No special instructions were received'