A series of lanthanide(III) metal-organic frameworks derived from a pyridyl-dicarboxylate ligand: single-molecule magnet behaviour and luminescence properties.
Zhang, Chengcheng; Ma, Xiufang; Cen, Peipei; Jin, Xiaoyong; Yang, Jinhui; Zhang, Yi-Quan; Ferrando-Soria, Jesús; Pardo, Emilio; Liu, Xiangyu; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14123–14132; doi:10.1039/d0dt02736g

data_7705436
_publ_section_title
;
 A series of lanthanide(III) metal-organic frameworks derived from a
 pyridyl-dicarboxylate ligand: single-molecule magnet behaviour and
 luminescence properties.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14123
_journal_page_last               14132
_journal_paper_doi               10.1039/d0dt02736g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '0.5(C130 H78 N10 O42 Tb6), H4 O2'
_chemical_formula_sum            'C65 H43 N5 O23 Tb3'
_chemical_formula_weight         1738.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-29 deposited with the CCDC.	2020-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4772(5)
_cell_length_b                   27.6587(13)
_cell_length_c                   11.5564(5)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.71
_cell_volume                     3589.3(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.0
_diffrn_measured_fraction_theta_full 0.998
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            83567
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         1.957
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.999
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             1694
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         8383
_refine_ls_number_restraints     857
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+6.9668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7564
_reflns_number_total             8383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02736g16.cif
_cod_data_source_block           an1tb4_sq
_cod_depositor_comments
'Adding full bibliography for 7705434--7705437.cif.'
_cod_database_code               7705436
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2A-C7 \\sim O2-C7
 with sigma of 0.02
 O1-C7 \\sim O1A-C7
 with sigma of 0.02
 O1-O2 \\sim O1A-O2A
 with sigma of 0.02
 Tb1-O2A \\sim Tb1-O2
 with sigma of 0.02
 Tb1-O1 \\sim Tb1-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O1A \\sim O2 \\sim O2A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O6A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C34 \\sim C35 \\sim C36 \\sim N3 \\sim C37 \\sim C38 \\sim C9 \\sim C10 \\sim
N1 \\sim C11 \\sim C12 \\sim C12A \\sim C11A \\sim N1A \\sim C10A \\sim C9A
\\sim C8A \\sim C8: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N3, C27, C28, C29, C30, C31, C32, C34, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N1, C1, C2, C3, C4, C5, C6, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N1A, C1, C2A, C3A, C4, C5A, C6A, C8A, C9A, C10A, C11A, C12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O5, O6, O7, O8, C14, C15, C16, C17, C18, C19, C20, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O5, O6A, O7A, O8A, C14A, C15, C16, C17A, C18A, C19A, C20A, C21A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O1A, O2A, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O1, O2, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(N1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12C)=1-FVAR(1)
 Sof(N1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=
 Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=
 FVAR(1)
 Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(C14A)=Sof(H15A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(C21A)=1-FVAR(2)
 Sof(O6)=Sof(O7)=Sof(O8)=Sof(C14)=Sof(H15)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(C26)=FVAR(2)
 Sof(O1A)=Sof(O2A)=1-FVAR(3)
 Sof(O1)=Sof(O2)=FVAR(3)
 Fixed Sof: H12A(0.5) H12B(0.5) N3(0.5) C28(0.5) H28(0.5) C29(0.5) C31(0.5)
 H31(0.5) C32(0.5) H32(0.5) C34(0.5) C35(0.5) H35(0.5) C36(0.5) H36(0.5)
 C37(0.5) H37(0.5) C38(0.5) H38(0.5) O13(0.25) H13A(0.25) H13B(0.25) O14(0.5)
 H14A(0.5) H14B(0.5) O15(0.25) H15B(0.25) H15C(0.25)
6.a Riding coordinates:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15B,H15C)
6.b Rotating group:
 O12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N1A(H1A), C2(H2), C2A(H2A), C5(H5), C5A(H5A), C6(H6), C6A(H6A),
 C9(H9), C9A(H9A), C10(H10), C10A(H10A), C11(H11), C11A(H11A), C12(H12),
 C12A(H12C), C15(H15), C15(H15A), C18(H18), C18A(H18A), C19(H19), C19A(H19A),
 C22(H22), C23(H23), C24(H24), C25(H25), C28(H28), C31(H31), C32(H32), C35(H35),
  C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              21253
_shelx_fab_checksum              17405
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'