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_7705437
_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 Eu6 N10 O42), 1.25(H4 O2)'
_chemical_formula_sum            'C65 H44 Eu3 N5 O23.5'
_chemical_formula_weight         1726.93
_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             2020-06-16
_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                 102.121(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.520(2)
_cell_length_b                   27.700(5)
_cell_length_c                   11.600(2)
_cell_measurement_reflns_used    9031
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.27
_cell_volume                     3619.1(11)
_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      298.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            78404
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.407
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         8452
_refine_ls_number_restraints     829
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0322P)^2^+9.8181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7966
_reflns_number_total             8452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02736g16.cif
_cod_data_source_block           an1eu_sq
_cod_depositor_comments
'Adding full bibliography for 7705434--7705437.cif.'
_cod_original_cell_volume        3619.2(12)
_cod_original_formula_sum        'C65 H44 Eu3 N5 O23.50'
_cod_database_code               7705437
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.742
_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) groups, All O(H,H) groups
2. Restrained distances
 O9A-C27 \\sim O9-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34A \\sim C35A \\sim C36A \\sim N3A \\sim C37A \\sim C38A \\sim C34 \\sim C38
\\sim C37 \\sim N3 \\sim C36 \\sim C35 \\sim C8 \\sim C9 \\sim C10 \\sim N1
\\sim C11 \\sim C12: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N3, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N3A, C28, C29A, C30A, C31, C32A, C33A, C34A, C35A, C36A, C37A, C38A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O5, O4A, C14A, C15A, C20A, C19A, C18A, C26A, O6A, O7A, C17, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O5, C14, O4, C15, C20, C19, C18, C26, O6, O7, C17, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(N3A)=Sof(H3A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=
 Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(O9A)=1-FVAR(1)
 Sof(O9)=Sof(N3)=Sof(H3)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=
 Sof(C38)=Sof(H38)=FVAR(1)
 Sof(H16A)=Sof(O4A)=Sof(O6A)=Sof(O7A)=Sof(C14A)=Sof(C15A)=Sof(C18A)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C26A)=1-FVAR(2)
 Sof(O4)=Sof(O6)=Sof(O7)=Sof(C14)=Sof(C15)=Sof(H16)=Sof(C18)=Sof(C19)=Sof(H19)=
 Sof(C20)=Sof(H20)=Sof(C26)=FVAR(2)
 Fixed Sof: O13(0.25) H13A(0.25) H13B(0.25) N1(0.5) C3(0.5) H3B(0.5) C4(0.5)
 C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5)
 C11(0.5) H11(0.5) C12(0.5) H12A(0.5) O14(0.5) H14A(0.5) H14B(0.5) O15(0.25)
 H15A(0.25) H15B(0.25) O16(0.25) H16B(0.25) H16C(0.25)
6.a Riding coordinates:
 O12(H12), O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16B,H16C)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N3A(H3A), C3(H3B), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12A), C16(H16), C16(H16A), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C29(H29), C29A(H29A), C32(H32), C32A(H32A), C33(H33),
 C33A(H33A), C35(H35), C35A(H35A), C36(H36), C36A(H36A), C37(H37), C37A(H37A),
 C38(H38), C38A(H38A), C19A(H19A), C20A(H20A)
;
_shelx_res_checksum              9146
_shelx_fab_checksum              63874
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'