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_7705435
_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 H75.89 Gd6 N10 O42), 1.5(H2 O)'
_chemical_formula_sum            'C65 H40.85 Gd3 N5 O22.5'
_chemical_formula_weight         1723.63
_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             2020-06-17
_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                 102.164(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.513(3)
_cell_length_b                   27.717(6)
_cell_length_c                   11.592(3)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.27
_cell_volume                     3616.0(15)
_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 0.999
_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  0.0645
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            70947
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.797
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.793
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         8437
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0474P)^2^+15.2618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7061
_reflns_number_total             8437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02736g16.cif
_cod_data_source_block           an1gd_sq
_cod_depositor_comments
'Adding full bibliography for 7705434--7705437.cif.'
_cod_original_cell_volume        3616.0(14)
_cod_original_formula_sum        'C65 H40.85 Gd3 N5 O22.50'
_cod_database_code               7705435
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.663
_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
 C18-C17 \\sim C18A-C17
 with sigma of 0.02
 C19A-C18A \\sim C19-C18
 with sigma of 0.02
 C20-C19 \\sim C20A-C19A
 with sigma of 0.02
 C20A-C15A \\sim C20-C15
 with sigma of 0.02
 C16-C15 \\sim C16-C15A
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A
 with sigma of 0.02
 O5-C14A \\sim O5-C14
 with sigma of 0.02
 O4A-C14A \\sim O4-C14
 with sigma of 0.02
 O6-C26 \\sim O6A-C26A
 with sigma of 0.02
 C26-C18 \\sim C26A-C18A
 with sigma of 0.02
 O19-C27 \\sim O9-C27
 with sigma of 0.02
 Gd2-O19 \\sim Gd2-O9
 with sigma of 0.02
3. Restrained planarity
 C14A, C15A, C16, C17, C19A, C20A, C18A, C26A
 with sigma of 0.1
 O6A, O7A, C18A, C26A
 with sigma of 0.1
 O4A, O5, C14A, C15A
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 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
 O4, O5, O6, O7, C14, C15, C16, C18, C19, C20, C26, C17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O4A, O5, O6A, O7A, C14A, C15A, C16, C17, C18A, C19A, C20A, C26A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O8, O9, O10, O11, N3, C00D, C27, 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
 O8, O9, O10, O11, N7, C00D, C27, 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
5. Others
 Sof(N7)=Sof(H7)=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(O19)=1-FVAR(1)
 Sof(O9)=Sof(N3)=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(O4A)=Sof(O6A)=Sof(O7A)=Sof(C14A)=Sof(C15A)=Sof(H16A)=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: C3(0.5) H3(0.5) C4(0.5) C6(0.5) H6(0.5) C7(0.5) H7A(0.5) C8(0.5)
 C9(0.5) H9(0.5) C10(0.5) H10(0.5) N1(0.5) C11(0.5) H11(0.5) C12(0.5) H12A(0.5)
 O13(0.5) H13A(0.5) H13B(0.5) O14(0.25) H14A(0.25) H14B(0.25)
6.a Riding coordinates:
 O12(H12), O13(H13A,H13B), O14(H14A,H14B)
6.b Aromatic/amide H refined with riding coordinates:
 N7(H7), C3(H3), C6(H6), C7(H7A), C9(H9), C10(H10), C11(H11), C12(H12A),
 C16(H16), C16(H16A), C19(H19), C19A(H19A), C20(H20), C20A(H20A), 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)
6.c Fitted hexagon refined as free rotating group:
 C8(C9,C10,N1,C11,C12)
;
_shelx_res_checksum              62423
_shelx_fab_checksum              34763
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'