Luminescence properties of mixed-ligand MOFs containing fluorene scaffolds functionalized with isonicotinoyl arms
Delledonne, Andrea; Orlandini, Martina; Terenziani, Francesca; Mazzeo, Paolo Pio; Bacchi, Alessia; Carlucci, Lucia; Comotti, Angiolina; Perego, Jacopo; Pelagatti, Paolo; CrystEngComm 25 (2023) 2085–2095; doi:10.1039/D3CE00087G

data_7246380
_publ_section_title
;
 Luminescence properties of mixed-ligand MOFs containing fluorene
 scaffolds functionalized with isonicotinoyl arms
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2085
_journal_page_last               2095
_journal_paper_doi               10.1039/D3CE00087G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C64 H43 N5 O15 Zn3, 0.5(C3 H7 N O)'
_chemical_formula_sum            'C65.5 H46.5 N5.5 O15.5 Zn3'
_chemical_formula_weight         1354.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-24 deposited with the CCDC.	2023-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.08(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.28(6)
_cell_length_b                   17.76(3)
_cell_length_c                   19.21(3)
_cell_measurement_reflns_used    461452
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.893
_cell_measurement_theta_min      2.186
_cell_volume                     10682(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'abstract diffractometer'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.1433
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            461452
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.893
_diffrn_reflns_theta_min         2.186
_exptl_absorpt_coefficient_mu    0.710
_exptl_crystal_density_diffrn    0.842
_exptl_crystal_description       prism
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.238
_refine_diff_density_min         -1.769
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         30230
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1675
_refine_ls_R_factor_gt           0.1013
_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^)+(0.1725P)^2^+36.3370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2967
_refine_ls_wR_factor_ref         0.3684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13635
_reflns_number_total             30230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00087g2.cif
_cod_data_source_block           PUM310
_cod_depositor_comments
'Adding full bibliography for 7246378--7246380.cif.'
_cod_original_cell_volume        10685(31)
_cod_original_formula_sum        'C65.50 H46.50 N5.50 O15.50 Zn3'
_cod_database_code               7246380
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-C40
 1.55 with sigma of 0.02
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C26-C27 \\sim C26A-C27A
 with sigma of 0.02
 C26-C31 \\sim C26A-C31A
 with sigma of 0.02
 C29-C33 \\sim C29A-C33A
 with sigma of 0.04
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 N25-C26 \\sim N25-C26A
 with sigma of 0.02
 C28-H28 \\sim C28A-H28A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C32-C30 \\sim C32A-C30A
 with sigma of 0.02
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C29-C34 \\sim C29A-C34A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 C30-C33 \\sim C30A-C33A
 with sigma of 0.04
 C31-H31 \\sim C31A-H31A
 with sigma of 0.02
 C32-H32B \\sim C32A-H32D
 with sigma of 0.02
 C37-C33 \\sim C37A-C33A
 with sigma of 0.04
 C38-C36 \\sim C38A-C36A
 with sigma of 0.04
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 C37-C36 \\sim C37A-C36A
 with sigma of 0.02
 C33-C35 \\sim C33A-C35A
 with sigma of 0.04
 C34-C36 \\sim C34A-C36A
 with sigma of 0.04
 N39-C37 \\sim N39-C37A
 with sigma of 0.02
 C32-H32A \\sim C32A-H32C
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.02
 C38-C33 \\sim C38A-C33A
 with sigma of 0.02
 C27-H28 \\sim C27A-H28A
 with sigma of 0.04
 C27-C31 \\sim C27A-C31A
 with sigma of 0.04
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 C28-C34 \\sim C28A-C34A
 with sigma of 0.04
 C34-C35 \\sim C34A-C35A
 with sigma of 0.02
 C35-H35 \\sim C35A-H35A
 with sigma of 0.02
 H28-C29 \\sim H28A-C29A
 with sigma of 0.04
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C29-C31 \\sim C29A-C31A
 with sigma of 0.04
 C29-C35 \\sim C29A-C35A
 with sigma of 0.04
 N25-C27 \\sim N25-C27A
 with sigma of 0.04
 C30-H31 \\sim C30A-H31A
 with sigma of 0.04
 N25-C31 \\sim N25-C31A
 with sigma of 0.04
 C30-C34 \\sim C30A-C34A
 with sigma of 0.04
 N39-C38 \\sim N39-C38A
 with sigma of 0.04
 N39-C36 \\sim N39-C36A
 with sigma of 0.04
 C32-C29 \\sim C32A-C29A
 with sigma of 0.04
 C32-C31 \\sim C32A-C31A
 with sigma of 0.04
 C32-C38 \\sim C32A-C38A
 with sigma of 0.04
 C32-C34 \\sim C32A-C34A
 with sigma of 0.04
 C37-H38 \\sim C37A-H38A
 with sigma of 0.04
 C37-C35 \\sim C37A-C35A
 with sigma of 0.04
 C38-C34 \\sim C38A-C34A
 with sigma of 0.04
 H32A-H32B \\sim H32C-H32D
 with sigma of 0.04
 H32A-C30 \\sim H32C-C30A
 with sigma of 0.04
 H32A-C33 \\sim H32C-C33A
 with sigma of 0.04
 H38-C33 \\sim H38A-C33A
 with sigma of 0.04
 H32B-C30 \\sim H32D-C30A
 with sigma of 0.04
 C34-H35 \\sim C34A-H35A
 with sigma of 0.04
 H32B-C33 \\sim H32D-C33A
 with sigma of 0.04
 H35-C36 \\sim H35A-C36A
 with sigma of 0.04
 C26-C28 \\sim C26A-C28A
 with sigma of 0.04
 C26-C30 \\sim C26A-C30A
 with sigma of 0.04
 C38-H38 \\sim C38A-H38A
 with sigma of 0.02
 C26-H31 \\sim C26A-H31A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C27) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C28)
Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C31) = Uanis(C30) = Uanis(C29) =
Uanis(C34) = Uanis(C33) = Uanis(C32) = Uanis(C35) = Uanis(C36) = Uanis(C37) =
Uanis(C38)
Uanis(O1G) = Uanis(N3G) = Uanis(C2G)
Uanis(N45) = Uanis(C44) = Uanis(C43) = Uanis(C42) = Uanis(C47) = Uanis(C46)
Uanis(O1G) = Uanis(C2G) = Uanis(N3G) = Uanis(C4G) = Uanis(C5G)
Uanis(O41) = Uanis(C40) = Uanis(N39) = Uanis(N25) = Uanis(C23) = Uanis(O24)
Uanis(C32) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) =
Uanis(C31) = Uanis(C37) = Uanis(C38) = Uanis(C33) = Uanis(C34) = Uanis(C35) =
Uanis(C36) = Uanis(C32A) = Uanis(C26A) = Uanis(C27A) = Uanis(C28A) =
Uanis(C29A) = Uanis(C30A) = Uanis(C31A) = Uanis(C37A) = Uanis(C38A) =
Uanis(C33A) = Uanis(C34A) = Uanis(C35A) = Uanis(C36A) = Uanis(N17) = Uanis(N45)
= Uanis(C46) = Uanis(C47) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(O24) =
Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C18) = Uanis(C23) = Uanis(C19) =
Uanis(N25) = Uanis(O41) = Uanis(N39) = Uanis(C40)
Uanis(N17) = Uanis(N45) = Uanis(C46) = Uanis(C47) = Uanis(C42) = Uanis(C43) =
Uanis(C44) = Uanis(O24) = Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C18) =
Uanis(C23) = Uanis(C19) = Uanis(N25) = Uanis(O41) = Uanis(N39) = Uanis(C40) =
Uanis(C32) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) =
Uanis(C31) = Uanis(C37) = Uanis(C38) = Uanis(C33) = Uanis(C34) = Uanis(C35) =
Uanis(C36) = Uanis(C32A) = Uanis(C26A) = Uanis(C27A) = Uanis(C28A) =
Uanis(C29A) = Uanis(C30A) = Uanis(C31A) = Uanis(C37A) = Uanis(C38A) =
Uanis(C33A) = Uanis(C34A) = Uanis(C35A) = Uanis(C36A)
4. Others
 Sof(H25A)=Sof(H39A)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C26A)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=
 Sof(C37A)=Sof(C38A)=Sof(H38A)=Sof(C33A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(H25)=Sof(H39)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C26)=Sof(C27)=Sof(H27)=
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(H31)=Sof(C37)=Sof(C38)=
 Sof(H38)=Sof(C33)=Sof(C34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=FVAR(1)
 Fixed Sof: N3G(0.5) C4G(0.5) H4GA(0.5) H4GB(0.5) H4GC(0.5) O1G(0.5) C2G(0.5)
 H2G(0.5) C5G(0.5) H5GA(0.5) H5GB(0.5) H5GC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C32A(H32C,H32D)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C21(H21), C22(H22), C13(H13), C68(H68), C46(H46),
 C47(H47), C43(H43), C44(H44), C56(H56), C11(H11), C5(H5), C10(H10), C57(H57),
 C74(H74), C8(H8), C9(H9), C60(H60), C76(H76), C58(H58), C73(H73), C82(H82),
 C52(H52), C72(H72), C53(H53), C71(H71), N25(H25), N25(H25A), N39(H39),
 N39(H39A), C27(H27), C28(H28), C31(H31), C38(H38), C35(H35), C36(H36),
 C2G(H2G), C27A(H27A), C28A(H28A), C31A(H31A), C38A(H38A), C35A(H35A),
 C36A(H36A)
5.c Fitted hexagon refined as free rotating group:
 N17(C18,C19,C20,C21,C22), N45(C46,C47,C42,C43,C44), C26(C27,C28,C29,C30,C31),
 C37(C38,C33,C34,C35,C36), C26A(C27A,C28A,C29A,C30A,C31A), C37A(C38A,C33A,C34A,
 C35A,C36A)
5.d Idealised Me refined as rotating group:
 C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C4G(H4GA,H4GB,H4GC), C5G(H5GA,H5GB,
 H5GC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42981
_shelx_fab_checksum              31297
_olex2_submission_special_instructions 'No special instructions were received'