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_7246379
_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 H41 N5 O16 Zn3'
_chemical_formula_sum            'C64 H41 N5 O16 Zn3'
_chemical_formula_weight         1332.13
_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             2022-10-24
_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                 105.392(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.752(2)
_cell_length_b                   17.8208(5)
_cell_length_c                   19.1271(8)
_cell_measurement_reflns_used    7793
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8970
_cell_measurement_theta_min      1.8490
_cell_volume                     10434.8(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 360.00   0.50    5.00   0.00   0.00   0.00    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Synchrotron source, Elettra XRD1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            132861
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.944
_diffrn_reflns_theta_min         1.727
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.013
_refine_diff_density_min         -2.574
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.0011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.467
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         21230
_refine_ls_number_restraints     620
_refine_ls_restrained_S_all      1.631
_refine_ls_R_factor_all          0.2076
_refine_ls_R_factor_gt           0.1563
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4290
_refine_ls_wR_factor_ref         0.4615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10045
_reflns_number_total             21230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00087g2.cif
_cod_data_source_block           PUM310CO
_cod_depositor_comments
'Adding full bibliography for 7246378--7246380.cif.'
_cod_original_cell_volume        10434.8(10)
_cod_database_code               7246379
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Restrained distances
 C15-O24B
 1.269 with sigma of 0.02
 C32B-C31B
 1.604 with sigma of 0.02
 C31B-C29B
 1.604 with sigma of 0.02
 C28B-C37B
 1.532 with sigma of 0.02
 C28B-C29B
 1.39 with sigma of 0.02
 C37B-C32B
 1.39 with sigma of 0.02
 C29B-C32B
 2.385 with sigma of 0.02
 C29B-C28B
 1.39 with sigma of 0.02
 C32B-C37B
 1.39 with sigma of 0.02
 C41B-C39B
 1.568 with sigma of 0.02
 C39B-N38B
 1.32 with sigma of 0.02
 N38B-C34B
 1.562 with sigma of 0.02
 C39B-O40B
 1.32 with sigma of 0.02
 C37A-C28A
 1.352 with sigma of 0.02
 C32A-C31A
 1.605 with sigma of 0.02
 C31A-C29A
 1.605 with sigma of 0.02
 C32A-O47A
 2.576 with sigma of 0.02
 O47A-C29A
 2.576 with sigma of 0.02
 O24B-C30B
 2.786 with sigma of 0.04
 O24B-C25B
 2.7869 with sigma of 0.04
 N23B-O24B
 2.298 with sigma of 0.04
 O47B-C32B
 2.614 with sigma of 0.04
 C29B-O47B
 2.614 with sigma of 0.04
 C41B-O40B
 2.416 with sigma of 0.04
 C41B-N38B
 2.293 with sigma of 0.04
 C25A-C27A \\sim C25A-C26A
 with sigma of 0.02
 C28A-C27A \\sim C28A-C26A
 with sigma of 0.02
2. Restrained planarity
 C41B, C42B, C45B, C46B, N44B, C43B, C34B, N38B, C33B, C32B, C37B, C35B, C36B,
 C31B, O47B, C29B, C30B, C25B, C15, N23B, O24B, C26B, C27B, C28B
 with sigma of 0.1
 O47B, C31B, C29B, C28B, C36B, C37B
 with sigma of 0.1
 O47B, C31B, C29B, C28B, C36B, C37B, C32B, C33B, C35B, C27B, C26B, C25B, C30B
 with sigma of 0.1
 C34B, C41B, N38B, C42B, C35B, C33B, C43B, C45B, C46B, N44B
 with sigma of 0.01
 O40B, C39B, N38B, C41B
 with sigma of 0.1
 C34A, C35A, C36A, C32A, O47A, C31A, C37A, C19A, C18A, C20A, C21A, N16B, C17A
 with sigma of 0.1
 C32A, C31A, O47A, C29A, C28A, C37A, C36A, C35A, C34A, C33A, C30A, C27A, C25A
 with sigma of 0.1
 C41A, C39A, O40A, N38A
 with sigma of 0.1
3. Rigid bond restraints
 C17A, C18A, C19A, C20A, C21A, N16B, N23B, C15, O24B, C28B, C29B, C30B, C25B,
 C26B, C27B, C33B, C32B, C37B, C36B, C35B, C34B, O47B, C31B, N38B, C41B, C42B,
 C43B, C46B, C45B, N44B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O40B, C39B, N38B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N38B, C34B, C39B, O40B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17B, C18B, C19B, C20B, C21B, N16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27B, C28B, C37B, C36B, C35B, C34B, N38B, C33B, C32B, C31B, C29B, O47B, C30B,
 C25B, C26B, N23B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43B, C42B, C41B, C45B, C46B, N44B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N38B \\sim C39B \\sim C34B \\sim O40B \\sim N44B \\sim C43B \\sim C42B \\sim
C41B \\sim C45B \\sim C46B \\sim C35B \\sim C36B \\sim C37B \\sim C32B \\sim
C33B \\sim C31B \\sim O47B \\sim C29B \\sim C28B \\sim C27B \\sim C26B \\sim
C25B \\sim C30B \\sim N23B \\sim C15 \\sim O24B \\sim C19A \\sim C18A \\sim
C20A \\sim C21A \\sim N16B \\sim C17A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
C49 \\sim C51: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
C67 \\sim C65: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
C34A \\sim C33A \\sim C32A \\sim C37A \\sim C36A \\sim C35A \\sim C28A \\sim
C29A \\sim C31A \\sim O47A \\sim C30A \\sim C27A \\sim C25A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C17B \\sim C18B \\sim C19B \\sim C20B \\sim C21B \\sim N16A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C46A \\sim C45A \\sim C42A \\sim C41A \\sim C43A \\sim N44A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C43B) \\sim Ueq, Uanis(C39B) \\sim Ueq, Uanis(N38B) \\sim Ueq,
Uanis(O40B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(N82) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(N23B) = Uanis(C15) = Uanis(O24B)
Uanis(N16B) = Uanis(N16A) = Uanis(C21A) = Uanis(C21B) = Uanis(C20B) =
Uanis(C20A) = Uanis(C19A) = Uanis(C19B) = Uanis(C17A) = Uanis(C18B) =
Uanis(C18A) = Uanis(C17B)
Uanis(C18B) = Uanis(C19B) = Uanis(C20B) = Uanis(C21B) = Uanis(N16A) =
Uanis(C17B)
Uanis(C34B) = Uanis(N38B) = Uanis(C39B)
Uanis(N44B) = Uanis(C46B) = Uanis(C45B) = Uanis(C41B) = Uanis(C42B) =
Uanis(C43B)
Uanis(O15) = Uanis(O3)
Uanis(C84) = Uanis(N82) = Uanis(C83) = Uanis(C81) = Uanis(O80)
Uanis(O48) = Uanis(C49) = Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C56) =
Uanis(C54) = Uanis(C55) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60) =
Uanis(C61) = Uanis(O62) = Uanis(O63)
Uanis(C26A) = Uanis(C25A) = Uanis(C30A) = Uanis(C29A) = Uanis(C28A) =
Uanis(C27A)
Uanis(O24B) = Uanis(O24A)
Uanis(O3) = Uanis(O15) = Uanis(O1) = Uanis(O16) = Uanis(C13) = Uanis(C11) =
Uanis(C4) = Uanis(C12) = Uanis(C2) = Uanis(C7) = Uanis(C9) = Uanis(C14) =
Uanis(C8) = Uanis(C6) = Uanis(C5) = Uanis(C10)
5. Others
 Fixed Sof: C21A(0.5) H21A(0.5) N16B(0.5) C17A(0.5) H17A(0.5) C18A(0.5)
 H18A(0.5) C19A(0.5) C20A(0.5) H20A(0.5) N23B(0.5) H23B(0.5) O24B(0.5)
 C28B(0.5) C29B(0.5) C30B(0.5) H30B(0.5) C25B(0.5) C26B(0.5) H26B(0.5)
 C27B(0.5) H27B(0.5) C33B(0.5) H33B(0.5) C32B(0.5) C37B(0.5) C36B(0.5)
 H36B(0.5) C35B(0.5) H35B(0.5) C34B(0.5) O47B(0.5) C31B(0.5) N38B(0.5)
 H38B(0.5) C41B(0.5) C42B(0.5) H42B(0.5) C43B(0.5) H43B(0.5) N44B(0.5)
 C46B(0.5) H46B(0.5) C45B(0.5) H45B(0.5) C39B(0.5) O40B(0.5) C19B(0.5)
 C20B(0.5) H20B(0.5) C21B(0.5) H21B(0.5) N16A(0.5) C17B(0.5) H17B(0.5)
 C18B(0.5) H18B(0.5) C31A(0.5) O47A(0.5) C35A(0.5) H35A(0.5) C36A(0.5)
 H36A(0.5) C37A(0.5) C32A(0.5) C33A(0.5) H33A(0.5) C34A(0.5) N38A(0.5)
 H38A(0.5) C39A(0.5) O40A(0.5) C45A(0.5) H45A(0.5) C41A(0.5) C42A(0.5)
 H42A(0.5) C43A(0.5) H43A(0.5) N44A(0.5) C46A(0.5) H46A(0.5) N23A(0.5)
 H23A(0.5) C25A(0.5) C30A(0.5) H30A(0.5) C29A(0.5) C28A(0.5) C27A(0.5)
 H27A(0.5) C26A(0.5) H26A(0.5) O24A(0.5)
6.a Free rotating group:
 C28B(C29B,C30B,C25B,C26B,C27B)
6.b Aromatic/amide H refined with riding coordinates:
 C69(H69), C74(H74), C56(H56), C73(H73), C76(H76), C60(H60), C53(H53),
 C68(H68), C72(H72), C52(H52), C57(H57), C58(H58), C21A(H21A), C17A(H17A),
 C18A(H18A), C20A(H20A), C81(H81), N23B(H23B), C30B(H30B), C26B(H26B),
 C27B(H27B), C33B(H33B), C36B(H36B), C35B(H35B), N38B(H38B), C42B(H42B),
 C43B(H43B), C46B(H46B), C45B(H45B), C20B(H20B), C21B(H21B), C17B(H17B),
 C18B(H18B), C35A(H35A), C36A(H36A), C33A(H33A), N38A(H38A), C45A(H45A),
 C42A(H42A), C43A(H43A), C46A(H46A), N23A(H23A), C30A(H30A), C27A(H27A),
 C26A(H26A), C13(H13), C11(H11), C9(H9), C6(H6), C5(H5), C10(H10)
6.c Fitted hexagon refined as free rotating group:
 C21A(N16B,C17A,C18A,C19A,C20A), C33B(C32B,C37B,C36B,C35B,C34B), C41B(C42B,
 C43B,N44B,C46B,C45B), C19B(C20B,C21B,N16A,C17B,C18B), C35A(C36A,C37A,C32A,C33A,
 C34A), C45A(C41A,C42A,C43A,N44A,C46A), C25A(C30A,C29A,C28A,C27A,C26A)
6.d Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30442
_shelx_fab_checksum              89295
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;