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_7246378
_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         'C132 H93 N10 O30 Zn6, 3(C3 H7 N O)'
_chemical_formula_sum            'C141 H114 N13 O33 Zn6'
_chemical_formula_weight         2910.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                104.948(3)
_cell_angle_beta                 103.585(3)
_cell_angle_gamma                90.131(3)
_cell_formula_units_Z            2
_cell_length_a                   17.6312(7)
_cell_length_b                   19.4232(4)
_cell_length_c                   31.8390(12)
_cell_measurement_reflns_used    65457
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.944
_cell_measurement_theta_min      1.554
_cell_volume                     10216.7(6)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Synchrotron ELETTRA XRD1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            65422
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.944
_diffrn_reflns_theta_min         1.554
_exptl_absorpt_coefficient_mu    0.719
_exptl_crystal_density_diffrn    0.946
_exptl_crystal_description       plate
_exptl_crystal_F_000             2990
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.092
_refine_diff_density_min         -2.137
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       0.0038(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   1.512
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         38133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.512
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.1422
_refine_ls_shift/su_max          0.009
_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          0.4017
_refine_ls_wR_factor_ref         0.4218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24457
_reflns_number_total             38133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00087g2.cif
_cod_data_source_block           pum310me2
_cod_depositor_comments
'Adding full bibliography for 7246378--7246380.cif.'
_cod_database_code               7246378
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Zn3) = Uanis(Zn6) = Uanis(Zn5)
Uanis(O172) = Uanis(C173) = Uanis(N174)
Uanis(O134) = Uanis(C132) = Uanis(O133) = Uanis(C130) = Uanis(C131) =
Uanis(C129) = Uanis(C128) = Uanis(C126) = Uanis(C125) = Uanis(C124) =
Uanis(C123) = Uanis(C122) = Uanis(C127) = Uanis(C120) = Uanis(O121) =
Uanis(O119)
Uanis(C95) = Uanis(C109) = Uanis(C108) = Uanis(C107) = Uanis(C97) = Uanis(C96)
= Uanis(C98) = Uanis(C101) = Uanis(C102) = Uanis(C103) = Uanis(C104) =
Uanis(C105) = Uanis(C106)
Uanis(C59) = Uanis(C58) = Uanis(C57) = Uanis(C56) = Uanis(C55) = Uanis(C60) =
Uanis(C52) = Uanis(C50) = Uanis(C49) = Uanis(C48) = Uanis(C47) = Uanis(C46) =
Uanis(C51)
Uanis(O36) = Uanis(C33) = Uanis(O34) = Uanis(C30) = Uanis(C31) = Uanis(C32) =
Uanis(C27) = Uanis(C28) = Uanis(C23) = Uanis(C21) = Uanis(O20) = Uanis(O22) =
Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C29)
Uanis(O151) = Uanis(C152) = Uanis(N153)
Uanis(O3) = Uanis(C2) = Uanis(O1)
Uanis(C146) = Uanis(C145) = Uanis(C147) = Uanis(C141) = Uanis(C142) =
Uanis(C144)
Uanis(O150) = Uanis(C148) = Uanis(O18) = Uanis(O149)
Uanis(C7) = Uanis(C6) = Uanis(C13) = Uanis(C5) = Uanis(C8) = Uanis(C4) =
Uanis(C9) = Uanis(C10) = Uanis(C12) = Uanis(C11)
Uanis(C114) = Uanis(N116) = Uanis(C115) = Uanis(C117) = Uanis(C113) =
Uanis(C118)
Uanis(N86) = Uanis(C87) = Uanis(C91) = Uanis(C90) = Uanis(C88) = Uanis(C89)
Uanis(N37) = Uanis(C42) = Uanis(C39) = Uanis(C41) = Uanis(C38) = Uanis(C40)
Uanis(C161) = Uanis(C165) = Uanis(C166) = Uanis(C160) = Uanis(C162) =
Uanis(C159) = Uanis(C167) = Uanis(C164) = Uanis(C168) = Uanis(C163)
Uanis(N67) = Uanis(C64) = Uanis(C66) = Uanis(C69) = Uanis(C68) = Uanis(C65)
Uanis(C77) = Uanis(C78) = Uanis(C76) = Uanis(C73) = Uanis(C79) = Uanis(C75) =
Uanis(C74) = Uanis(C81) = Uanis(C82) = Uanis(C80)
3.a Aromatic/amide H refined with riding coordinates:
 C77(H77), C78(H78), C123(H123), C25(H25), C147(H147), C165(H165), C13(H13),
 C152(H152), C29(H29), C28(H28), C139(H139), C131(H131), C24(H24), C42(H42),
 C166(H166), C5(H5), C39(H39), C32(H32), C160(H160), C8(H8), C31(H31), C41(H41),
  C140(H140), C79(H79), C9(H9), C173(H173), C10(H10), C124(H124), C38(H38),
 C74(H74), C145(H145), C164(H164), C129(H129), C168(H168), C11(H11), C144(H144),
  C114(H114), C81(H81), C143(H143), C82(H82), C115(H115), C163(H163),
 C03R(H03R), C117(H117), N45(H45), C66(H66), C69(H69), N110(H110), N61(H61),
 C7G(H7G), C68(H68), C60(H60), C2G(H2G), C102(H102), C48(H48), C51(H51),
 C91(H91), C118(H118), C90(H90), C96(H96), N94(H94), C105(H105), C57(H57),
 C104(H104), C88(H88), C65(H65), C47(H47), C108(H108), C109(H109), C58(H58)
3.b Idealised Me refined as rotating group:
 C155(H15A,H15B,H15C), C154(H15D,H15E,H15F), C176(H17A,H17B,H17C), C175(H17D,
 H17E,H17F), C5G(H5GA,H5GB,H5GC), C10G(H10D,H10E,H10F), C9G(H9GA,H9GB,H9GC),
 C14G(H14A,H14B,H14C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C4G(H4GA,H4GB,
 H4GC), C100(H10A,H10B,H10C), C13G(H13A,H13B,H13C), C99(H99A,H99B,H99C)
;
_shelx_res_checksum              92097
_shelx_fab_checksum              54502
_olex2_submission_special_instructions 'No special instructions were received'