Constructing Spin Crossover-Fluorescence Bifunctional Iron(II) complexes based on Tetraphenyl Ethylene-Decorated AIEgen
Yi, Cheng; Zhang, Shi-Hui; Zhao, Liang; Yao, Nian-Tao; Zhao, Guo-Hui; Meng, Yin-Shan; Liu, Tao; Dalton Transactions  (2023) –; doi:10.1039/D2DT04130H

data_7712502
_publ_section_title
;
 Constructing Spin Crossover-Fluorescence Bifunctional Iron(II) complexes
 based on Tetraphenyl Ethylene-Decorated AIEgen
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT04130H
_journal_year                    2023
_chemical_formula_moiety         'C78 H58 Fe N10, 2.875(C H2 Cl2), 2(Cl O4)'
_chemical_formula_sum            'C80.88 H63.75 Cl7.75 Fe N10 O8'
_chemical_formula_weight         1634.25
_chemical_properties_physical    Efflorescent,Heat-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-06
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                105.490(6)
_cell_angle_beta                 101.434(6)
_cell_angle_gamma                101.383(5)
_cell_formula_units_Z            4
_cell_length_a                   14.5133(19)
_cell_length_b                   23.240(4)
_cell_length_c                   24.914(4)
_cell_measurement_reflns_used    9229
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.42
_cell_volume                     7653(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            146531
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         2.246
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       plate
_exptl_crystal_F_000             3363
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.783
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2292
_refine_ls_number_reflns         34866
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+10.3528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27945
_reflns_number_total             34866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04130h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        7654(2)
_cod_database_code               7712502
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl22-C163 = C163-Cl21
 1.7 with sigma of 0.02
 Cl20-C162 = C162-Cl19
 1.7 with sigma of 0.02
 C39-C34 = C34-C35
 1.4 with sigma of 0.02
 C35A-C34A = C34A-C39A
 1.4 with sigma of 0.02
 Cl22-Cl21
 2.8 with sigma of 0.02
 Cl20-Cl19
 2.8 with sigma of 0.02
 Cl26-C165 = C165-Cl25
 1.7 with sigma of 0.02
 Cl24-C164 = C164-Cl23
 1.7 with sigma of 0.02
3. Rigid bond restraints
 C16, C17, C18, C20, C21, C27, C29, C28, C19, C22, C24, C25, C23, C26, C34,
 C35, C36, C37, C38, C39, C33, C31, C30, C32, C15, C14, C15A, C16A, C17A, C18A,
 C20A, C21A, C26A, C25A, C24A, C23A, C22A, C27A, C28A, C33A, C32A, C31A, C30A,
 C29A, C34A, C35A, C36A, C37A, C38A, C39A, C19A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl21, Cl22, Cl19, Cl20, C163, C162
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl11, Cl14, Cl12, Cl13, C160
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl26, Cl23, Cl25, Cl24, C164, C165
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C28A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl21) \\sim Ueq, Uanis(Cl19) \\sim Ueq, Uanis(Cl20) \\sim Ueq,
Uanis(Cl22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C162) \\sim Ueq, Uanis(C163) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C164) \\sim Ueq, Uanis(C165) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Cl21, Cl22, Cl19, Cl20, C163, C162
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C20)=Sof(C21)=Sof(C27)=
 Sof(C29)=Sof(H29)=Sof(C28)=Sof(C19)=Sof(H19)=Sof(C22)=Sof(H22)=Sof(C24)=
 Sof(H24)=Sof(C25)=Sof(H25)=Sof(C23)=Sof(H23)=Sof(C26)=Sof(H26)=Sof(C34)=
 Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=
 Sof(C39)=Sof(H39)=Sof(C33)=Sof(H33)=Sof(C31)=Sof(H31)=Sof(C30)=Sof(H30)=
 Sof(C32)=Sof(H32)=Sof(C15)=Sof(H15)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=
 Sof(C20A)=Sof(C21A)=Sof(C26A)=Sof(H26A)=Sof(C25A)=Sof(H25A)=Sof(C24A)=
 Sof(H24A)=Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(H22A)=Sof(C27A)=Sof(C28A)=
 Sof(C33A)=Sof(H33A)=Sof(C32A)=Sof(H32A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=
 Sof(H30A)=Sof(C29A)=Sof(H29A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=
 Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=
 Sof(C19A)=Sof(H19A)=FVAR(1)
 Sof(Cl7)=Sof(Cl8)=Sof(C158)=Sof(H15b)=Sof(H15c)=1-FVAR(2)
 Sof(Cl6)=Sof(Cl5)=Sof(C157)=Sof(H15f)=Sof(H15g)=FVAR(2)
 Sof(Cl23)=Sof(Cl24)=Sof(C164)=Sof(H16l)=Sof(H16m)=1-FVAR(3)
 Sof(Cl26)=Sof(Cl25)=Sof(C165)=Sof(H16j)=Sof(H16k)=FVAR(3)
 Sof(Cl16)=Sof(Cl15)=Sof(H16h)=Sof(H16i)=1-FVAR(4)
 Sof(Cl18)=Sof(Cl17)=Sof(H16f)=Sof(H16g)=FVAR(4)
 Sof(Cl14)=Sof(Cl13)=Sof(H16d)=Sof(H16e)=1-FVAR(5)
 Sof(Cl11)=Sof(Cl12)=Sof(H16b)=Sof(H16c)=FVAR(5)
 Fixed Sof: Cl21(0.25) Cl22(0.25) Cl19(0.5) Cl20(0.5) C163(0.25) H16n(0.25)
 H16o(0.25) C162(0.5) H16p(0.5) H16q(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C158(H15b,H15c), C160(H16b,H16c), C160(H16d,H16e), C164(H16l,H16m), C165(H16j,
 H16k), C161(H16f,H16g), C161(H16h,H16i), C159(H15d,H15e), C163(H16n,H16o),
 C162(H16p,H16q), C157(H15f,H15g)
7.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C29(H29), C19(H19), C22(H22), C24(H24), C25(H25),
 C23(H23), C26(H26), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C33(H33),
  C31(H31), C30(H30), C32(H32), C15(H15), C49(H49), C47(H47), C43(H43),
 C44(H44), C45(H45), C40(H40), C41(H41), C42(H42), C51(H51), C52(H52), C54(H54),
  C55(H55), C57(H57), C58(H58), C65(H65), C64(H64), C63(H63), C62(H62),
 C61(H61), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75),
  C76(H76), C77(H77), C78(H78), C8(H8), C10(H10), C1(H1), C2(H2), C3(H3),
 C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C15A(H15A), C16A(H16A), C18A(H18A),
  C26A(H26A), C25A(H25A), C24A(H24A), C23A(H23A), C22A(H22A), C33A(H33A),
 C32A(H32A), C31A(H31A), C30A(H30A), C29A(H29A), C35A(H35A), C36A(H36A),
 C37A(H37A), C38A(H38A), C39A(H39A), C19A(H19A), C88(H88), C86(H86), C82(H82),
 C83(H83), C84(H84), C79(H79), C80(H80), C81(H81), C90(H90), C91(H91), C93(H93),
  C94(H94), C96(H96), C97(H97), C104(H104), C103(H103), C102(H102), C101(H101),
 C100(H100), C107(H107), C108(H108), C109(H109), C110(H110), C111(H111),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117), C125(H125),
 C127(H127), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C129(H129), C130(H130), C132(H132), C133(H133), C135(H135),
 C136(H136), C139(H139), C140(H140), C141(H141), C142(H142), C143(H143),
 C150(H150), C149(H149), C148(H148), C147(H147), C146(H146), C156(H156),
 C155(H155), C154(H154), C153(H153), C152(H152)
;
_shelx_res_checksum              44236
_shelx_hkl_checksum              83192
_olex2_submission_special_instructions 'No special instructions were received'