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_7712499
_publ_section_title
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 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, 0.661(C H2 Cl2), 2(B F4), 2(C H4 O), 0.5[], 1[CH3OH], 1[], 1[], 0.5[]'
_chemical_formula_sum            'C81.66 H71.32 B2 Cl1.32 F8 Fe N10 O3'
_chemical_formula_weight         1517.11
_chemical_name_systematic        3-275
_chemical_properties_physical    Efflorescent
_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     iterative
_audit_creation_date             2023-02-09
_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                63.673(10)
_cell_angle_beta                 84.103(12)
_cell_angle_gamma                86.368(12)
_cell_formula_units_Z            2
_cell_length_a                   13.064(4)
_cell_length_b                   17.158(6)
_cell_length_c                   19.208(6)
_cell_measurement_reflns_used    9177
_cell_measurement_temperature    275.03
_cell_measurement_theta_max      24.791
_cell_measurement_theta_min      2.374
_cell_volume                     3838(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      275.03
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34320
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.046
_diffrn_reflns_theta_max         25.046
_diffrn_reflns_theta_min         2.374
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       prism
_exptl_crystal_F_000             1572
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         13257
_refine_ls_number_restraints     233
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0974P)^2^+2.0097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8570
_reflns_number_total             13257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04130h2.cif
_cod_data_source_block           2_sq
_cod_database_code               7712499
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H2A-F2_$1
 2.3 with sigma of 0.02
 F8-B2 \\sim B2-F7
 with sigma of 0.02
 F7-B2 \\sim B2-F5
 with sigma of 0.02
 F6A-F5A \\sim F8A-F7A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F7A)
\\sim Ueq, Uanis(F5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(F2) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F1A)
\\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 F5, F5A, F6, F6A, F7, F7A, F8, F8A, B2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F1A, F2, F2A, F3, F3A, F4, F4A, B1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=1-FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(2)
 Sof(Cl)=Sof(Cl1)=Sof(C79)=Sof(H79A)=Sof(H79B)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C54(H54), C55(H55), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C64(H64),
  C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74),
 C75(H75), C76(H76), C77(H77), C78(H78)
6.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2A)
;
_shelx_res_checksum              56838
_shelx_hkl_checksum              39642
_shelx_fab_checksum              88323
_platon_squeeze_special_details
;
A solvent mask was calculated and 39 electrons were 
found in a volume of 262\%A^3^ in 5 voids per unit cell. 
This is consistent with the presence of 
1[CH3OH] per Asymmetric Unit 
which account for 36 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'