Synthesis and spectral characterization of the first fluorescein-tagged iron(ii) clathrochelates, their supramolecular interactions with globular proteins, and cellular uptake
Selin, Roman O.; Klemt, Insa; Chernii, Viktor Ya.; Losytskyy, Mykhaylo Yu.; Chernii, Svitlana; Mular, Andrzej; Gumienna-Kontecka, Elzbieta; Kovalska, Vladyslava B.; Voloshin, Yan Z.; Vologzhanina, Anna V.; Dorovatovskii, Pavel V.; Mokhir, Andriy; RSC Advances 11 (2021) 8163–8177; doi:10.1039/D0RA10502C

data_7242299
_publ_section_title
;
 Synthesis and spectral characterization of the first fluorescein-tagged
 iron(ii) clathrochelates, their supramolecular interactions with globular
 proteins, and cellular uptake
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              8163
_journal_page_last               8177
_journal_paper_doi               10.1039/D0RA10502C
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C47 H33 B2 F2 Fe N7 O9 S2, 0.75(C7 H16)'
_chemical_formula_sum            'C52.25 H45 B2 F2 Fe N7 O9 S2'
_chemical_formula_weight         1094.54
_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
_audit_creation_date             2020-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-28 deposited with the CCDC.	2021-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                104.83(3)
_cell_angle_beta                 103.52(3)
_cell_angle_gamma                90.14(3)
_cell_formula_units_Z            4
_cell_length_a                   13.293(3)
_cell_length_b                   18.175(4)
_cell_length_c                   22.565(5)
_cell_measurement_reflns_used    847
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      1.64
_cell_volume                     5113(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Mar CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7927
_diffrn_reflns_av_unetI/netI     0.2408
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17347
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        28.400
_diffrn_reflns_theta_max         28.192
_diffrn_reflns_theta_min         1.296
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_correction_T_min  0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prism
_exptl_crystal_F_000             2262
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1325
_refine_ls_number_reflns         17347
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.2246
_refine_ls_R_factor_gt           0.0959
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+12.7928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.2272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7195
_reflns_number_total             17347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10502c1.cif
_cod_data_source_block           sr441
_cod_database_code               7242299
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.846(7)
 0.154(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 C03V-H03V
 0.98 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C93) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C94) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(C045) = Uanis(C047) = Uanis(C044) = Uanis(C042) = Uanis(C043) =
Uanis(C03Y) = Uanis(C041)
Uanis(C046) = Uanis(C03P)
5. Others
 Fixed Sof: O18A(0.5) H18A(0.5) O19(0.5) H19(0.5) C046(0.5) H04O(0.5)
 H04P(0.5) H04Q(0.5) O19A(0.5) C96(0.5) C96A(0.5) O18(0.5) H03V(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C87(H87A,H87B), C38(H38A,H38B), C03P(H03C,H03D), C03V(H03E,H03F), C03W(H03G,
 H03H), C03Y(H03A,H03B), C042(H04D,H04E), C043(H04F,H04G), C044(H04H,H04I),
 C047(H04M,H04N)
6.b Aromatic/amide H refined with riding coordinates:
 C42(H42), N7(H7), N17(H17), C41(H41), C32(H32), C44(H44), C30(H30), C67(H67),
 C84(H84), C85(H85), C66(H66), C36(H36), C82(H82), C33(H33), C18(H18), C26(H26),
  C91(H91), C61(H61), C63(H63), C45(H45), C12(H12), C76(H76), C81(H81),
 C79(H79), C65(H65), C15(H15), C8(H8), C77(H77), C14(H14), C29(H29), C21(H21),
 C95(H95), C75(H75), C60(H60), C20(H20), C64(H64), C16(H16), C78(H78), C35(H35),
  C10(H10), C17(H17A), C71(H71), C57(H57), C24(H24), C27(H27), C58(H58),
 C9(H9A), C59(H59), C22(H22), C11(H11), C92(H92), C72(H72), C69(H69), C73(H73),
 C28(H28), C23(H23), C70(H70), C94(H94)
6.c Idealised Me refined as rotating group:
 C041(H04A,H04B,H04C), C045(H04J,H04K,H04L), C046(H04O,H04P,H04Q)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O18A(H18A), O19(H19)
6.e :
 C89(H89), C40(H40)
;
_shelx_res_checksum              30322
_olex2_submission_special_instructions 'No special instructions were received'