Multistep synthesis and X-ray structure of the carboxyl-terminated hybrid iron(II) phthalocyaninatoclathrochelates and their postsynthetic transformation into polytopic carboranyl-containing derivatives
Chuprin, Alexander S.; Pavlov, Alexander A.; Vologzhanina, Anna V. V.; Dorovatovskii, Pavel; Makarenkov, Anton V.; Ol'shevskaya, Valentina Antonovna; Dudkin, Semyon V.; Voloshin, Yan Z.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00076A

data_7712327
_publ_section_title
;
 Multistep synthesis and X-ray structure of the carboxyl-terminated hybrid
 iron(II) phthalocyaninatoclathrochelates and their postsynthetic
 transformation into polytopic carboranyl-containing derivatives
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00076A
_journal_year                    2023
_chemical_formula_moiety         'C5 D6 N, C57 H44 B Fe Hf N14 O8, 2(C5 D5 N)'
_chemical_formula_sum            'C72 H44 B D16 Fe Hf N17 O8'
_chemical_formula_weight         1552.61
_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
_audit_creation_date             2022-09-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-07 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                73.19(3)
_cell_angle_beta                 87.98(3)
_cell_angle_gamma                64.78(3)
_cell_formula_units_Z            2
_cell_length_a                   14.080(3)
_cell_length_b                   16.520(3)
_cell_length_c                   17.020(3)
_cell_measurement_reflns_used    769
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      1.85
_cell_volume                     3410.7(16)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rayonix CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33975
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         26.660
_diffrn_reflns_theta_min         1.668
_diffrn_source                   'Belok beamline of NRC "Kurchatov Institute"'
_exptl_absorpt_coefficient_mu    2.018
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       plate
_exptl_crystal_F_000             1556
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pyridine-d5'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.695
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         12067
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0380P)^2^+12.7083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9536
_reflns_number_total             12067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00076a2.cif
_cod_data_source_block           ac70
_cod_original_cell_volume        3410.8(15)
_cod_database_code               7712327
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.906
_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, All N(H) groups
2. Uiso/Uaniso restraints and constraints
N1S \\sim C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
3. Others
 Fixed Sof: H3AA(0.75) H3AB(0.75) H3BC(0.25) H3BD(0.25) C4(0.75) H4A(0.75)
 H4B(0.75) C4A(0.25) H4AA(0.25) H4AB(0.25) C5(0.75) H5A(0.75) H5B(0.75)
 C5A(0.25) H5AA(0.25) H5AB(0.25) H6AA(0.75) H6AB(0.75) H6BC(0.25) H6BD(0.25)
 H15C(0.5) H15D(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C16A(0.5)
 H16C(0.5) H16D(0.5) C17(0.5) H17A(0.5) H17B(0.5) C17A(0.5) H17C(0.5) H17D(0.5)
 H18C(0.5) H18D(0.5) H18A(0.5) H18B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4A,H4B), C4A(H4AA,H4AB), C5(H5A,H5B),
 C5A(H5AA,H5AB), C6(H6AA,H6AB), C6(H6BC,H6BD), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C12(H12A,H12B), C15(H15C,H15D), C15(H15A,H15B), C16(H16A,H16B),
  C16A(H16C,H16D), C17(H17A,H17B), C17A(H17C,H17D), C18(H18C,H18D), C18(H18A,
 H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30), C31(H31),
 C32(H32), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45), C46(H46), C47(H47),
  C48(H48), C52(H52), C53(H53), C55(H55), C56(H56), N1S(D1S), C1S(D1SA),
 C2S(D2S), C3S(D3S), C4S(D4S), C5S(D5S), C6S(D6S), C7S(D7S), C8S(D8S), C9S(D9S),
  C10S(D10S), C11S(D11S), C12S(D12S), C13S(D13S), C14S(D14S), C15S(D15S)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29730
_shelx_hkl_checksum              72735
_shelx_fab_checksum              90113
_olex2_submission_special_instructions 'No special instructions were received'