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_7712325
_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         'C28 H34 B Fe N7 O7'
_chemical_formula_sum            'C28 H34 B Fe N7 O7'
_chemical_formula_weight         647.28
_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             2021-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-07 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                87.32(3)
_cell_angle_beta                 88.96(3)
_cell_angle_gamma                78.04(3)
_cell_formula_units_Z            2
_cell_length_a                   9.970(2)
_cell_length_b                   11.030(2)
_cell_length_c                   13.310(3)
_cell_measurement_reflns_used    847
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.72
_cell_volume                     1430.3(5)
_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 0.956
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rayonix CCD'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32478
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         31.013
_diffrn_reflns_theta_min         2.631
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.113
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane -- hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0496P)^2^+1.0946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6859
_reflns_number_total             7487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00076a2.cif
_cod_data_source_block           ac102
_cod_database_code               7712325
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.937
_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
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H3AA(0.66667) H3AB(0.66667) H3BC(0.33333) H3BD(0.33333)
 C4(0.66667) H4A(0.66667) H4B(0.66667) C5(0.66667) H5A(0.66667) H5B(0.66667)
 H6AA(0.66667) H6AB(0.66667) H6BC(0.33333) H6BD(0.33333) H15C(0.5) H15D(0.5)
 H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) H18D(0.5) C17A(0.5) H17C(0.5) H17D(0.5)
 C4A(0.33333) H4AA(0.33333) H4AB(0.33333) C5A(0.33333) H5AA(0.33333)
 H5AB(0.33333) C16A(0.5) H16C(0.5) H16D(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4A,H4B), C5(H5A,H5B), 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), C17(H17A,H17B), C18(H18A,H18B),
  C18(H18C,H18D), C26(H26A,H26B), C17A(H17C,H17D), C4A(H4AA,H4AB), C5A(H5AA,
 H5AB), C16A(H16C,H16D)
3.b Aromatic/amide H refined with riding coordinates:
 N7(H7), C20(H20), C21(H21), C23(H23), C24(H24)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
3.d :
 C28(H28)
;
_shelx_res_checksum              88273
_shelx_hkl_checksum              40546
_olex2_submission_special_instructions 'No special instructions were received'