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_7712323
_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         'C25 H31 B Fe N6 O8'
_chemical_formula_sum            'C26 H33 B Cl2 Fe N6 O8'
_chemical_formula_weight         695.14
_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             2020-08-20
_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                78.968(4)
_cell_angle_beta                 77.178(4)
_cell_angle_gamma                73.981(5)
_cell_formula_units_Z            2
_cell_length_a                   9.757(2)
_cell_length_b                   10.204(2)
_cell_length_c                   16.040(3)
_cell_measurement_reflns_used    2083
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.21
_cell_volume                     1482.2(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      120
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.1100
_diffrn_reflns_av_unetI/netI     0.1708
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20425
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.605
_diffrn_reflns_theta_min         2.097
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.4141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0717 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8391.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane -- hexane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         9051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1677
_refine_ls_R_factor_gt           0.0816
_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^)+(0.0200P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4622
_reflns_number_total             9051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00076a2.cif
_cod_data_source_block           a_sq
_cod_original_cell_volume        1482.1(5)
_cod_database_code               7712323
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.780
_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
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H3BC(0.5) H3BD(0.5) H3AA(0.5) H3AB(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) H6AA(0.5) H6AB(0.5) H6BC(0.5) H6BD(0.5) C5A(0.5)
 H5AA(0.5) H5AB(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5)
 Fixed Uiso: C4(0.03) C5(0.03) C5A(0.03) C4A(0.03)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3BC,H3BD), C3(H3AA,H3AB), 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(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C5A(H5AA,H5AB),
  C4A(H4AA,H4AB)
3.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C24(H24)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O6(H6), O8(H8)
;
_shelx_res_checksum              8941
_shelx_hkl_checksum              91828
_shelx_fab_checksum              3929
_olex2_submission_special_instructions 'No special instructions were received'