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_7712324
_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         'C57 H45 B Fe N14 O8 Zr, 2.5(C6 H6)'
_chemical_formula_sum            'C72 H60 B Fe N14 O8 Zr'
_chemical_formula_weight         1407.22
_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                90.70(3)
_cell_angle_beta                 93.99(3)
_cell_angle_gamma                106.72(3)
_cell_formula_units_Z            2
_cell_length_a                   12.236(3)
_cell_length_b                   12.862(3)
_cell_length_c                   23.178(5)
_cell_measurement_reflns_used    942
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.092
_cell_measurement_theta_min      1.846
_cell_volume                     3483.1(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52706
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         31.012
_diffrn_reflns_theta_min         1.734
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.093
_exptl_absorpt_correction_T_min  0.041
_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    1.342
_exptl_crystal_description       plate
_exptl_crystal_F_000             1450
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene -- iso-octane'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0046(3)
_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   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         19204
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0400P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13159
_reflns_number_total             19204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00076a2.cif
_cod_data_source_block           ac68
_cod_original_cell_volume        3483.1(13)
_cod_database_code               7712324
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.945
_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 O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C16S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Rigid body (RIGU) restrains
 C18S, C13S, C17S, C16S, C14S, C15S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C14S(0.5) H14S(0.5) C15S(0.5) H15S(0.5) C18S(0.5) H18S(0.5)
 C13S(0.5) H13S(0.5) C17S(0.5) H17S(0.5) C16S(0.5) H16S(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B), C12(H12A,H12B), C15(H15A,H15B), C3(H3A,H3B),
 C16(H16A,H16B), C11(H11A,H11B), C10(H10A,H10B), C18(H18A,H18B), C4(H4A,H4B),
 C17(H17A,H17B), C5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C5S(H5S), C22(H22), C45(H45), C32(H32), C12S(H12S), C47(H47),
 C21(H21), C2S(H2S), C56(H56), C10S(H10S), C38(H38), C55(H55), C48(H48),
 C40(H40), C52(H52), C37(H37), C1S(H1S), C24(H24), C7S(H7S), C29(H29), C39(H39),
  C8S(H8S), C30(H30), C9S(H9S), C53(H53), C46(H46), C31(H31), C11S(H11S),
 C3S(H3S), C6S(H6S), C4S(H4S), C14S(H14S), C15S(H15S), C18S(H18S), C13S(H13S),
 C17S(H17S), C16S(H16S)
5.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              14958
_shelx_hkl_checksum              49921
_shelx_fab_checksum              63439
_olex2_submission_special_instructions 'No special instructions were received'