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_7712326
_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         'C60 H48 B Fe N15 O7 Zr, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C61.5 H51 B Cl3 Fe N15 O7 Zr'
_chemical_formula_weight         1376.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-09
_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
_cell_angle_beta                 93.33(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.242(3)
_cell_length_b                   17.942(4)
_cell_length_c                   23.090(5)
_cell_measurement_reflns_used    2700
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.48
_cell_measurement_theta_min      2.27
_cell_volume                     5890(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      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rayonix CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  Si
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34977
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         28.526
_diffrn_reflns_theta_min         1.508
_diffrn_source                   'Belok beamline of NRC "Kurchatov Institute"'
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1913 before and 0.0983 after correction.
The Ratio of minimum to maximum transmission is 0.5940.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       prism
_exptl_crystal_F_000             2812
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane -- hexane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.957
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.00155(19)
_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   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         12892
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0535P)^2^+42.6084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9633
_reflns_number_total             12892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00076a2.cif
_cod_data_source_block           ac99
_cod_original_formula_sum        'C61.50 H51 B Cl3 Fe N15 O7 Zr'
_cod_database_code               7712326
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C61-Cl3 \\sim C61-Cl4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: Cl3(0.5) Cl4(0.5) C61(0.5) H61A(0.5) H61B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C01F(H01A,H01B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,
 H9B), C10(H10A,H10B), C11(H11A,H11B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C25(H25A,H25B), C60(H60A,H60B), C61(H61A,H61B)
5.b Aromatic/amide H refined with riding coordinates:
 N7(H7), C19(H19), C20(H20), C22(H22), C23(H23), C30(H30), C31(H31), C32(H32),
 C33(H33), C38(H38), C39(H39), C40(H40), C41(H41), C46(H46), C47(H47), C48(H48),
  C49(H49), C54(H54), C55(H55), C56(H56), C57(H57)
5.c :
 C27(H27)
;
_shelx_res_checksum              1479
_shelx_hkl_checksum              19643
_olex2_submission_special_instructions 'No special instructions were received'