Synthesis and reactivity of the apically functionalized (pseudo)macrobicyclic iron(ii) tris-dioximates and their hybrid phthalocyaninatoclathrochelate derivatives comprising reactive and vector terminal groups
Chuprin, Alexander S.; Dudkin, Semyon V.; Belova, Svetlana A.; Lebed, Ekaterina G.; Dorovatovskii, Pavel V.; Vologzhanina, Anna V.; Voloshin, Yan Z.; New Journal of Chemistry 46 (2022) 10863–10877; doi:10.1039/D2NJ01560A

data_7061482
_publ_section_title
;
 Synthesis and reactivity of the apically functionalized
 (pseudo)macrobicyclic iron(ii) tris-dioximates and their hybrid
 phthalocyaninatoclathrochelate derivatives comprising reactive and vector
 terminal groups
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10863
_journal_page_last               10877
_journal_paper_doi               10.1039/D2NJ01560A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C57 H45 B Fe N14 O7 Zr, 3.5(C H Cl3)'
_chemical_formula_sum            'C60.5 H48.5 B Cl10.5 Fe N14 O7 Zr'
_chemical_formula_weight         1613.74
_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             2020-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-28 deposited with the CCDC.	2022-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                111.16(3)
_cell_angle_beta                 94.87(3)
_cell_angle_gamma                92.81(3)
_cell_formula_units_Z            2
_cell_length_a                   13.398(3)
_cell_length_b                   15.250(3)
_cell_length_c                   17.404(4)
_cell_measurement_reflns_used    846
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      4.01
_cell_volume                     3292.1(14)
_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 0.989
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Mar CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80246
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45507
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.865
_diffrn_reflns_theta_min         3.222
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       plate
_exptl_crystal_F_000             1630
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3 : heptane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.266
_refine_diff_density_min         -1.818
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0163(6)
_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   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         14133
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0810
_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^)+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11559
_reflns_number_total             14133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01560a2.cif
_cod_data_source_block           sd207_chcl3
_cod_depositor_comments
'Adding full bibliography for 7061481--7061484.cif.'
_cod_original_cell_volume        3292.2(13)
_cod_original_formula_sum        'C60.50 H48.50 B Cl10.50 Fe N14 O7 Zr'
_cod_database_code               7061482
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.781
_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
2. Restrained distances
 Cl1A-C0AA = Cl5A-C0AA = Cl10-C0AA
 1.78 with sigma of 0.005
 C10-C11
 1.5 with sigma of 0.02
 Cl1A-Cl10
 2.9 with sigma of 0.005
 Cl10-Cl5A
 2.9 with sigma of 0.005
 Cl5A-Cl1A
 2.9 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(C0) = Uiso(C11)
Uiso(C10) = Uiso(C5AA)
Uanis(O7B) = Uanis(O7A)
4. Others
 Fixed Sof: H3AA(0.5) H3AB(0.5) H3BC(0.5) H3BD(0.5) H6AA(0.5) H6AB(0.5)
 H6BC(0.5) H6BD(0.5) H9AA(0.5) H9AB(0.5) H9BC(0.5) H9BD(0.5) H12A(0.5)
 H12B(0.5) H12C(0.5) H12D(0.5) H25(0.75) H25A(0.25) C0(0.5) H0A(0.5) H0B(0.5)
 C2AA(0.5) H2AA(0.5) H2AB(0.5) C3AA(0.5) H3AC(0.5) H3AD(0.5) C5AA(0.5)
 H5AA(0.5) H5AB(0.5) O7A(0.75) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5) Cl1(0.25)
 Cl11(0.25) Cl12(0.25) C4S(0.25) H4S(0.25) Cl1A(0.25) Cl5A(0.25) Cl10(0.25)
 C0AA(0.25) H0AA(0.25) O7B(0.25)
5.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C0AA(H0AA)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C6(H6AA,H6AB), C6(H6BC,H6BD), C9(H9AA,H9AB),
 C9(H9BC,H9BD), C12(H12A,H12B), C12(H12C,H12D), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), C0(H0A,H0B), C2AA(H2AA,H2AB), C3AA(H3AC,H3AD),
 C5AA(H5AA,H5AB), C4(H4A,H4B), C5(H5A,H5B), C10(H10A,H10B), C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C25(H25A), C29(H29),
 C30(H30), C31(H31), C32(H32), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45),
  C46(H46), C47(H47), C48(H48), C53(H53), C54(H54), C55(H55), C56(H56)
;
_shelx_res_checksum              84852
_olex2_submission_special_instructions 'No special instructions were received'