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_7061484
_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         'C63 H50 B Fe N17 O7 Zr'
_chemical_formula_sum            'C63 H50 B Fe N17 O7 Zr'
_chemical_formula_weight         1315.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-04
_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                90
_cell_angle_beta                 103.223(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.989(3)
_cell_length_b                   12.810(2)
_cell_length_c                   29.843(6)
_cell_measurement_reflns_used    9272
_cell_measurement_temperature    295
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.19
_cell_volume                     8183(2)
_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      295
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1707
_diffrn_reflns_av_unetI/netI     0.2531
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            100915
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.689
_diffrn_reflns_theta_min         2.056
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1365 before and 0.0819 after correction.
The Ratio of minimum to maximum transmission is 0.7744.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       prism
_exptl_crystal_F_000             2696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3 : heptane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         25163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.2097
_refine_ls_R_factor_gt           0.0735
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7442
_reflns_number_total             25163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01560a2.cif
_cod_data_source_block           ac90
_cod_depositor_comments
'Adding full bibliography for 7061481--7061484.cif.'
_cod_database_code               7061484
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.969
_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, All C(H,H,H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(C5A) = Uiso(C5) = Uiso(C4) = Uiso(C4A)
Uanis(C41) = Uanis(C42)
3. 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) H9AA(0.5)
 H9AB(0.5) H9BC(0.5) H9BD(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) H12C(0.5) H12D(0.5) H12A(0.5) H12B(0.5) 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) C5A(0.5) H5AA(0.5) H5AB(0.5) C4A(0.5)
 H4AA(0.5) H4AB(0.5) C17A(0.5) H17C(0.5) H17D(0.5) C16A(0.5) H16C(0.5)
 H16D(0.5) C11A(0.5) H11C(0.5) H11D(0.5) C10A(0.5) H10C(0.5) H10D(0.5)
4.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(H9AA,H9AB), C9(H9BC,H9BD), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12C,H12D), C12(H12A,H12B), C15(H15C,H15D), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C18(H18C,H18D), C5A(H5AA,H5AB), C4A(H4AA,
 H4AB), C17A(H17C,H17D), C16A(H16C,H16D), C11A(H11C,H11D), C10A(H10C,H10D)
4.b Aromatic/amide H refined with riding coordinates:
 N8(H8), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29),
 C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C42(H42), C43(H43),
  C44(H44), C45(H45), C50(H50), C51(H51), C52(H52), C53(H53), C58(H58),
 C59(H59), C60(H60), C61(H61)
;
_shelx_res_checksum              22726
_shelx_fab_checksum              28735
_olex2_submission_special_instructions 'No special instructions were received'