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_7061481
_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         'C25 H32 B Fe N6 O7'
_chemical_formula_sum            'C25 H32 B Fe N6 O7'
_chemical_formula_weight         595.22
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-13
_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                 109.458(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5430(6)
_cell_length_b                   18.7340(14)
_cell_length_c                   13.9340(9)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    295
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.99
_cell_volume                     2595.0(3)
_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 0.970
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON detector'
_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  0.1225
_diffrn_reflns_av_unetI/netI     0.1109
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36905
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.579
_diffrn_reflns_theta_min         2.174
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.1611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1697 before and 0.0997 after correction.
The Ratio of minimum to maximum transmission is 0.2159.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2 : hexane'
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3281
_reflns_number_total             6410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01560a2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7061481--7061484.cif.'
_cod_database_code               7061481
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.728
_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(C11) = Uanis(C10)
Uanis(O7) = Uanis(C25)
3.a Riding coordinates:
 O2(H2), O4(H4), O6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              17958
_olex2_submission_special_instructions 'No special instructions were received'