Hybrid Iron(II) Phthalocyaninoclathrochelates with Terminal Reactive Vinyl Group and their Organo-Inorganic Polymeric Derivatives: Synthetic Approaches, X-ray Structures and Copolymerization with Styrene
Dudkin, Semyon V.; Chuprin, Alexander S.; Belova, Svetlana; Vologzhanina, Anna V. V.; Zubavichus, Yan V.; Kaletina, Polina M.; Shundrina, Inna; Bagryanskaya, Elena; Voloshin, Yan Z.; Dalton Transactions  (2022) –; doi:10.1039/D1DT04187H

data_7709711
_publ_section_title
;
 Hybrid Iron(II) Phthalocyaninoclathrochelates with Terminal Reactive
 Vinyl Group and their Organo-Inorganic Polymeric Derivatives: Synthetic
 Approaches, X-ray Structures and Copolymerization with Styrene
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04187H
_journal_year                    2022
_chemical_formula_moiety
'C52 H41 B Fe N14 O6 Zr, 1.5(C H Cl3), 0.5(C7 H16)'
_chemical_formula_sum            'C57 H50.5 B Cl4.5 Fe N14 O6 Zr'
_chemical_formula_weight         1345.02
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-23 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                74.184(3)
_cell_angle_beta                 85.283(3)
_cell_angle_gamma                62.992(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0551(7)
_cell_length_b                   12.7677(7)
_cell_length_c                   22.1716(13)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    120
_cell_measurement_theta_max      72.47
_cell_measurement_theta_min      4.03
_cell_volume                     2921.9(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      120
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1691
_diffrn_reflns_av_unetI/netI     0.1415
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55496
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.850
_diffrn_reflns_theta_min         2.073
_exptl_absorpt_coefficient_mu    5.875
_exptl_absorpt_correction_T_max  0.543
_exptl_absorpt_correction_T_min  0.280053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.3399 before and 0.3047 after correction.
The Ratio of minimum to maximum transmission is 0.2801.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             1372
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/heptane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.845
_refine_diff_density_min         -1.939
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         11186
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.1157
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2469
_refine_ls_wR_factor_ref         0.2572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9543
_reflns_number_total             11186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04187h2.cif
_cod_data_source_block           a
_cod_original_formula_sum        'C57 H50.50 B Cl4.50 Fe N14 O6 Zr'
_cod_database_code               7709711
_shelxl_version_number           2014-3
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2AA-C1AA = C2AA-C1AB
 1.5 with sigma of 0.02
 C1AB-C0AA
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C2S) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C3AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
Uanis(C0AA) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
4. Others
 Fixed Sof: Cl4(0.5) Cl5(0.5) Cl6(0.5) C2S(0.5) H2S(0.5) H2AA(0.5) H2AB(0.5)
 H2AC(0.5) H2AD(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C0AA(0.5)
 H0AA(0.5) H0AB(0.5) H0AC(0.5) C1AB(0.5) H1AD(0.5) H1AE(0.5)
 Fixed Uiso: C1AA(0.084) C1AB(0.08)
5.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S)
5.b Secondary CH2 refined with riding coordinates:
 C2AA(H2AA,H2AB), C2AA(H2AC,H2AD), C3AA(H3AA,H3AB), C1AB(H1AD,H1AE)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25),
 C26(H26), C31(H31), C32(H32), C33(H33), C34(H34), C39(H39), C40(H40), C41(H41),
  C42(H42), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51)
5.d X=CH2 refined with riding coordinates:
 C52(H52A,H52B)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C12(H12A,H12B,H12C), C1AA(H1AA,H1AB,H1AC), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              6851
_olex2_submission_special_instructions 'No special instructions were received'