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_7709712
_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         'C58 H47 B Fe N14 O6 Zr, 2.13(C H Cl3)'
_chemical_formula_sum            'C60.12 H49.12 B Cl6.38 Fe N14 O6 Zr'
_chemical_formula_weight         1447.63
_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             2020-06-16
_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                101.30(3)
_cell_angle_beta                 104.72(3)
_cell_angle_gamma                96.60(3)
_cell_formula_units_Z            2
_cell_length_a                   12.875(3)
_cell_length_b                   14.749(3)
_cell_length_c                   19.981(4)
_cell_measurement_reflns_used    841
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      3.58
_cell_volume                     3543.9(15)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Mar CCD'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80246
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            58183
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.879
_diffrn_reflns_theta_min         3.212
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       needle
_exptl_crystal_F_000             1470
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/heptane'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.467
_refine_diff_density_min         -1.813
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0105(7)
_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   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         15466
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+37.3704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2070
_refine_ls_wR_factor_ref         0.2109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13642
_reflns_number_total             15466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04187h2.cif
_cod_data_source_block           sd204
_cod_original_cell_volume        3543.8(14)
_cod_database_code               7709712
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.730
_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
 Cl6S-C2S = Cl5S-C2S = Cl4S-C2S
 1.78 with sigma of 0.005
 Cl14-C5S = Cl13-C5S = Cl15-C5S
 1.7 with sigma of 0.02
 Cl13-Cl14 = Cl14-Cl15 = Cl15-Cl13
 2.9 with sigma of 0.02
 Cl4S-Cl6S
 2.9 with sigma of 0.004
 Cl6S-Cl5S
 2.9 with sigma of 0.004
 Cl5S-Cl4S
 2.9 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
Uanis(Cl0A) \\sim Ueq, Uanis(Cl2S) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Cl12) \\sim Ueq, Uanis(Cl1S) \\sim Ueq, Uanis(Cl10) \\sim Ueq, Uanis(C4S)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl6S) = Uanis(Cl5S) = Uanis(C2S) = Uanis(Cl4S)
Uanis(C5S) = Uanis(Cl15) = Uanis(Cl14) = Uanis(Cl13)
Uanis(C5S) = Uanis(Cl13) = Uanis(Cl14) = Uanis(Cl15)
Uanis(Cl13) = Uanis(C5S) = Uanis(Cl14) = Uanis(Cl15)
4. Others
 Sof(H3BC)=Sof(H3BD)=Sof(H6BC)=Sof(H6BD)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(H6AA)=Sof(H6AB)=FVAR(1)
 Fixed Sof: C4A(0.5) H4AA(0.5) H4AB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) Cl0A(0.5) Cl2S(0.5) Cl3S(0.5)
 C1S(0.5) H1S(0.5) Cl1S(0.25) Cl10(0.25) Cl12(0.25) C4S(0.25) H4S(0.25)
 Cl4S(0.25) Cl5S(0.25) Cl6S(0.25) C2S(0.25) H2S(0.25) Cl13(0.125) Cl14(0.125)
 Cl15(0.125) C5S(0.125) H5S(0.125)
5.a Ternary CH refined with riding coordinates:
 C1S(H1S), C4S(H4S), C2S(H2S), C3S(H3S), C5S(H5S)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3BC,H3BD), C3(H3AA,H3AB), C6(H6BC,H6BD), C6(H6AA,H6AB), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C4(H4A,H4B),
 C5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), 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)
5.d X=CH2 refined with riding coordinates:
 C26(H26A,H26B)
;
_shelx_res_checksum              91698
_olex2_submission_special_instructions 'No special instructions were received'