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_7709713
_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)'
_chemical_formula_sum            'C54.5 H43.5 B Cl6 Fe N14 O6 Zr'
_chemical_formula_weight         1361.11
_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
;
2020-06-23 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                73.63(3)
_cell_angle_beta                 87.99(3)
_cell_angle_gamma                76.02(3)
_cell_formula_units_Z            2
_cell_length_a                   13.061(3)
_cell_length_b                   13.926(3)
_cell_length_c                   17.455(4)
_cell_measurement_reflns_used    695
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      3.89
_cell_volume                     2954.1(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0732
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64452
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.735
_diffrn_reflns_theta_min         3.240
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       plate
_exptl_crystal_F_000             1379
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.736
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.0224(9)
_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   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         12733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+21.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11881
_reflns_number_total             12733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04187h2.cif
_cod_data_source_block           sd206_chcl3
_cod_original_cell_volume        2953.9(12)
_cod_original_formula_sum        'C54.50 H43.50 B Cl6 Fe N14 O6 Zr'
_cod_database_code               7709713
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.792
_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 C(H,H,H) groups
2. Others
 Fixed Sof: Cl7S(0.5) Cl8S(0.5) Cl9S(0.5) C3S(0.5) H3S(0.5)
3.a Ternary CH refined with riding coordinates:
 C1S(H1S), C3S(H3S)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
 C25(H25), C26(H26), C31(H31), C32(H32), C33(H33), C34(H34), C39(H39), C40(H40),
  C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C50(H50)
3.c X=CH2 refined with riding coordinates:
 C20(H20A,H20B)
3.d 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)
;
_shelx_res_checksum              10696
_shelx_fab_checksum              86900
_olex2_submission_special_instructions 'No special instructions were received'