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_7709710
_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, C6 H6, C8 H18'
_chemical_formula_sum            'C66 H65 B Fe N14 O6 Zr'
_chemical_formula_weight         1308.20
_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                92.23(3)
_cell_angle_beta                 97.04(3)
_cell_angle_gamma                94.21(3)
_cell_formula_units_Z            2
_cell_length_a                   12.904(3)
_cell_length_b                   13.289(3)
_cell_length_c                   17.715(4)
_cell_measurement_reflns_used    891
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      3.12
_cell_volume                     3003.2(12)
_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 0.967
_diffrn_measured_fraction_theta_max 0.958
_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  0.1055
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54921
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.903
_diffrn_reflns_theta_min         2.619
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       prism
_exptl_crystal_F_000             1356
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/isooctane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.503
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0235(14)
_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   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         12626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+6.2147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10651
_reflns_number_total             12626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04187h2.cif
_cod_data_source_block           sd206a
_cod_original_cell_volume        3003.4(11)
_cod_database_code               7709710
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.900
_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: H10S(0.75) H10A(0.25) C9S(0.75) H9SA(0.75) H9SB(0.75) C11S(0.75)
 H11A(0.75) H11B(0.75) H11C(0.75) C13S(0.75) H13A(0.75) H13B(0.75) H13C(0.75)
 C9T(0.25) H9TA(0.25) H9TB(0.25) C11T(0.25) H11D(0.25) H11E(0.25) H11F(0.25)
 C13T(0.25) H13D(0.25) H13E(0.25) H13F(0.25)
3.a Ternary CH refined with riding coordinates:
 C10S(H10S), C10S(H10A)
3.b Secondary CH2 refined with riding coordinates:
 C9S(H9SA,H9SB), C9T(H9TA,H9TB)
3.c 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), C1S(H1S),
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
3.d X=CH2 refined with riding coordinates:
 C20(H20A,H20B)
3.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), C7S(H7SA,H7SB,H7SC), C12S(H12D,H12E,H12F),
 C14S(H14A,H14B,H14C), C11S(H11A,H11B,H11C), C13S(H13A,H13B,H13C), C11T(H11D,
 H11E,H11F), C13T(H13D,H13E,H13F)
;
_shelx_res_checksum              16755
_olex2_submission_special_instructions 'No special instructions were received'