Synthesis, structure and spectroelectrochemistry of hybrid metal(iv)phthalocyaninato-capped 3d-metal pyrazoloximates as prospective precursors of stimuli-induced (responsive) single-molecule magnets, logic gates and qubits
Belova, Svetlana A.; Dudkin, Semyon V.; Belov, Alexander S.; Danshina, Anastasia A.; Dorovatovskii, Pavel V.; Budnikova, Yulia H.; Khrizanforova, Vera V.; Bratskaya, Svetlana Yu.; Balatskiy, Denis V.; Voloshin, Yan Z.; New Journal of Chemistry 48 (2024) 17831–17848; doi:10.1039/D4NJ02908A

data_7063453
_publ_section_title
;
 Synthesis, structure and spectroelectrochemistry of hybrid
 metal(iv)phthalocyaninato-capped 3d-metal pyrazoloximates as prospective
 precursors of stimuli-induced (responsive) single-molecule magnets, logic
 gates and qubits
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17831
_journal_page_last               17848
_journal_paper_doi               10.1039/D4NJ02908A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'C47 H34 Fe N17 O3 Zr, 2(C H Cl3), Cl, 2[CHCl3]'
_chemical_formula_sum            'C51 H38 Cl13 Fe N17 O3 Zr'
_chemical_formula_weight         1544.90
_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   mixed
_audit_creation_date             2024-08-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                105.651(2)
_cell_angle_beta                 94.089(2)
_cell_angle_gamma                94.732(2)
_cell_formula_units_Z            4
_cell_length_a                   12.7743(5)
_cell_length_b                   20.9149(8)
_cell_length_c                   24.0058(9)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      2.35
_cell_volume                     6125.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SC-XRD SUITE  (Bruker, 2019)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.1126
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55033
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.770
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1481 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.7758.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       plate
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.123
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1410
_refine_ls_number_reflns         21513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2144
_refine_ls_wR_factor_ref         0.2444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12568
_reflns_number_total             21513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02908a3.cif
_cod_data_source_block           ss223_zr_fe
_cod_depositor_comments
'Adding full bibliography for 7063450--7063453.cif.'
_cod_database_code               7063453
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N7(H7), N8(H8), N9(H9), N7A(H7A), N8A(H8AA), N9A(H9AA)
2.b Ternary CH refined with riding coordinates:
 C2S(H2S), C4S(H4S), C1S(H1S), C3S(H3S)
2.c Me refined with riding coordinates:
 C10A(H10D,H10E,H10F)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8A), C9(H9A), C13(H13), C14(H14), C18(H18), C19(H19),
 C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35),
  C36(H36), C37(H37), C42(H42), C43(H43), C44(H44), C45(H45), C3A(H3A),
 C4A(H4A), C8A(H8AB), C9A(H9AB), C13A(H13A), C14A(H14A), C18A(H18A), C19A(H19A),
  C20A(H20A), C21A(H21A), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A),
 C34A(H34A), C35A(H35A), C36A(H36A), C37A(H37A), C42A(H42A), C43A(H43A),
 C44A(H44A), C45A(H45A)
2.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C5A(H5AA,H5AB,
 H5AC), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              6989
_shelx_hkl_checksum              14402
_shelx_fab_checksum              96304
_olex2_submission_special_instructions 'No special instructions were received'