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_7063451
_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
'C94 H62 Fe3 N34 O6 Zr2, 6(C H2 Cl2), 2[CH2Cl2]'
_chemical_formula_sum            'C102 H78 Cl16 Fe3 N34 O6 Zr2'
_chemical_formula_weight         2793.17
_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             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                97.067(5)
_cell_angle_beta                 101.196(5)
_cell_angle_gamma                92.140(5)
_cell_formula_units_Z            1
_cell_length_a                   12.632(2)
_cell_length_b                   13.972(3)
_cell_length_c                   15.789(3)
_cell_measurement_reflns_used    720
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      17.34
_cell_measurement_theta_min      2.31
_cell_volume                     2707.5(9)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2269
_diffrn_reflns_av_unetI/netI     0.3712
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22663
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.896
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.2047
_exptl_absorpt_correction_T_min  0.1260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1004 before and 0.0677 after correction.
The Ratio of minimum to maximum transmission is 0.6155.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.0066(8)
_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   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         9369
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.2579
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1047P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3327
_reflns_number_total             9369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02908a3.cif
_cod_data_source_block           ss223_zr_fe_fe_fe_zr
_cod_depositor_comments
'Adding full bibliography for 7063450--7063453.cif.'
_cod_original_cell_volume        2707.4(9)
_cod_database_code               7063451
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.950
_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. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), 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)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              98510
_shelx_hkl_checksum              62665
_shelx_fab_checksum              74649
_olex2_submission_special_instructions 'No special instructions were received'