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_7063452
_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 Co N17 O3 Zr, 2(Cl), C6 H6, 1[H2O], 0.7[H2O], 0.5[H2O]'
_chemical_formula_sum            'C53 H44.4 Cl2 Co N17 O5.2 Zr'
_chemical_formula_weight         1223.70
_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                81.418(9)
_cell_angle_beta                 72.559(9)
_cell_angle_gamma                79.554(9)
_cell_formula_units_Z            2
_cell_length_a                   11.2098(17)
_cell_length_b                   15.554(2)
_cell_length_c                   15.734(2)
_cell_measurement_reflns_used    9334
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.73
_cell_measurement_theta_min      2.38
_cell_volume                     2560.6(6)
_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
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0720
_diffrn_reflns_av_unetI/netI     0.1165
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16785
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.811
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1124 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.7449.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.428
_refine_diff_density_min         -2.156
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         9022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1482
_refine_ls_R_factor_gt           0.0991
_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^)+(0.1580P)^2^+11.6507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2527
_refine_ls_wR_factor_ref         0.3002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5516
_reflns_number_total             9022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02908a3.cif
_cod_data_source_block           ss226_zr_co
_cod_depositor_comments
'Adding full bibliography for 7063450--7063453.cif.'
_cod_original_cell_volume        2560.6(7)
_cod_original_formula_sum        'C53 H44.40 Cl2 Co N17 O5.20 Zr'
_cod_database_code               7063452
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.908
_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)
2.b 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), C1S(H1S),
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              65035
_shelx_hkl_checksum              83064
_shelx_fab_checksum              44279
_olex2_submission_special_instructions 'No special instructions were received'