Perchlorinated vanadyl tetrapyrazinoporphyrazine: spectral, redox and magnetic properties
Finogenov, Daniil N.; Faraonov, Maxim A.; Kopylova, Alina S.; Ivanov, Timur E.; Romanenko, Nikita R.; Yakushev, Ilya A.; Konarev, Dmitri V.; Stuzhin, Pavel A.; New Journal of Chemistry 48 (2024) 10067–10073; doi:10.1039/D4NJ01145G

data_7063202
_publ_section_title
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 Perchlorinated vanadyl tetrapyrazinoporphyrazine: spectral, redox and
 magnetic properties
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10067
_journal_page_last               10073
_journal_paper_doi               10.1039/D4NJ01145G
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'C39 H5 Cl16 Fe N8 O2 Sn, C20 H30 Cr, 1[C6H4Cl2], 1[C6H4Cl2]'
_chemical_formula_sum            'C71 H43 Cl20 Cr Fe N8 O2 Sn'
_chemical_formula_weight         1975.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2dcbpt
_audit_creation_date             2023-03-08
_audit_creation_method
;FinalCif V118 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2024-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8458(6)
_cell_length_b                   29.6617(11)
_cell_length_c                   27.4200(11)
_cell_measurement_reflns_used    9684
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      21.0150
_cell_measurement_theta_min      1.9040
_cell_volume                     15327.7(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  52.00   1.00  120.00    --   -8.21-129.00 -84.00   51
  2  \w    -59.00 -34.00   1.00  120.00    --   -8.21 129.00 -11.00   25
  3  \w    -69.00 -44.00   1.00  120.00    --   -8.21 139.00 162.00   25
  4  \w    -84.00 -57.00   1.00  120.00    --   -8.21 -77.00 150.00   27
  5  \w    -25.00   3.00   1.00  120.00    --   -8.21 -77.00 150.00   28
  6  \w   -100.00  84.00   1.00  120.00    --   -8.21   0.00 120.00  184
  7  \w    -11.00  22.00   1.00  120.00    --   -3.42  57.00  90.00   33
  8  \w    -71.00 -45.00   1.00  120.00    --   -3.42 -37.00 -30.00   26
  9  \w    -14.00  12.00   1.00  120.00    --   -3.42 -37.00 -30.00   26
 10  \w    -55.00 -30.00   1.00  120.00    --   -3.42 -37.00  90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1908
_diffrn_reflns_av_unetI/netI     0.1010
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            131167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.000
_diffrn_reflns_theta_max         23.000
_diffrn_reflns_theta_min         1.636
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_T_max  0.64173
_exptl_absorpt_correction_T_min  0.63424
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.60a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             7848
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.135
_exptl_crystal_size_rad          0.106
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         10669
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1562
_refine_ls_R_factor_gt           0.0970
_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^)+(0.1256P)^2^+86.3771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5857
_reflns_number_total             10669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01145g2.cif
_cod_data_source_block           exp_400_int1
_cod_depositor_comments          'Adding full bibliography for 7063202.cif.'
_cod_database_code               7063202
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Cl14, C106
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C312, C313
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C121, C122
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C111, C112
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N104, C117
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C120, C121
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C202, C203
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C207) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C201(H201), C202(H202), C203(H203), C204(H204), C205(H205)
4.b Idealised Me refined as rotating group:
 C306(H30A,H30B,H30C), C307(H30D,H30E,H30F), C308(H30G,H30H,H30I), C309(H30J,
 H30K,H30L), C310(H31A,H31B,H31C), C316(H31D,H31E,H31F), C317(H31G,H31H,H31I),
 C318(H31J,H31K,H31L), C319(H31M,H31N,H31O), C320(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_shelxl_version_number     2018/3
_smtbx_masks_special_details
;
A solvent mask was calculated and 1252 electrons were 
found in a volume of 3984\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C6H4Cl2], 1[C6H4Cl2] per Asymmetric Unit 
which account for 1184 electrons 
per unit cell.
;
_shelx_estimated_absorpt_t_min   0.659
_shelx_estimated_absorpt_t_max   0.834
_shelx_res_checksum              70302
_shelx_hkl_checksum              83514
_shelx_fab_checksum              23560