Structural modification of nickel tetra(thiocyano)corroles during electrochemical water oxidation.
Nayak, Panisha; Singh, Ajit Kumar; Nayak, Manisha; Kar, Subhajit; Sahu, Kasturi; Meena, Kiran; Topwal, Dinesh; Indra, Arindam; Kar, Sanjib; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14922–14932; doi:10.1039/d4dt01628a

data_7716828
_publ_section_title
;
 Structural modification of nickel tetra(thiocyano)corroles during
 electrochemical water oxidation.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14922
_journal_page_last               14932
_journal_paper_doi               10.1039/d4dt01628a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'0.5(C44 H14.4 N11 Ni S4), 0.5(C44 H16 N11 Ni S4), 1.5[C5H5N], 1.5[C5H5N]'
_chemical_formula_sum            'C59 H30.2 N14 Ni S4'
_chemical_formula_weight         1122.149
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2024-07-04
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.05.30 svn.r93eb12d9 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-07-18 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                97.682(2)
_cell_angle_beta                 102.718(2)
_cell_angle_gamma                90.036(2)
_cell_formula_units_Z            4
_cell_length_a                   13.5052(3)
_cell_length_b                   16.0286(4)
_cell_length_c                   25.3258(7)
_cell_measurement_reflns_used    13890
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      30.6880
_cell_measurement_theta_min      3.5390
_cell_volume                     5297.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9595
_diffrn_measured_fraction_theta_max 0.9595
_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      0.00  51.00   0.50  119.90    --    7.32-117.00  62.00  102
  2  \w     30.00  66.00   0.50  119.90    --    7.32-162.00 -87.00   72
  3  \w    -42.00 -15.00   0.50  119.90    --   -7.95 -77.00  90.00   54
  4  \w    -30.00  19.00   0.50  119.90    --   -7.95  77.00 -30.00   98
  5  \w    -22.00  13.00   0.50  119.90    --   -7.95 -77.00-150.00   70
  6  \w    -29.00   8.00   0.50  119.90    --   -7.95  77.00  60.00   74
  7  \w    -71.00   3.00   0.50  119.90    --   -7.95 -57.00 120.00  148
  8  \w    -72.00  -7.00   0.50  119.90    --   -7.95 -37.00-150.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_Laue_measured_fraction_full 0.9595
_diffrn_reflns_Laue_measured_fraction_max 0.9595
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            59334
_diffrn_reflns_point_group_measured_fraction_full 0.9595
_diffrn_reflns_point_group_measured_fraction_max 0.9595
_diffrn_reflns_theta_full        24.9998
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       needle
_exptl_crystal_F_000             2301.492
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.1502
_refine_diff_density_min         -0.7867
_refine_diff_density_rms         0.1281
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             6.3328
_refine_ls_goodness_of_fit_ref   1.0907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         17879
_refine_ls_number_restraints     1068
_refine_ls_restrained_S_all      1.0576
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+18.1332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2314
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                11888
_reflns_number_total             17879
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt01628a2.cif
_cod_data_source_block           ni_tccscn
_cod_depositor_comments          'Adding full bibliography for 7716828.cif.'
_cod_original_formula_sum        'C59 H30.2 N14 Ni1 S4'
_cod_database_code               7716828
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C9BA, Ni0A, N3AA, N1AA, N0AA, N2AA, C8BA, C5BA, C5AA, C8AA, C3AA, C0AA, C0BA,
 C3BA, C7BA, C4BA, C6BA, C6AA, C4AA, C7AA, C9AA, C2AA, C1AA, C1BA, C2BA, S3AA,
 C3DA, S2AA, C6CA, S1AA, S0AA, C3EA, C8DA, C4DA, C2EA, C4CA, C0CA, C7CA, C1DA,
 C1EA, C0EA, N0BA, C7DA, C5DA, N12, C3CA, C1CA, C8CA, C0DA, N8AA, N7AA, C6DA,
 C2CA, C9CA, C9DA, C5CA, C2DA, N6AA, N4AA, N5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, Ni1, N4, N1, N2, N3, C19, C16, C1, C4, C9, C6, C11, C14, C18, C15, C17,
 C2, C3, C5, C8, C10, C7, C12, C13, S4, C34, S3, S1, S2, C20, C27, C44, C35,
 C39, C43, C41, C42, C21, C25, C28, N11, C36, C38, N10, N8, N9, C22, C24, C29,
 C31, C37, C23, C30, C40, C26, C33, N7, N5, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: S5(0.1) S11(0.1) H6AA(0.9) H2BA(0.9) H1BA(0.9) H7AA(0.9) H4CA(0.9)
 H8CA(0.9) H7CA(0.9) H0CA(0.9) H3CA(0.9) H1CA(0.9) H8DA(0.9) H0DA(0.9)
 H4DA(0.9) H7DA(0.9) H1DA(0.9) H5DA(0.9)
 Fixed Uiso: C49(0.08) C46(0.051688) C45(0.051905) C50(0.030339) C48(0.050119)
 C51(0.04999) C47(0.046628)
4.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C8(H8), C6AA(H6AA), C22(H22), C2BA(H2BA), C12(H12), C7(H7),
 C1BA(H1BA), C13(H13), C25(H25), C7AA(H7AA), C4CA(H4CA), C24(H24), C8CA(H8CA),
 C7CA(H7CA), C35(H35), C36(H36), C28(H28), C39(H39), C38(H38), C0CA(H0CA),
 C3CA(H3CA), C1CA(H1CA), C8DA(H8DA), C0DA(H0DA), C4DA(H4DA), C29(H29),
 C7DA(H7DA), C1DA(H1DA), C32(H32), C5DA(H5DA), C31(H31)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_special_details
;
A solvent mask was calculated and 512 electrons were 
found in a volume of 1851\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1.5[C5H5N], 1.5[C5H5N] per Formula Unit 
which account for 504 electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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
;