NIR-emissive, singlet-oxygen-sensitizing gold tetra(thiocyano)corroles
Sahu, Kasturi; Angeloni, Sara; Conradie, Jeanet; Villa, Marco; Nayak, Manisha; Ghosh, Abhik; Ceroni, Paola; Kar, Sanjib; Dalton Transactions  (2022) –; doi:10.1039/D2DT01959K

data_7710982
_publ_section_title
;
 NIR-emissive, singlet-oxygen-sensitizing gold tetra(thiocyano)corroles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01959K
_journal_year                    2022
_chemical_formula_moiety         'C49 H23 Au N10 O2 S4'
_chemical_formula_sum            'C49 H23 Au N10 O2 S4'
_chemical_formula_weight         1108.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-17
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   52.0552(6)
_cell_length_b                   51.4324(5)
_cell_length_c                   7.14602(8)
_cell_measurement_reflns_used    32124
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1210
_cell_measurement_theta_min      3.7840
_cell_volume                     19132.2(4)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_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    -76.00  14.00   0.50   29.08    --  -38.50 102.00 120.00  180
  2  \w      8.00  86.00   0.50   29.08    --   48.56-102.00  17.00  156
  3  \w     37.00 107.00   0.50   29.08    --  106.21-102.00  17.00  140
  4  \w    104.00 176.00   0.50   29.08    --  106.21 102.00 120.00  144
  5  \w   -101.00 -27.00   0.50   29.08    --  -38.50 -57.00  90.00  148
  6  \w     45.00 115.00   0.50   29.08    --   48.56  37.00 -30.00  140
  7  \w     37.00 112.00   0.50   29.08    --   48.56  57.00-150.00  150
  8  \w    103.00 171.00   0.50   29.08    --  106.21  77.00-150.00  136
  9  \w    103.00 171.00   0.50   29.08    --  106.21  77.00 -90.00  136
 10  \w     44.00 119.00   0.50   29.08    --  106.21 -61.00   0.00  150
 11  \w     37.00 109.00   0.50   29.08    --  106.21-111.00 -60.00  144
 12  \w     38.00 110.00   0.50   29.08    --  106.21 -30.00 -90.00  144
 13  \w    103.00 171.00   0.50   29.08    --  106.21  77.00  30.00  136
 14  \w    102.00 171.00   0.50   29.08    --  106.21  45.00 -60.00  138
 15  \w     42.00 111.00   0.50   29.08    --  106.21 -45.00 120.00  138
 16  \w     37.00 110.00   0.50   29.08    --   48.56  57.00 150.00  146
 17  \w     37.00 112.00   0.50   29.08    --   48.56  57.00  30.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0102964000
_diffrn_orient_matrix_UB_12      0.0174980000
_diffrn_orient_matrix_UB_13      -0.1581467000
_diffrn_orient_matrix_UB_21      -0.0264004000
_diffrn_orient_matrix_UB_22      0.0010815000
_diffrn_orient_matrix_UB_23      0.0973191000
_diffrn_orient_matrix_UB_31      0.0085665000
_diffrn_orient_matrix_UB_32      0.0242719000
_diffrn_orient_matrix_UB_33      0.1095875000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            33394
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         3.807
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48981
_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 reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       needle
_exptl_crystal_F_000             8736
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.911
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7692
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+1414.0991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.671
_reflns_Friedel_fraction_full    0.800
_reflns_Friedel_fraction_max     0.800
_reflns_number_gt                7176
_reflns_number_total             7692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01959k2.cif
_cod_data_source_block           sk-napssau
_cod_database_code               7710982
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C49 H23 Au1 N10 O2 S4'
_diffrn_oxdiff_digest_frames
;
01ab23daee110073abf38751148044bf2c02476ec8f
;
_diffrn_oxdiff_digest_hkl
;
0193413fbf96f1e0412dce01cde05314f653c0
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 N9, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C45
 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(C32) = Uanis(C27)
Uanis(C45) = Uanis(C26)
Uanis(C26) = Uanis(C45)
4. Rigid body (RIGU) restrains
 N3, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N1, C1, C2, C3, C4
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C15, C14, N3, Au1, N4, C16
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C9, C8, C7, C6, N2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C12(H12), C8(H8), C44(H44), C7(H7), C33(H33), C32(H32), C25(H25),
 C13(H13), C21(H21), C24(H24), C29(H29), C35(H35), C22(H22), C43(H43), C41(H41),
  C40(H40)
5.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.657
_oxdiff_exptl_absorpt_empirical_full_min 0.163