Glutathione peroxidase mimics based on conformationally-restricted, <i>peri</i>-like, 4,5-disubstituted fluorene dichalcogenides.
Jagdev, Kesar; Tanini, Damiano; Lownes, Jack W.; Figliola, Carlotta; Male, Louise; Capperucci, Antonella; Grainger, Richard S.; Organic & biomolecular chemistry 19 (2021) 10565–10569; doi:10.1039/d1ob02153b

data_7158423
_publ_section_title
;
 Glutathione peroxidase mimics based on conformationally-restricted,
 <i>peri</i>-like, 4,5-disubstituted fluorene dichalcogenides.
;
_journal_issue                   48
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              10565
_journal_page_last               10569
_journal_paper_doi               10.1039/d1ob02153b
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C15 H12 Se2'
_chemical_formula_sum            'C15 H12 Se2'
_chemical_formula_weight         350.17
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-25 deposited with the CCDC.	2021-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1924(2)
_cell_length_b                   17.1924(2)
_cell_length_c                   8.8177(2)
_cell_measurement_reflns_used    10977
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2920
_cell_measurement_theta_min      5.1020
_cell_volume                     2606.32(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1768
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -65.00  30.00   1.00    1.00    --  -42.56  38.00  60.00   95
  2  \w     20.00 115.00   1.00    1.00    --   42.56  38.00-150.00   95
  3  \w     23.00  98.00   1.00    1.00    --   42.56-125.00-180.00   75
  4  \w     79.00 177.00   1.00    1.94    --  106.63  61.00-180.00   98
  5  \w     35.00 118.00   1.00    1.94    --  106.63-125.00-180.00   83
  6  \w     75.00 178.00   1.00    1.94    --  106.63  77.00 150.00  103
  7  \w     44.00 143.00   1.00    1.94    --  106.63-163.00  55.00   99
  8  \w     20.00 178.00   1.00    1.94    --  106.63   0.00  30.00  158
  9  \w     79.00 177.00   1.00    1.94    --  106.63  59.00 166.23   98
 10  \w   -116.00 -11.00   1.00    1.00    --  -42.56 -77.00 -60.00  105
 11  \w    -69.00  28.00   1.00    1.00    --  -42.56  57.00 -90.00   97
 12  \w     16.00 113.00   1.00    1.00    --   42.56  57.00  90.00   97
 13  \w     76.00 172.00   1.00    1.94    --  106.63  72.00-142.00   96
 14  \w     36.00 134.00   1.00    1.94    --  106.63 -61.00 150.00   98
 15  \w     83.00 178.00   1.00    1.94    --  106.63  30.00  90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0318070000
_diffrn_orient_matrix_UB_12      -0.0642087000
_diffrn_orient_matrix_UB_13      -0.1048809000
_diffrn_orient_matrix_UB_21      0.0827033000
_diffrn_orient_matrix_UB_22      0.0328620000
_diffrn_orient_matrix_UB_23      0.0190145000
_diffrn_orient_matrix_UB_31      0.0126584000
_diffrn_orient_matrix_UB_32      -0.0533288000
_diffrn_orient_matrix_UB_33      0.1384349000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12547
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.575
_diffrn_reflns_theta_min         3.636
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.862
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1192 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.040(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0146
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+1.7030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0368
_refine_ls_wR_factor_ref         0.0369
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                2608
_reflns_number_total             2627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob02153b2.cif
_cod_data_source_block           dimethyl-9H-fluoreno-diselenine
_cod_depositor_comments
'Adding full bibliography for 7158423--7158424.cif.'
_cod_original_cell_volume        2606.32(8)
_cod_database_code               7158423
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H12 Se2'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              32490
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.825