Storing redox equivalent in the phenalenyl backbone towards catalytic multi-electron reduction.
Bhunia, Mrinal; Sahoo, Sumeet Ranjan; Shaw, Bikash Kumar; Vaidya, Shefali; Pariyar, Anand; Vijaykumar, Gonela; Adhikari, Debashis; Mandal, Swadhin K.; Chemical science 10 (2019) 7433–7441; doi:10.1039/c9sc02057h

data_1555252
_publ_section_title
;
 Storing redox equivalent in the phenalenyl backbone towards catalytic
 multi-electron reduction.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              7433
_journal_page_last               7441
_journal_paper_doi               10.1039/c9sc02057h
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C17 H15 Co0.5 O3'
_chemical_formula_sum            'C17 H15 Co0.5 O3'
_chemical_formula_weight         296.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-23
_audit_creation_method
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Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
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_audit_update_record
;
2018-03-07 deposited with the CCDC.	2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.068(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6119(5)
_cell_length_b                   16.0078(7)
_cell_length_c                   12.0749(7)
_cell_measurement_reflns_used    2200
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.8650
_cell_measurement_theta_min      3.6650
_cell_volume                     1853.23(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
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_diffrn_detector_type            Eos
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_diffrn_measurement_details
;
  1 omega   25.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000   60.0000 63

  2 omega   75.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000   60.0000 25

  3 omega   83.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000   90.0000 28

  4 omega   56.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -54.0000   90.0000 29

  5 omega   48.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000   60.0000 26

  6 omega   29.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   21.0000   60.0000 149

  7 omega  133.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   30.0000 34

  8 omega  139.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000  150.0000 36

  9 omega  101.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.3430  111.0000   60.0000 46

 10 omega  101.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.3430  111.0000 -150.0000 27

 11 omega   89.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000 -180.0000 53

 12 omega   40.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6859   77.0000 -150.0000 60

 13 omega   44.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000  -60.0000 41

 14 omega   59.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000  -90.0000 27

 15 omega  106.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -65.0000  -90.0000 36

 16 omega   58.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6859 -178.0000    0.0000 48

 17 omega   41.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.3430 -111.0000 -120.0000 66

 18 omega   53.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6859  -99.0000 -180.0000 27

 19 omega   53.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000  -30.0000 26

 20 omega   32.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -54.0000  -60.0000 42

 21 omega   28.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  -30.0000 68

 22 omega   55.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000 -150.0000 25

 23 omega   12.00   38.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.3430 -111.0000 -120.0000 26

 24 omega   -9.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6859   57.0000  120.0000 47

 25 omega   41.00  138.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.3430   61.0000  150.0000 97

 26 omega   53.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000  150.0000 36

 27 omega   32.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -54.0000  150.0000 76

 28 omega   31.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       67.3430   77.0000   30.0000 106

 29 omega  -15.00   19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6859   77.0000 -150.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0511824000
_diffrn_orient_matrix_UB_12      0.0875371000
_diffrn_orient_matrix_UB_13      0.0365745000
_diffrn_orient_matrix_UB_21      -0.0499934000
_diffrn_orient_matrix_UB_22      -0.0156793000
_diffrn_orient_matrix_UB_23      0.1167306000
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_diffrn_orient_matrix_UB_32      -0.0366282000
_diffrn_orient_matrix_UB_33      0.0377287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7256
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_diffrn_reflns_theta_max         66.32
_diffrn_reflns_theta_min         5.38
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.918
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.0636
_exptl_crystal_description       block
_exptl_crystal_F_000             615.0820
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.3670
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_refine_ls_d_res_low             8.2252
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9725
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9725
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0944P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1490
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_reflns_limit_h_max              8
_reflns_limit_h_min              -11
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_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              -7
_reflns_number_gt                2514
_reflns_number_total             3218
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9sc02057h2.cif
_cod_data_source_block           SKM_AP_CoPLY
_cod_original_cell_volume        1853.22(17)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1555252
_chemical_oxdiff_formula         C26H14O4Co1
_reflns_odcompleteness_completeness 97.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C13(H13a,H13b), C12(H12a,H12b), C11(H11a,H11b)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C2(H2), C3(H3), C4(H4), C6(H6), C5(H5)
;
_olex2_date_sample_data_collection 2014-05-01
_olex2_submission_special_instructions 'No special instructions were received'