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_1555253
_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         'C13 H8.65 O2'
_chemical_formula_sum            'C13 H8.64 O2'
_chemical_formula_weight         196.84
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-06-01 deposited with the CCDC.	2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.3790(5)
_cell_length_b                   14.8543(10)
_cell_length_c                   16.8845(10)
_cell_measurement_reflns_used    3670
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      24.9730
_cell_measurement_theta_min      2.7160
_cell_volume                     1850.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -66.00   50.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1399   57.0000  120.0000 116

  2 omega  -16.00  116.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.5461   77.0000  -30.0000 132

  3 omega   35.00  126.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.5461  178.0000  150.0000 91

  4 omega  -10.00  105.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.5461   57.0000 -120.0000 115

  5 omega  -10.00   15.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.5461   57.0000  120.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0569733000
_diffrn_orient_matrix_UB_12      -0.0080636000
_diffrn_orient_matrix_UB_13      0.0330849000
_diffrn_orient_matrix_UB_21      0.0658070000
_diffrn_orient_matrix_UB_22      -0.0295771000
_diffrn_orient_matrix_UB_23      0.0161076000
_diffrn_orient_matrix_UB_31      0.0405409000
_diffrn_orient_matrix_UB_32      0.0366224000
_diffrn_orient_matrix_UB_33      0.0203419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10323
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             821
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.0621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                1372
_reflns_number_total             1635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9sc02057h2.cif
_cod_data_source_block           ply_dimer
_cod_database_code               1555253
_chemical_oxdiff_formula         'C H N O'
_reflns_odcompleteness_completeness 86.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C5(H5), C3A(H3A)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_date_sample_data_collection 2018-03-29
_olex2_submission_special_instructions 'No special instructions were received'