Switching between mono and doubly reduced odd alternant hydrocarbon: designing a redox catalyst.
Ahmed, Jasimuddin; Datta, Paramita; Das, Arpan; Jomy, Stephy; Mandal, Swadhin K.; Chemical science 12 (2020) 3039–3049; doi:10.1039/d0sc05972b

data_1559860
_publ_section_title
;
 Switching between mono and doubly reduced odd alternant hydrocarbon:
 designing a redox catalyst.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              3039
_journal_page_last               3049
_journal_paper_doi               10.1039/d0sc05972b
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C25 H31 K O8'
_chemical_formula_sum            'C25 H31 K O8'
_chemical_formula_weight         498.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-18 deposited with the CCDC.	2020-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.071(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3399(4)
_cell_length_b                   27.1397(12)
_cell_length_c                   11.0226(5)
_cell_measurement_reflns_used    7126
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.2200
_cell_measurement_theta_min      3.2570
_cell_volume                     2456.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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    -12.00 102.00   1.00    4.00    --   26.33  57.00  30.00  114
  2  \w    -50.00  64.00   1.00    4.00    --   26.33 -57.00 -90.00  114
  3  \w    -12.00 102.00   1.00    4.00    --   26.33  57.00 150.00  114
  4  \w     -9.00 104.00   1.00   18.00    --   67.17 -61.00  90.00  113
  5  \w     30.00 144.00   1.00   18.00    --   67.17  61.00 -30.00  114
  6  \w     20.00 147.00   1.00   18.00    --   67.17  45.00  60.00  127
  7  \w     57.00 150.00   1.00   18.00    --   67.17 178.00   0.00   93
  8  \w     82.00 146.00   1.00   18.00    --   67.17 146.00-142.00   64
  9  \w     29.00 145.00   1.00   22.00    --  108.00 -65.00 -30.00  116
 10  \w     65.00 178.00   1.00   22.00    --  108.00  77.00 -30.00  113
 11  \w     19.00 158.00   1.00   22.00    --  108.00 -89.00 -30.00  139
 12  \w    101.00 178.00   1.00   22.00    --  108.00 104.00 120.00   77
 13  \w     69.00 178.00   1.00   22.00    --  108.00  54.00  30.00  109
 14  \w     58.00 178.00   1.00   22.00    --  108.00  43.00-180.00  120
 15  \w     21.00 113.00   1.00   22.00    --  108.00-104.00 -30.00   92
 16  \w     21.00 113.00   1.00   22.00    --  108.00-104.00-120.00   92
 17  \w     71.00 178.00   1.00   22.00    --  108.00  65.00  60.00  107
 18  \w     86.00 178.00   1.00   22.00    --  108.00 138.00-150.00   92
 19  \w    101.00 178.00   1.00   22.00    --  108.00 104.00  60.00   77
 20  \w    101.00 178.00   1.00   22.00    --  108.00 104.00 -90.00   77
 21  \w     36.00 178.00   1.00   22.00    --  108.00  32.00 120.00  142
 22  \w     69.00 140.00   1.00   22.00    --  108.00  54.00  60.00   71
 23  \w     54.00 152.00   1.00   22.00    --  108.00 -47.00  74.81   98
 24  \w     82.00 119.00   1.00   22.00    --  108.00  54.00 -30.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0144809000
_diffrn_orient_matrix_UB_12      -0.0555702000
_diffrn_orient_matrix_UB_13      0.0286592000
_diffrn_orient_matrix_UB_21      -0.0054106000
_diffrn_orient_matrix_UB_22      -0.0109384000
_diffrn_orient_matrix_UB_23      -0.1377811000
_diffrn_orient_matrix_UB_31      0.1869128000
_diffrn_orient_matrix_UB_32      0.0039916000
_diffrn_orient_matrix_UB_33      0.0187554000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16231
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.366
_diffrn_reflns_theta_max         66.366
_diffrn_reflns_theta_min         3.257
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.1134
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1679P)^2^+11.3134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3001
_refine_ls_wR_factor_ref         0.3068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3810
_reflns_number_total             4218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05972b2.cif
_cod_data_source_block           chok1_ply
_cod_depositor_comments
;Adding full bibliography for 1559860--1559862.cif.

 Adding full bibliography for 1559860--1559862.cif.
;
_cod_database_code               1559860
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O K'
_reflns_odcompleteness_completeness 98.02
_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. Restrained distances
 O4-C19
 1.39 with sigma of 0.02
 O5-C17
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) = Uanis(C17)
Uanis(C19) = Uanis(O4)
4.a Secondary CH2 refined with riding coordinates:
 C00U(H00A,H00B), C00V(H00C,H00D), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12)
;
_shelx_res_checksum              5369
_olex2_date_sample_data_collection 2020-01-25
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.612