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_1559862
_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_absolute_configuration ad
_chemical_formula_moiety         'C37 H53 K2 O14, 2(C7 H8)'
_chemical_formula_sum            'C51 H69 K2 O14'
_chemical_formula_weight         984.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.23700(10)
_cell_length_b                   18.7126(2)
_cell_length_c                   19.1013(2)
_cell_measurement_reflns_used    22202
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.1460
_cell_measurement_theta_min      3.2850
_cell_volume                     5088.80(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -58.00   70.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -77.0000 -180.0000 128

  2 omega  -12.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000 -180.0000 114

  3 omega  100.00  153.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000 -180.0000 53

  4 omega  -17.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  -30.0000 -180.0000 161

  5 omega   57.00  150.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  178.0000  -30.0000 93

  6 omega   95.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  126.0000   69.0000 52

  7 omega   69.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000  150.0000 109

  8 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   90.0000 77

  9 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  -30.0000 77

 10 omega   71.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   65.0000 -150.0000 107

 11 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000 -150.0000 92

 12 omega   21.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000    0.0000 92

 13 omega   21.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000 -150.0000 92

 14 omega   21.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  120.0000 92

 15 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   30.0000 77

 16 omega   71.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   65.0000  -90.0000 107

 17 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000 -180.0000 77

 18 omega   69.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   68.0000   77.1316 109

 19 omega   70.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   56.0000 -113.2181 108

 20 omega  -12.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000  -60.0000 114

 21 omega  -50.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -57.0000   30.0000 114

 22 omega   57.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  178.0000   90.0000 64

 23 omega  -12.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000   60.0000 114

 24 omega   20.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   45.0000 -120.0000 127

 25 omega   20.00  135.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   45.0000   60.0000 115

 26 omega   20.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   45.0000  -30.0000 127
;
_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      0.0920513000
_diffrn_orient_matrix_UB_12      -0.0430501000
_diffrn_orient_matrix_UB_13      0.0046459000
_diffrn_orient_matrix_UB_21      0.0564800000
_diffrn_orient_matrix_UB_22      0.0701727000
_diffrn_orient_matrix_UB_23      0.0026218000
_diffrn_orient_matrix_UB_31      -0.0070802000
_diffrn_orient_matrix_UB_32      0.0001585000
_diffrn_orient_matrix_UB_33      0.0804616000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34892
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.146
_diffrn_reflns_theta_max         66.146
_diffrn_reflns_theta_min         3.306
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       needle
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 3669 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.450(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         8827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0565P)^2^+4.4367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                8624
_reflns_number_total             8827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05972b2.cif
_cod_data_source_block           jasi_3ktollt
_cod_depositor_comments
;Adding full bibliography for 1559860--1559862.cif.

 Adding full bibliography for 1559860--1559862.cif.
;
_cod_database_code               1559862
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O K'
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.612
_reflns_odcompleteness_completeness 98.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5
 0.5
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C30(H30), C37(H37)
3.b Secondary CH2 refined with riding coordinates:
 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), C24(H24a,H24b), C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b),
  C28(H28a,H28b), C29(H29a,H29b), C31(H31a,H31b), C32(H32a,H32b), C33(H33a,
 H33b), C34(H34a,H34b), C35(H35a,H35b), C36(H36a,H36b)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C38(H38),
 C39(H39), C40(H40), C41(H41), C43(H43), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51)
3.d Idealised Me refined as rotating group:
 C44(H44a,H44b,H44c), C45(H45a,H45b,H45c)
;
_olex2_date_sample_data_collection 2019-12-08
_olex2_submission_special_instructions 'No special instructions were received'