Systematic arrangement control of functional organic molecules
Akai, Ryota; Oka, Kouki; Nishida, Ryunosuke; Tohnai, Norimitsu; CrystEngComm  (2022) –; doi:10.1039/D2CE00336H

data_7244940
_publ_section_title
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 Systematic arrangement control of functional organic molecules
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00336H
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C20 H12 O6 S4, 2(C3.592 H10.777 N)'
_chemical_formula_sum            'C28 H34 N2 O6 S4'
_chemical_formula_weight         622.81
_chemical_name_systematic        BTDS-rac-sec-BuA
_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_block_doi                 10.5517/ccdc.csd.cc2b8scs
_audit_creation_date             2021-07-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-20 deposited with the CCDC.	2022-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.013(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.2637(8)
_cell_length_b                   6.0279(2)
_cell_length_c                   11.1259(3)
_cell_measurement_reflns_used    3575
_cell_measurement_temperature    293
_cell_measurement_theta_max      74.0260
_cell_measurement_theta_min      3.8440
_cell_volume                     1548.53(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.969
_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     33.00  69.00   0.50    1.00    --    0.00  77.00-120.00   72
  2  \w     16.00  50.00   0.50    1.00    --    0.00  37.00 120.00   68
  3  \w    -14.00  89.00   0.50    1.00    --    0.00  37.00 -60.00  206
  4  \w     44.00  70.00   0.50    5.00    --   94.90 -82.00 150.00   52
  5  \w      7.00  44.00   0.50    5.00    --   94.90 -61.00 -60.00   74
  6  \w     54.00  85.00   0.50    5.00    --   94.90 -61.00 -60.00   62
  7  \w     33.00 124.00   0.50    5.00    --   94.90 -82.00-180.00  182
  8  \w     17.00 123.00   0.50    5.00    --   94.90 -82.00 120.00  212
  9  \w     93.00 118.00   0.50    5.00    --   94.90 -61.00 -60.00   50
 10  \w     68.00 142.00   0.50    5.00    --   94.90  77.00 -60.00  148
 11  \w     93.00 123.00   0.50    5.00    --   94.90 -82.00  60.00   60
 12  \w     90.00 116.00   0.50    5.00    --   94.90 -82.00-120.00   52
 13  \w      7.00  34.00   0.50    5.00    --   94.90 -82.00 150.00   54
 14  \w    158.00 183.00   0.50    5.00    --   94.90  30.00-120.00   50
 15  \w     71.00 164.00   0.50    5.00    --   94.90  15.00  60.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0334270000
_diffrn_orient_matrix_UB_12      -0.2194145000
_diffrn_orient_matrix_UB_13      -0.0231771000
_diffrn_orient_matrix_UB_21      0.0561628000
_diffrn_orient_matrix_UB_22      -0.1309846000
_diffrn_orient_matrix_UB_23      0.0378985000
_diffrn_orient_matrix_UB_31      -0.0133675000
_diffrn_orient_matrix_UB_32      -0.0010480000
_diffrn_orient_matrix_UB_33      0.1322871000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8780
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.165
_diffrn_reflns_theta_min         3.829
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
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    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0904P)^2^+0.0501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2436
_reflns_number_total             3060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00336h2.cif
_cod_data_source_block           exp_3003
_cod_database_code               7244940
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOS
_chemical_oxdiff_usercomment     YY-2
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
2.a Ternary CH refined with riding coordinates:
 C00H(H00J)
2.b Secondary CH2 refined with riding coordinates:
 C00J(H00N,H00O)
2.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G)
2.d Idealised Me refined as rotating group:
 N006(H00A,H00H,H00I), C00I(H00K,H00L,H00M), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              32366
_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 2.824
_oxdiff_exptl_absorpt_empirical_full_min 0.560