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

data_7244939
_publ_section_title
;
 Systematic arrangement control of functional organic molecules
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00336H
_journal_year                    2022
_chemical_formula_moiety         'C20 H12 O6 S4, 2(H3 O), 2(H2 O), C4 H8 O2'
_chemical_formula_sum            'C24 H30 O12 S4'
_chemical_formula_weight         638.72
_chemical_name_systematic        BTDBS
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2b8vxd
_audit_creation_date             2022-01-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-21 deposited with the CCDC.	2022-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.928(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.8387(11)
_cell_length_b                   6.0329(4)
_cell_length_c                   13.8772(10)
_cell_measurement_reflns_used    685
_cell_measurement_temperature    213
_cell_measurement_theta_max      74.0150
_cell_measurement_theta_min      6.4660
_cell_volume                     1374.00(17)
_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      213
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.958
_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    -83.00 -36.00   0.50    1.00    --    0.00 -37.00 -30.00   94
  2  \w    -30.00  16.00   0.50    1.00    --    0.00 -37.00 -30.00   92
  3  \w     -4.00  87.00   0.50    1.00    --    0.00  57.00-150.00  182
  4  \w      6.00 125.00   0.50    3.00    --   94.90 -82.00-180.00  238
  5  \w      5.00  69.00   0.50    3.00    --   94.90 -82.00-120.00  128
  6  \w     87.00 120.00   0.50    3.00    --   94.90 -82.00-120.00   66
  7  \w     74.00 115.00   0.50    3.00    --   94.90  15.00-150.00   82
  8  \w     83.00 109.00   0.50    3.00    --   94.90 -61.00 -60.00   52
  9  \w      5.00  72.00   0.50    3.00    --   94.90 -61.00 -60.00  134
 10  \w     77.00 146.00   0.50    3.00    --   94.90  82.00 -30.00  138
 11  \w    140.00 184.00   0.50    3.00    --   94.90  15.00-150.00   88
 12  \w     79.00 104.00   0.50    3.00    --   94.90 -82.00 120.00   50
 13  \w     85.00 149.00   0.50    3.00    --   94.90  82.00  30.00  128
;
_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      -0.0799944000
_diffrn_orient_matrix_UB_12      -0.0673870000
_diffrn_orient_matrix_UB_13      -0.0717772000
_diffrn_orient_matrix_UB_21      0.0223799000
_diffrn_orient_matrix_UB_22      -0.2463376000
_diffrn_orient_matrix_UB_23      0.0187893000
_diffrn_orient_matrix_UB_31      -0.0435849000
_diffrn_orient_matrix_UB_32      -0.0028310000
_diffrn_orient_matrix_UB_33      0.0864972000
_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  0.1078
_diffrn_reflns_av_unetI/netI     0.1315
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7363
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.287
_diffrn_reflns_theta_min         5.391
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38085
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0757P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1551
_reflns_number_total             2692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00336h2.cif
_cod_data_source_block           exp_3314
_cod_database_code               7244939
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOS
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.706
_reflns_odcompleteness_completeness 99.37
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O005(H00K,H00L), O006(H00N,H00O)
2.b Secondary CH2 refined with riding coordinates:
 C00J(H00B,H00C), C00K(H00E,H00J)
2.c Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00D(H00D), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I)
;
_shelx_res_checksum              3718
_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 2.401
_oxdiff_exptl_absorpt_empirical_full_min 0.539