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

data_7244937
_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_formula_moiety         'C20 H12 O6 S4, 2(C4 H12 N)'
_chemical_formula_sum            'C28 H36 N2 O6 S4'
_chemical_formula_weight         624.83
_chemical_name_systematic        BTDS-isoBuA
_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.cc2b8s3j
_audit_creation_date             2021-07-15
_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                 94.855(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.9234(7)
_cell_length_b                   7.4749(2)
_cell_length_c                   7.6043(2)
_cell_measurement_reflns_used    2408
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.2480
_cell_measurement_theta_min      4.7720
_cell_volume                     1581.51(7)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_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    -87.00  14.00   0.50    1.00    --    0.00 -19.00   0.00  202
  2  \w    -39.00   5.00   0.50    1.00    --    0.00 -37.00  90.00   88
  3  \w    -72.00 -43.00   0.50    1.00    --    0.00 -37.00  90.00   58
  4  \w    140.00 166.00   0.50    5.00    --   94.90  45.00  90.00   52
  5  \w    130.00 172.00   0.50    5.00    --   94.90  15.00-150.00   84
  6  \w     74.00 184.00   0.50    5.00    --   94.90  77.00-120.00  220
  7  \w     25.00 111.00   0.50    5.00    --   94.90 -61.00 120.00  172
  8  \w     18.00 119.00   0.50    5.00    --   94.90 -77.00  90.00  202
  9  \w    104.00 130.00   0.50    5.00    --   94.90  45.00  90.00   52
 10  \w     75.00 174.00   0.50    5.00    --   94.90  45.00 -30.00  198
 11  \w     69.00 112.00   0.50    5.00    --   94.90 -45.00 120.00   86
;
_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      -0.0238005000
_diffrn_orient_matrix_UB_12      -0.1821774000
_diffrn_orient_matrix_UB_13      0.0293335000
_diffrn_orient_matrix_UB_21      -0.0488495000
_diffrn_orient_matrix_UB_22      0.0755088000
_diffrn_orient_matrix_UB_23      -0.0756701000
_diffrn_orient_matrix_UB_31      0.0108988000
_diffrn_orient_matrix_UB_32      -0.0595104000
_diffrn_orient_matrix_UB_33      -0.1863545000
_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  0.0564
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.292
_diffrn_reflns_theta_min         3.177
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70006
_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    1.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0638P)^2^+0.5068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2320
_reflns_number_total             3124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00336h2.cif
_cod_data_source_block           exp_3004
_cod_database_code               7244937
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNSO
_reflns_odcompleteness_completeness 99.93
_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, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00I(H00I)
2.b Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00H)
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:
 N8(H8A,H8B,H8C), C00J(H00J,H00K,H00L), C00K(H00M,H00N,H00O)
;
_shelx_res_checksum              79460
_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 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.543