Recrystallization solvent-dependent elastic/plastic flexibility of an <i>n</i>-dodecyl-substituted tetrachlorophthalimide.
Kusumoto, Sotaro; Suzuki, Ryo; Tachibana, Masaru; Sekine, Yoshihiro; Kim, Yang; Hayami, Shinya; Chemical communications (Cambridge, England) 58 (2022) 5411–5414; doi:10.1039/d2cc00663d

data_7129915
_publ_section_title
;
 Recrystallization solvent-dependent elastic/plastic flexibility of an
 <i>n</i>-dodecyl-substituted tetrachlorophthalimide.
;
_journal_issue                   35
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5411
_journal_page_last               5414
_journal_paper_doi               10.1039/d2cc00663d
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C20 H25 Cl4 N O2'
_chemical_formula_sum            'C20 H25 Cl4 N O2'
_chemical_formula_weight         453.21
_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             2020-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-26 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.384(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.9756(2)
_cell_length_b                   7.2308(2)
_cell_length_c                   57.2041(19)
_cell_measurement_reflns_used    12730
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.1590
_cell_measurement_theta_min      2.7630
_cell_volume                     2056.28(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_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_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.861
_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    -14.00  55.00   0.50    2.50    --  -10.30  45.00 150.00  138
  2  \w    -99.00 -15.00   0.50    2.50    --  -10.30  45.00  60.00  168
  3  \w    -99.00  73.00   0.50    2.50    --  -10.30  45.00   0.00  344
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0210935000
_diffrn_orient_matrix_UB_12      -0.0477099000
_diffrn_orient_matrix_UB_13      -0.0107642000
_diffrn_orient_matrix_UB_21      0.0423986000
_diffrn_orient_matrix_UB_22      -0.0836397000
_diffrn_orient_matrix_UB_23      0.0054740000
_diffrn_orient_matrix_UB_31      -0.1346118000
_diffrn_orient_matrix_UB_32      -0.0187329000
_diffrn_orient_matrix_UB_33      0.0028401000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            20363
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.076
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+9.1796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5135
_reflns_number_total             5694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00663d4.cif
_cod_data_source_block           kusumoto200219teracl-2
_cod_depositor_comments
'Adding full bibliography for 7129915--7129916.cif.'
_cod_database_code               7129915
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C Cl O N'
_chemical_oxdiff_usercomment     100K
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.589
_diffrn_oxdiff_ac4_digest_frames
;
01716b01adaa3b98c32705c494b342de54006500817
;
_diffrn_oxdiff_ac4_digest_hkl
;
014bb9153ce822a15206edefd99a0d0e07947a
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C12(H12A,H12B), C16(H16A,H16B), C14(H14A,H14B),
 C11(H11A,H11B), C18(H18A,H18B), C13(H13A,H13B), C17(H17A,H17B), C15(H15A,H15B),
  C19(H19A,H19B)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              47706
_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 1.403
_oxdiff_exptl_absorpt_empirical_full_min 0.634