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_7129916
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-07
_audit_creation_method
;
Olex2 1.5-ac5-020
(compiled 2021.11.16 svn.r5db059d7 for Rigaku Oxford Diffraction, GUI svn.r6430)
;
_audit_update_record
;
2022-03-07 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.695(5)
_cell_angle_beta                 90.006(6)
_cell_angle_gamma                105.259(6)
_cell_formula_units_Z            2
_cell_length_a                   4.9963(4)
_cell_length_b                   5.9993(4)
_cell_length_c                   36.274(2)
_cell_measurement_reflns_used    2735
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.6160
_cell_measurement_theta_min      3.4810
_cell_volume                     1048.87(13)
_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 1.5-ac5-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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    -94.00 -46.00   0.50    4.00    --  -10.50  45.00  90.00   96
  2  \w    -20.00  37.00   0.50    4.00    --  -10.50  45.00  90.00  114
  3  \w    -88.00  77.00   0.50    4.00    --  -10.50  45.00 150.00  330
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            7278
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.246
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0844
_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^)+(0.0653P)^2^+8.6723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3176
_reflns_number_total             3598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00663d4.cif
_cod_data_source_block           kusumoto200219tetraclc12
_cod_depositor_comments
'Adding full bibliography for 7129915--7129916.cif.'
_cod_database_code               7129916
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C1) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C11(H11A,H11B), C14(H14A,H14B), C12(H12A,H12B),
 C13(H13A,H13B), C16(H16A,H16B), C15(H15A,H15B), C18(H18A,H18B), C17(H17A,H17B),
  C19(H19A,H19B)
3.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              82867
_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
;