Thermally induced reversible solid-state transformation of novel s-indacene 1,3,5,7-tetraone derivatives
Xiaoqin Shen; Yonghao Zheng; Fred Wudl; Journal of Materials Chemistry C 4 (2016) 2427–2431; doi:10.1039/C5TC03953C

data_7234596
_publ_section_title
;
 Thermally induced reversible solid-state transformation of novel
 s-indacene 1,3,5,7-tetraone derivatives
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              2427
_journal_page_last               2431
_journal_paper_doi               10.1039/C5TC03953C
_journal_volume                  4
_journal_year                    2016
_chemical_formula_sum            'C34 H34 O6 S2'
_chemical_formula_weight         602.73
_chemical_melting_point          469.0(10)
_chemical_name_common            iso-DTID-Hep2
_chemical_name_systematic
'3,5-dioxo-2,6-di(thiophen-2-yl)-3,5-dihydro-s-indacene-1,7-diyl diheptanoate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.427(18)
_cell_length_b                   28.01(3)
_cell_length_c                   5.260(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3010(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1153
_diffrn_reflns_av_unetI/netI     0.1617
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            15780
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.200
_diffrn_reflns_theta_min         1.234
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.3091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       needle
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane, ethanol'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 977 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.03(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0686
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                3116
_reflns_number_total             5190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Mater-Chem-C-2016-4-2427.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '468 - 470' was changed to
'469.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7234596
_shelxl_version_number           2013-3
_shelx_res_checksum              7312
_shelx_hkl_checksum              58478