The Bisindolylmaleimides With Anti-Parallel Conformation by N-Dodecyl Chains on Indole Rings:Thermal Property and Intensive Solid-State Fluorescence in Single Crystal
Li, Ting-Ting; Gao, Yong-Chen; Zhou, Jin-Xiu; Huang, Mu-Hua; Luo, Yunjun; RSC Adv.  (2015) –; doi:10.1039/C5RA14860J

data_7222409
_publ_section_title
;
 The Bisindolylmaleimides With Anti-Parallel Conformation by N-Dodecyl
 Chains on Indole Rings:Thermal Property and Intensive Solid-State
 Fluorescence in Single Crystal
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA14860J
_journal_year                    2015
_chemical_formula_moiety         'C44 H61 N3 O2'
_chemical_formula_sum            'C44 H61 N3 O2'
_chemical_formula_weight         663.96
_chemical_melting_point          368
_chemical_name_common            N',N''-Didodecylbisindolylmaleimide
_chemical_name_systematic
3,4-bis(1-dodecyl-1H-indol-3-yl)-1H-pyrrole-2,5-dione
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-09-25
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2015-10-01 deposited with the CCDC.
2015-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                88.215(7)
_cell_angle_beta                 79.997(7)
_cell_angle_gamma                83.701(7)
_cell_formula_units_Z            2
_cell_length_a                   11.2782(9)
_cell_length_b                   11.2830(9)
_cell_length_c                   15.7258(13)
_cell_measurement_reflns_used    3237
_cell_measurement_temperature    102.3
_cell_measurement_theta_max      29.1674
_cell_measurement_theta_min      3.1720
_cell_volume                     1958.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      102.3
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   16.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9831   77.0000  -30.0000 38

  2 omega  -18.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2956 -102.0000   92.0000 83

  3 omega  -19.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2956  -37.0000  -30.0000 56

  4 omega   -5.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2956  -77.0000  -60.0000 55

  5 omega  -38.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2956  -37.0000   90.0000 82

  6 omega   -9.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2956   77.0000 -120.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0305009000
_diffrn_orient_matrix_UB_12      -0.0029655000
_diffrn_orient_matrix_UB_13      -0.0356015000
_diffrn_orient_matrix_UB_21      -0.0547921000
_diffrn_orient_matrix_UB_22      0.0242999000
_diffrn_orient_matrix_UB_23      0.0256694000
_diffrn_orient_matrix_UB_31      0.0139519000
_diffrn_orient_matrix_UB_32      0.0582918000
_diffrn_orient_matrix_UB_33      -0.0131374000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14911
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.18
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             724
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethyl Acetate and Petroleum Ether'
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7680
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+1.1308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                5830
_reflns_number_total             7680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra14860j2.cif
_cod_data_source_block           exp_830
_cod_database_code               7222409
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32