Direct Formation of Large-Area 2D Nanosheets from Fluorescent Semiconducting Homopolymer with Orthorhombic Crystalline Orientation.
Yang, Sanghee; Shin, Suyong; Choi, Inho; Lee, Jaeho; Choi, Tae-Lim; Journal of the American Chemical Society 139 (2017) 3082–3088; doi:10.1021/jacs.6b12378

data_4125655
_publ_section_title
;
 Direct Formation of Large-Area 2D Nanosheets from Fluorescent
 Semiconducting Homopolymer with Orthorhombic Crystalline Orientation.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3082
_journal_page_last               3088
_journal_paper_doi               10.1021/jacs.6b12378
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C31 H38'
_chemical_formula_sum            'C31 H38'
_chemical_formula_weight         410.61
_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
_audit_creation_date             2016-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                99.798(2)
_cell_angle_beta                 93.975(2)
_cell_angle_gamma                94.800(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3612(3)
_cell_length_b                   15.0007(4)
_cell_length_c                   15.3112(4)
_cell_measurement_reflns_used    18244
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      76.3560
_cell_measurement_theta_min      4.5450
_cell_volume                     2553.05(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2262
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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   -117.00  -9.00   1.00    4.69    --  -41.24 -77.00  60.00  108
  2  \w    -69.00  32.00   1.00    4.69    --  -41.24  57.00-180.00  101
  3  \w      1.00  82.00   1.00    4.69    --   41.24 -99.00   0.00   81
  4  \w      1.00  82.00   1.00    4.69    --   41.24 -99.00-120.00   81
  5  \w     17.00 116.00   1.00    4.69    --   41.24  38.00 -30.00   99
  6  \w     36.00 116.00   1.00   11.67    --  112.00-111.00-180.00   80
  7  \w     36.00 116.00   1.00   11.67    --  112.00-111.00-120.00   80
  8  \w     40.00 141.00   1.00   11.67    --  112.00 -61.00  60.00  101
  9  \w     86.00 178.00   1.00   11.67    --  112.00  45.00  60.00   92
 10  \w     29.00 109.00   1.00   11.67    --  112.00 -94.00 -30.00   80
 11  \w     79.00 178.00   1.00   11.67    --  112.00  77.00 -30.00   99
 12  \w     39.00 116.00   1.00   11.67    --  112.00-111.00 150.00   77
 13  \w     65.00 135.00   1.00   11.67    --  112.00 -77.00-120.00   70
 14  \w     38.00 165.00   1.00   11.67    --  112.00 -15.00   0.00  127
 15  \w    111.00 138.00   1.00   11.67    --  112.00 -77.00   0.00   27
 16  \w     45.00  93.00   1.00   11.67    --  112.00 -77.00   0.00   48
 17  \w     39.00 113.00   1.00   11.67    --  112.00-111.00  90.00   74
 18  \w     59.00  86.00   1.00   11.67    --  112.00 -94.00-180.00   27
 19  \w     71.00 116.00   1.00   11.67    --  112.00-111.00 -90.00   45
 20  \w     30.00 140.00   1.00   11.67    --  112.00 -15.00-180.00  110
 21  \w     48.00 118.00   1.00   11.67    --  112.00 -30.00  60.00   70
 22  \w     90.00 115.00   1.00   11.67    --  112.00-111.00   0.00   25
 23  \w    103.00 137.00   1.00   11.67    --  112.00  45.00  90.00   34
 24  \w     42.00  69.00   1.00   11.67    --  112.00 -94.00  60.00   27
 25  \w     87.00 173.00   1.00   11.67    --  112.00  45.00   0.00   86
 26  \w     58.00 143.00   1.00   11.67    --  112.00 178.00 120.00   85
 27  \w     44.00 138.00   1.00   11.67    --  112.00 -45.00-180.00   94
 28  \w     91.00 116.00   1.00    1.00    --  112.00-111.00 -60.00   25
 29  \w    153.00 178.00   1.00    1.00    --  112.00   0.00-150.00   25
 30  \w     92.00 136.00   1.00    1.00    --  112.00 -30.00-120.00   44
 31  \w     91.00 116.00   1.00    1.00    --  112.00-111.00  30.00   25
 32  \w     21.00  49.00   1.00   83.65    --   54.00  78.00 144.79   28
 33  \w     21.00  49.00   1.00   83.65    --   54.00  78.00-169.64   28
 34  \w     21.00  47.00   1.00   83.65    --   54.00  79.00 -99.66   26
 35  \w     20.00  46.00   1.00   83.65    --   54.00  81.00  28.00   26
 36  \w     49.00 147.00   1.00   83.65    --   74.00  43.00-128.97   98
 37  \w     86.00 178.00   1.00    1.00    --  112.00  45.00 -90.00   92
 38  \w     84.00 178.00   1.00    1.00    --  112.00  30.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1043133000
_diffrn_orient_matrix_UB_12      0.0577515000
_diffrn_orient_matrix_UB_13      0.0189798000
_diffrn_orient_matrix_UB_21      -0.0614457000
_diffrn_orient_matrix_UB_22      -0.0416855000
_diffrn_orient_matrix_UB_23      -0.0925167000
_diffrn_orient_matrix_UB_31      -0.0632057000
_diffrn_orient_matrix_UB_32      -0.0767607000
_diffrn_orient_matrix_UB_33      0.0397754000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39788
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.879
_diffrn_reflns_theta_min         3.814
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         10645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0552P)^2^+0.6646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9356
_reflns_number_total             10645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b12378_si_003.cif
_cod_data_source_block           ysh_sp3tbuf
_cod_database_code               4125655
_chemical_oxdiff_formula         C31H38
_chemical_oxdiff_usercomment     Hexane
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C01R)=Sof(H01T)=Sof(H01U)=Sof(H01V)=1-FVAR(1)
 Sof(C01Q)=Sof(H01Q)=Sof(H01R)=Sof(H01S)=FVAR(1)
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(2)
 Sof(C01P)=Sof(H01N)=Sof(H01O)=Sof(H01P)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C00K(H00N,H00O), C00P(H00P,H00R), C014(H7AA,HL), C015(H8AA,HM), C017(H9AA,HN),
  C018(H0BA,HO), C00D(H00A,H00B), C00S(H00C,H00D), C00T(H00E,H00F), C00Z(H00H,
 H00I), C01C(H01A,H01B), C010(H01W,H01X)
3.b Aromatic/amide H refined with riding coordinates:
 C00E(H00J), C00I(H00K), C00J(H00M), C00V(H00V), C013(H013), C016(H016),
 C00G(H00G), C00L(H00L), C00Q(H00Q), C004(H004), C005(H005), C006(H006)
3.c Idealised Me refined as rotating group:
 C01A(H01Z,H,HA), C01G(H1AA,HB,HC), C01J(H3AA,HD,HE), C01L(H4AA,HF,HG),
 C01M(H5AA,HH,HI), C01N(H6AA,HJ,HK), C0AA(H0AA,H0AB,H0AC), C01D(H01C,H01D,H01E),
  C01E(H01F,H01G,H01H), C01O(H01J,H01L,H01M), C01P(H01N,H01O,H01P), C01Q(H01Q,
 H01R,H01S), C01R(H01T,H01U,H01V), C019(H01Y,HP,HQ)
3.d :
 C01F(H01), C01H(H2AA), C01I(H01I), C01K(H01K)
;
_shelx_shelxl_version_number     2014/7
_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 2.104
_oxdiff_exptl_absorpt_empirical_full_min 0.665