Morphologically Tunable Square and Rectangular Nanosheets of a Simple Conjugated Homopolymer by Changing Solvents
Yang, Sanghee; Kang, Sung-Yun; Choi, Tae-Lim; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10904

data_4129087
_publ_section_title
;
 Morphologically Tunable Square and Rectangular Nanosheets of a Simple
 Conjugated Homopolymer by Changing Solvents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10904
_journal_year                    2019
_chemical_formula_moiety         'C41 H62 Si2'
_chemical_formula_sum            'C41 H62 Si2'
_chemical_formula_weight         611.08
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-08-07
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_cell_angle_alpha                85.1872(18)
_cell_angle_beta                 75.261(2)
_cell_angle_gamma                78.5459(19)
_cell_formula_units_Z            2
_cell_length_a                   10.8939(3)
_cell_length_b                   10.9617(2)
_cell_length_c                   16.6476(4)
_cell_measurement_reflns_used    11059
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      76.3190
_cell_measurement_theta_min      2.7350
_cell_volume                     1883.11(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2262
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -8.00  26.00   1.00    1.00    --  -41.24  57.00   0.00   34
  2  \w    -62.00 -14.00   1.00    1.00    --  -41.24  57.00   0.00   48
  3  \w   -129.00  40.00   1.00    1.00    --  -41.24   0.00-180.00  169
  4  \w     33.00  86.00   1.00    1.00    --   41.24-125.00  90.00   53
  5  \w     36.00 143.00   1.00    1.00    --  112.00 -77.00  60.00  107
  6  \w     77.00 115.00   1.00    1.00    --  112.00-111.00 -30.00   38
  7  \w     76.00 116.00   1.00    1.00    --  112.00-111.00-120.00   40
  8  \w     43.00 126.00   1.00    1.00    --  112.00 -61.00-180.00   83
  9  \w     89.00 172.00   1.00    1.00    --  112.00  30.00 -90.00   83
 10  \w    144.00 171.00   1.00    1.00    --  112.00  45.00-150.00   27
 11  \w    122.00 178.00   1.00    1.00    --  112.00  61.00-180.00   56
 12  \w     99.00 141.00   1.00    1.00    --  112.00  45.00-150.00   42
 13  \w     84.00 119.00   1.00    1.00    --  112.00  61.00-180.00   35
 14  \w     37.00 134.00   1.00    1.00    --  112.00 -30.00  30.00   97
 15  \w     36.00  62.00   1.00    1.00    --  112.00-111.00 -30.00   26
 16  \w     37.00 115.00   1.00    1.00    --  112.00-111.00  60.00   78
 17  \w     28.00  79.00   1.00    1.00    --   41.24-125.00 -90.00   51
 18  \w     29.00  57.00   1.00    1.00    --   41.24-125.00-180.00   28
 19  \w    107.00 178.00   1.00    1.00    --  112.00 111.00 120.00   71
 20  \w    105.00 174.00   1.00    1.00    --  112.00 111.00  90.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0902401000
_diffrn_orient_matrix_UB_12      -0.0011362000
_diffrn_orient_matrix_UB_13      -0.0878806000
_diffrn_orient_matrix_UB_21      0.0946682000
_diffrn_orient_matrix_UB_22      0.0579142000
_diffrn_orient_matrix_UB_23      0.0329326000
_diffrn_orient_matrix_UB_31      0.0708893000
_diffrn_orient_matrix_UB_32      -0.1312730000
_diffrn_orient_matrix_UB_33      0.0189750000
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12944
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         2.746
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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    1.078
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00235(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0355P)^2^+1.0634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6351
_reflns_number_total             6703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10904_si_002.cif
_cod_data_source_block           exp_857
_cod_original_cell_volume        1883.12(8)
_cod_database_code               4129087
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C41H62Si2
_diffrn_oxdiff_ac3_digest_frames
;
01b8552a152ca09af3cd8b0b858f85267b01287a7d8
;
_diffrn_oxdiff_ac3_digest_hkl
;
01138af57acba70265543f882a184ad9503337
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
 C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C)
2.e :
 C40(H40), C41(H41)
;
_shelx_res_checksum              28686
_shelx_hkl_checksum              77950
_olex2_date_sample_data_collection 2017-07-27
_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 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.834