Symmetry breaking-induced double-strand helices in H-bonded coassembly.
Liang, Juncong; Liang, Junhui; Hao, Aiyou; Xing, Pengyao; Nanoscale 13 (2021) 12929–12937; doi:10.1039/d1nr02515e

data_1563646
_publ_section_title
;
 Symmetry breaking-induced double-strand helices in H-bonded coassembly.
;
_journal_issue                   30
_journal_name_full               Nanoscale
_journal_page_first              12929
_journal_page_last               12937
_journal_paper_doi               10.1039/d1nr02515e
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C33 H24 N6'
_chemical_formula_sum            'C33 H24 N6'
_chemical_formula_weight         504.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.077(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2765(7)
_cell_length_b                   7.2467(3)
_cell_length_c                   24.6245(12)
_cell_measurement_reflns_used    3140
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.8640
_cell_measurement_theta_min      3.3400
_cell_volume                     2725.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     51.00  76.00   1.00    0.50    --   48.45  67.00  97.00   25
  2  \w    107.00 177.00   1.00    1.30    --  106.49  19.00  60.00   70
  3  \w     96.00 178.00   1.00    1.30    --  106.49  19.00  30.00   82
  4  \w     88.00 176.00   1.00    1.30    --  106.49  67.00  97.00   88
  5  \w     34.00  93.00   1.00    1.30    --  106.49 -99.00-120.00   59
  6  \w     34.00  95.00   1.00    1.30    --  106.49 -99.00 -90.00   61
  7  \w    -67.00  21.00   1.00    0.50    --  -48.45  67.00  97.00   88
  8  \w    -77.00 -24.00   1.00    1.30    --  -86.25  67.00  97.00   53
  9  \w    -43.00 -15.00   1.00    1.30    --  -86.25  38.00 -60.00   28
 10  \w    -40.00 -13.00   1.00    1.30    --  -86.25  38.00 -90.00   27
 11  \w   -108.00 -30.00   1.00    0.50    --  -48.45 -67.00 -36.00   78
 12  \w    -96.00 -71.00   1.00    1.30    --  -86.25 -67.00 -36.00   25
 13  \w   -159.00-134.00   1.00    1.30    --  -86.25 -67.00 -36.00   25
 14  \w   -117.00 -86.00   1.00    0.50    --  -48.45-125.00  30.00   31
 15  \w     34.00  64.00   1.00    1.30    --  106.49 -57.00 -90.00   30
 16  \w    -14.00  11.00   1.00    0.50    --   48.45 -67.00 -36.00   25
 17  \w     40.00  81.00   1.00    1.30    --  106.49 -67.00 -36.00   41
 18  \w     48.00 105.00   1.00    1.30    --  106.49 -77.00   0.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0703475000
_diffrn_orient_matrix_UB_12      -0.1406513000
_diffrn_orient_matrix_UB_13      0.0181175000
_diffrn_orient_matrix_UB_21      0.0000614000
_diffrn_orient_matrix_UB_22      -0.0817193000
_diffrn_orient_matrix_UB_23      -0.0577609000
_diffrn_orient_matrix_UB_31      0.0722626000
_diffrn_orient_matrix_UB_32      0.1367891000
_diffrn_orient_matrix_UB_33      -0.0159285000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15831
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.066
_diffrn_reflns_theta_max         67.066
_diffrn_reflns_theta_min         3.376
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.230
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.1091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3143
_reflns_number_total             4826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nr02515e2.cif
_cod_data_source_block           201201c
_cod_depositor_comments
'Adding full bibliography for 1563646--1563647.cif.'
_cod_database_code               1563646
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CN
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.983
_reflns_odcompleteness_completeness 99.04
_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 N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N003(H003), N005(H005), N007(H007), C00F(H00F), C00I(H00I), C00J(H00J),
 C00M(H00M), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S),
 C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013), C014(H014)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53040
_shelx_fab_checksum              52642
_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 1.507
_oxdiff_exptl_absorpt_empirical_full_min 0.529