Hydrogen bonded co-assembly of aromatic amino acids and bipyridines that serves as a sacrificial template in superstructure formation.
Wang, Zhuoer; Cheng, Qiuhong; Xing, Pengyao; Cao, Zhaozhen; Hao, Aiyou; Soft matter 15 (2019) 6596–6603; doi:10.1039/c9sm01271k

data_1552116
_publ_section_title
;
 Hydrogen bonded co-assembly of aromatic amino acids and bipyridines that
 serves as a sacrificial template in superstructure formation.
;
_journal_issue                   32
_journal_name_full               'Soft matter'
_journal_page_first              6596
_journal_page_last               6603
_journal_paper_doi               10.1039/c9sm01271k
_journal_volume                  15
_journal_year                    2019
_chemical_formula_moiety         '2(C17 H15 N O4), C10 H8 N2'
_chemical_formula_sum            'C44 H38 N4 O8'
_chemical_formula_weight         750.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.576(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   46.5364(17)
_cell_length_b                   4.8799(2)
_cell_length_c                   16.5283(6)
_cell_measurement_reflns_used    4452
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      74.8160
_cell_measurement_theta_min      3.8130
_cell_volume                     3689.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.982
_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   -123.00 -34.00   1.00    0.70    --  -48.45 -12.00 -45.00   89
  2  \w    -42.00  26.00   1.00    0.70    --  -48.45  12.00 126.00   68
  3  \w     49.00  97.00   1.00    0.70    --   48.45  12.00 126.00   48
  4  \w      5.00  57.00   1.00    0.70    --   48.45 -12.00 -45.00   52
  5  \w   -133.00 -92.00   1.00    4.50    --  -86.25 -12.00 -45.00   41
  6  \w    -81.00 -56.00   1.00    4.50    --  -86.25  12.00 126.00   25
  7  \w     73.00  99.00   1.00    4.50    --  106.49 -12.00 -45.00   26
  8  \w     91.00 172.00   1.00    4.50    --  106.49  12.00 126.00   81
  9  \w     43.00  92.00   1.00    0.70    --   48.45-125.00-120.00   49
 10  \w     32.00 119.00   1.00    4.50    --  106.49 -30.00 -60.00   87
 11  \w     56.00 129.00   1.00    4.50    --  106.49 -77.00  30.00   73
 12  \w     38.00  91.00   1.00    4.50    --  106.49 -94.00 -30.00   53
 13  \w     58.00 108.00   1.00    4.50    --  106.49 -94.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0780712000
_diffrn_orient_matrix_UB_12      -0.0429824000
_diffrn_orient_matrix_UB_13      0.0230158000
_diffrn_orient_matrix_UB_21      0.0509454000
_diffrn_orient_matrix_UB_22      -0.0343349000
_diffrn_orient_matrix_UB_23      -0.0245917000
_diffrn_orient_matrix_UB_31      0.0163942000
_diffrn_orient_matrix_UB_32      0.3107145000
_diffrn_orient_matrix_UB_33      0.0004429000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8998
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.035
_diffrn_reflns_theta_min         3.865
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
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    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0723
_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^)+(0.0438P)^2^+17.4454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2672
_reflns_number_total             3229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sm01271k2.cif
_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 1552116.cif.'
_cod_database_code               1552116
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         CNO
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.989
_reflns_odcompleteness_completeness 98.68
_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, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C6(H6), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21), C8(H8), C12(H12), C14(H14), C22(H22)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              57864
_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 1.982
_oxdiff_exptl_absorpt_empirical_full_min 0.690