Helical Folding of Meta-Connected Aromatic Oligoureas.
Hu, Ting; Connor, Alan L.; Miller, Daniel P.; Wang, Xiao; Pei, Qiang; Liu, Rui; He, Lan; Zheng, Chong; Zurek, Eva; Lu, Zhong-Lin; Gong, Bing; Organic letters 19 (2017) 2666–2669; doi:10.1021/acs.orglett.7b01005

data_1545991
_publ_section_title
;
 Helical Folding of Meta-Connected Aromatic Oligoureas.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2666
_journal_page_last               2669
_journal_paper_doi               10.1021/acs.orglett.7b01005
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C29 H42 N4 O9, C2 H6 O S'
_chemical_formula_sum            'C31 H48 N4 O10 S'
_chemical_formula_weight         668.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6779(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.96905(13)
_cell_length_b                   20.99152(16)
_cell_length_c                   10.22172(8)
_cell_measurement_reflns_used    10018
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4560
_cell_measurement_theta_min      4.8300
_cell_volume                     3403.22(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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    -32.00  32.00   1.00    1.00    --  -41.49  57.00 -90.00   64
  2  \w     -4.00  27.00   1.00    1.00    --  -41.49  77.00  30.00   31
  3  \w    -70.00 -36.00   1.00    1.00    --  -41.49  57.00 -90.00   34
  4  \w     66.00  91.00   1.00    1.00    --   41.49-125.00  30.00   25
  5  \w     42.00 144.00   1.00    1.00    --  112.00 -77.00 -60.00  102
  6  \w    114.00 140.00   1.00    1.00    --  112.00 -30.00-120.00   26
  7  \w     99.00 173.00   1.00    1.00    --  112.00  45.00 -30.00   74
  8  \w     95.00 168.00   1.00    1.00    --  112.00 125.00 -90.00   73
  9  \w     84.00 163.00   1.00    1.00    --  112.00  61.00  60.00   79
 10  \w     56.00  99.00   1.00    1.00    --  112.00 -94.00-120.00   43
 11  \w     37.00  64.00   1.00    1.00    --  112.00 -30.00-120.00   27
 12  \w     34.00  88.00   1.00    1.00    --  112.00 -94.00-150.00   54
 13  \w   -116.00 -29.00   1.00    1.00    --  -41.49 -37.00 120.00   87
;
_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      -0.0663434000
_diffrn_orient_matrix_UB_12      0.0513404000
_diffrn_orient_matrix_UB_13      -0.0440098000
_diffrn_orient_matrix_UB_21      0.0466541000
_diffrn_orient_matrix_UB_22      0.0475801000
_diffrn_orient_matrix_UB_23      0.0975335000
_diffrn_orient_matrix_UB_31      0.0534365000
_diffrn_orient_matrix_UB_32      0.0221321000
_diffrn_orient_matrix_UB_33      -0.1075514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14213
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.458
_diffrn_reflns_theta_min         3.493
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0393P)^2^+1.8172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6462
_reflns_number_total             6879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b01005_si_002.cif
_cod_data_source_block           20160307a
_cod_depositor_comments
'Adding full bibliography for 1545991--1545992.cif.'
_cod_database_code               1545991
_chemical_oxdiff_formula         C1H1N1O1
_shelx_estimated_absorpt_t_max   0.728
_shelx_estimated_absorpt_t_min   0.613
_reflns_odcompleteness_completeness 99.90
_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 C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8), C12(H12), C23(H23), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C22(H22A,H22B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C17(H17), C20(H20), N2(H2), N3(H3A)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              29808
_shelx_hkl_checksum              42853
_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 1.334
_oxdiff_exptl_absorpt_empirical_full_min 0.799