Synthesis and Conformational Analysis of Alternately N-Alkylated Aromatic Amide Oligomers.
Urushibara, Ko; Masu, Hyuma; Mori, Hirotoshi; Azumaya, Isao; Hirano, Tomoya; Kagechika, Hiroyuki; Tanatani, Aya; The Journal of organic chemistry 83 (2018) 14338–14349; doi:10.1021/acs.joc.8b02045

data_4035702
_publ_section_title
;
 Synthesis and Conformational Analysis of Alternately N-Alkylated Aromatic
 Amide Oligomers.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              14338
_journal_page_last               14349
_journal_paper_doi               10.1021/acs.joc.8b02045
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C31 H26 N4 O7'
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_space_group_name_Hall           '-P 1'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
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_cell_angle_gamma                93.724(3)
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_cell_length_c                   20.7293(10)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      4.33
_cell_volume                     2679.2(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33351
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.458
_diffrn_reflns_theta_min         4.326
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.840
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         9426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0636P)^2^+2.2176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7411
_reflns_number_total             9426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02045_si_002.cif
_cod_data_source_block           u140410uru1
_cod_database_code               4035702
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2013-4
_shelx_res_checksum              8902
_shelx_hkl_checksum              65039