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_4035704
_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            'C37 H31 Cl N4 O7'
_chemical_formula_weight         679.11
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.146(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2513(8)
_cell_length_b                   11.5028(5)
_cell_length_c                   15.5440(7)
_cell_measurement_reflns_used    8856
_cell_measurement_temperature    223
_cell_measurement_theta_max      68.15
_cell_measurement_theta_min      3.66
_cell_volume                     3306.4(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      223
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII Ultra CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22722
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.362
_diffrn_reflns_theta_min         2.389
_exptl_absorpt_coefficient_mu    1.501
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0686P)^2^+0.6028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4145
_reflns_number_total             5999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02045_si_004.cif
_cod_data_source_block           u140501uru2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4035704
_shelx_estimated_absorpt_t_min   0.585
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2013-3
_shelx_res_checksum              33421
_shelx_hkl_checksum              41122