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_4035703
_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            'C35 H34 N4 O7'
_chemical_formula_weight         622.66
_chemical_name_common            1b
_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
_cell_angle_alpha                90
_cell_angle_beta                 101.399(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0264(6)
_cell_length_b                   10.9646(4)
_cell_length_c                   15.9060(4)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      4.68
_cell_volume                     3252.81(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEXII Ultra CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21016
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         68.216
_diffrn_reflns_theta_min         2.37
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         5708
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.9188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                3876
_reflns_number_total             5708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02045_si_005.cif
_cod_data_source_block           u140314mas1
_cod_database_code               4035703