Helical Foldamer Containing a Combination of Cyclopentane-1,2-diamine and 2,2-Dimethylmalonic Acid
Norikazu Yamazaki; Yosuke Demizu; Yukiko Sato; Mitsunobu Doi; Masaaki Kurihara; Journal of Organic Chemistry 78 (2013) 9991–9994; doi:10.1021/jo401505b

data_4028633
_publ_section_title
;
 Helical Foldamer Containing a Combination of Cyclopentane-1,2-diamine and
 2,2-Dimethylmalonic Acid
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9991
_journal_page_last               9994
_journal_paper_doi               10.1021/jo401505b
_journal_volume                  78
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C56 H92 N10 O13, 3(C H Cl3)'
_chemical_formula_sum            'C59 H95 Cl9 N10 O13'
_chemical_formula_weight         1471.51
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.740(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6333(11)
_cell_length_b                   35.622(4)
_cell_length_c                   10.5239(12)
_cell_measurement_reflns_used    8202
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.25
_cell_volume                     3603.7(7)
_computing_cell_refinement       'SAINT-PLUS (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-PLUS (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD (Bruker APEX)'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'conforcal (Bruker Montel)'
_diffrn_radiation_source         'rotating anode (M18XCE)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31535
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.14
_diffrn_standards_decay_%        4.79
_diffrn_standards_interval_count 31535
_diffrn_standards_interval_time  720
_diffrn_standards_number         699
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.8566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack (1983), 7699 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         15765
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+1.5631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                15346
_reflns_number_total             15765
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo401505b_si_003.cif
_cod_data_source_block           dmz5
_cod_original_cell_volume        3603.6(7)
_cod_database_code               4028633