cis-2-Aminocyclohex-4-enecarboxylic acid as a new building block of helical foldamers
Kwon, Sunmi; Kang, Philjae; Choi, Moon-Gun; Choi, Soo Hyuk; New J. Chem. 39 (2015) 3221–; doi:10.1039/C4NJ02056A

data_7054624
_publ_section_title
;
 cis-2-Aminocyclohex-4-enecarboxylic acid as a new building block of
 helical foldamers
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              3221
_journal_paper_doi               10.1039/C4NJ02056A
_journal_volume                  39
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C29 H45 N5 O8'
_chemical_formula_sum            'C29 H45 N5 O8'
_chemical_formula_weight         591.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2014-12-23 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2829(8)
_cell_length_b                   17.955(2)
_cell_length_c                   23.143(3)
_cell_measurement_reflns_used    9709
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.34
_cell_measurement_theta_min      2.43
_cell_volume                     3857.3(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 Ver. 2014.9-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            130459
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.072
_diffrn_reflns_theta_min         2.269
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0719 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.9120.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.019
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 2570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0721P)^2^+0.5860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                6707
_reflns_number_total             7600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4nj02056a2.cif
_cod_data_source_block           Ala-ACHE_5mer_moon234
_cod_depositor_comments
'Adding full bibliography for 7054621--7054624.cif.'
_cod_database_code               7054624
_shelxl_version_number           2014/6
_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:
 C6(H6), C17(H17), C28(H28), C25(H25), C9(H9), C20(H20), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C21(H21A,H21B), C10(H10A,H10B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N27(H27), N16(H16), N8(H8), N19(H19), C23(H23), C22(H22), C11(H11),
 C12(H12)
2.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C35(H35A,H35B,H35C), C1(H1A,H1B,
 H1C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              18525
_olex2_submission_special_instructions 'No special instructions were received'