Three-Dimensional Structural Control of Diastereomeric Leu-Leu-Aib-Leu-Leu-Aib Sequences in the Solid State
Yosuke Demizu; Mitsunobu Doi; Yukiko Sato; Masakazu Tanaka; Haruhiro Okuda; Masaaki Kurihara; Journal of Organic Chemistry 75 (2010) 5234–5239; doi:10.1021/jo100965r

data_4025565
_publ_section_title
;
 Three-Dimensional Structural Control of Diastereomeric
 Leu-Leu-Aib-Leu-Leu-Aib Sequences in the Solid State
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5234
_journal_page_last               5239
_journal_paper_doi               10.1021/jo100965r
_journal_volume                  75
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C38 H70 N6 O9, C2 H3 N'
_chemical_formula_sum            'C40 H73 N7 O9'
_chemical_formula_weight         796.05
_chemical_name_systematic
; 
 Boc-Leu-D-Leu-Aib-D-Leu-Leu-Aib-OMe, MeCN 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.622(3)
_cell_angle_beta                 66.601(3)
_cell_angle_gamma                78.839(3)
_cell_formula_units_Z            2
_cell_length_a                   12.545(3)
_cell_length_b                   14.913(3)
_cell_length_c                   15.330(3)
_cell_measurement_reflns_used    8165
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.18
_cell_volume                     2552.1(9)
_computing_cell_refinement       'SAINTPLUS (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINTPLUS (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Seldrick & Gould, 1996)'
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker AXS SMART APEX (CCD area detector)'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator
'Bruker AXS Montel (conforcal multilayer optics)'
_diffrn_radiation_source         'MacScience M18XCE (rotating anode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18955
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 18955
_diffrn_standards_interval_time  660
_diffrn_standards_number         204
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel pairs'
_refine_ls_abs_structure_Flack   0.5(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         9915
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+1.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.1971
_reflns_number_gt                6637
_reflns_number_total             9915
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo100965r_si_003.cif
_cod_data_source_block           ldadla
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 '
_cod_database_code               4025565