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_4025564
_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_sum            'C38 H70 N6 O9'
_chemical_formula_weight         755.00
_chemical_name_systematic
; 
 Boc-Leu-D-Leu-Aib-Leu-D-Leu-OMe
;
_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                 99.125(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3911(19)
_cell_length_b                   21.278(4)
_cell_length_c                   11.662(2)
_cell_measurement_reflns_used    6075
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      2.20
_cell_volume                     2300.9(7)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19211
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.77
_diffrn_standards_interval_count 19211
_diffrn_standards_interval_time  480
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1.0(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5187
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                4063
_reflns_number_total             5187
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo100965r_si_002.cif
_cod_data_source_block           lep
_cod_original_cell_volume        2300.9(8)
_cod_database_code               4025564