Crystal Structure of t-Butyloxycarbonyl-L-prolyl-L-hydroxyprolyl-glicine methyl ester (Boc-Pro-Hyp-Gly-OMe)
ASANO, Akiko; IMORI, Kumiko; SAKAGUCHI, Noriko; DOI, Mitsunobu; X-ray Structure Analysis Online 26 (2010) 53–; doi:10.2116/xraystruct.26.53

data_1551752
_publ_section_title
;
 Crystal Structure of t-Butyloxycarbonyl-L-prolyl-L-hydroxyprolyl-glicine
 methyl ester (Boc-Pro-Hyp-Gly-OMe)
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              53
_journal_paper_doi               10.2116/xraystruct.26.53
_journal_volume                  26
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C18 H29 N3 O7'
_chemical_formula_sum            'C18 H29 N3 O7'
_chemical_formula_weight         399.44
_chemical_name_systematic
; 
 Boc-Pro-Hyp-Gly-OMe
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.8821(11)
_cell_length_b                   15.1509(18)
_cell_length_c                   30.928(4)
_cell_measurement_reflns_used    5956
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.39
_cell_volume                     4162.0(9)
_computing_cell_refinement       'SAINTPLUS (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINTPLUS (Bruker, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0935
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            45347
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.50
_diffrn_standards_interval_time  600
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'starting materials'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0748P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                4162
_reflns_number_total             5148
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            26_53_1.cif
_cod_data_source_block           phgm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 6524 2018-11-02 12:15:13Z antanas 

2022-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_Hall     'P 2ac 2ab  '
_cod_original_sg_symbol_H-M      'P2(1)2(1)2(1) '
_cod_original_formula_moiety     '2(C18 H29 N3 O7)'
_cod_original_formula_sum        'C36 H58 N6 O14'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     798.88
_cod_database_code               1551752