Solid-state conformations of oligopeptides possessing an -(Aib-ΔZPhe)2- segment
Inai, Yoshihito; Oshikawa, Tatsuo; Yamashita, Mitsuji; Hirabayashi, Tadamichi; Ashitaka, Satoru; Journal of the Chemical Society, Perkin Transactions 2  (2001) 892–; doi:10.1039/b100774m

data_7216946
_publ_section_title
;
 Solid-state conformations of oligopeptides possessing an -(Aib-\DZPhe)2-
 segment
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              892
_journal_paper_doi               10.1039/b100774m
_journal_year                    2001
_chemical_compound_source        ' Synthesis by Inai, et al.'
_chemical_formula_moiety         'C38 H53 N5 O9 '
_chemical_formula_sum            'C38 H53 N5 O9'
_chemical_formula_weight         723.86
_chemical_name_common            ' Boc-(Aib-\d^Z^Phe)~2~-Aib-OMe '
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_audit_creation_date             'Fri Oct 14 15:34:38 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 101.98(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.812(2)
_cell_length_b                   19.228(4)
_cell_length_c                   19.324(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    223.2
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      25.4
_cell_volume                     3929.8(13)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  SHELXL93
_diffrn_ambient_temperature      223.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.05781
_diffrn_orient_matrix_UB_12      0.00653
_diffrn_orient_matrix_UB_13      0.04714
_diffrn_orient_matrix_UB_21      -0.01761
_diffrn_orient_matrix_UB_22      -0.04872
_diffrn_orient_matrix_UB_23      0.01329
_diffrn_orient_matrix_UB_31      0.07271
_diffrn_orient_matrix_UB_32      -0.01699
_diffrn_orient_matrix_UB_33      -0.01999
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\ a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.068
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6321
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         59.62
_diffrn_standards_decay_%        4.15
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1552.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.48
_refine_diff_density_rms         0.07
_refine_ls_extinction_coef       0.0032
_refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ '
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.335
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.335
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_obs          0.0731
_refine_ls_shift/esd_max         0.0870
_refine_ls_shift/esd_mean        0.0060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2317
_reflns_number_observed          3124
_reflns_number_total             5964
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            b100774m.txt
_cod_data_source_block           (peptide_1:_Boc-(Aib-\d^Z^Phe)~2~-Aib-OMe)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3929(1)
_cod_original_formula_sum        'C38 H53 N5 O9 '
_cod_database_code               7216946