Versicotides D–F, new cyclopeptides with lipid-lowering activities
Chen, Ran; Cheng, Zhongbin; Huang, Jian; Liu, Dong; Wu, Chongming; Guo, Peng; Lin, Wenhan; RSC Adv. 7 (2017) 49235–; doi:10.1039/C7RA07940K

data_7229383
_publ_section_title
;
 Versicotides D--F, new cyclopeptides with lipid-lowering activities
;
_journal_issue                   78
_journal_name_full               'RSC Adv.'
_journal_page_first              49235
_journal_paper_doi               10.1039/C7RA07940K
_journal_volume                  7
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H29 N5 O5, C H4 O'
_chemical_formula_sum            'C26 H33 N5 O6'
_chemical_formula_weight         511.57
_chemical_name_systematic        LZD-14-1-4
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8934(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.91935(9)
_cell_length_b                   8.16154(7)
_cell_length_c                   15.73111(16)
_cell_measurement_reflns_used    24089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.2470
_cell_measurement_theta_min      2.8080
_cell_volume                     1271.92(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -90.00  60.00   1.00    1.00    --    0.00  60.00 120.00  150
  2  \w    -90.00  60.00   1.00    1.00    --    0.00   0.00  80.00  150
  3  \w   -120.00  60.00   1.00    1.00    --  -30.00  45.00   0.00  180
  4  \w   -120.00  60.00   1.00    1.00    --  -30.00  15.00   0.00  180
  5  \w   -120.00  36.00   1.00    1.00    --  -30.00   0.00 160.00  156
  6  \w   -120.00  54.00   1.00    1.00    --  -30.00  60.00 240.00  174
  7  \w   -150.00  30.00   1.00    2.00    --  -60.00  60.00 200.00  180
  8  \w   -150.00  30.00   1.00    2.00    --  -60.00   0.00 200.00  180
  9  \w   -150.00  30.00   1.00    2.00    --  -60.00  60.00  40.00  180
 10  \w   -150.00  15.00   1.00    2.00    --  -60.00  45.00   0.00  165
 11  \w   -150.00  30.00   1.00    2.00    --  -60.00  60.00 280.00  180
 12  \w   -180.00   0.00   1.00    3.00    --  -90.00  60.00 200.00  180
 13  \w   -180.00  -3.00   1.00    3.00    --  -90.00  60.00 320.00  177
 14  \w   -180.00   0.00   1.00    3.00    --  -90.00  15.00 240.00  180
 15  \w   -180.00   0.00   1.00    3.00    --  -90.00  60.00 280.00  180
 16  \w   -180.00  -2.00   1.00    3.00    --  -90.00  30.00  80.00  178
 17  \w   -157.00  -3.00   1.00    3.00    --  -90.00  45.00  40.00  154
 18  \w   -180.00   0.00   1.00    3.00    --  -90.00  60.00  80.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1551356000
_diffrn_orient_matrix_UB_12      0.0068985000
_diffrn_orient_matrix_UB_13      -0.0002741000
_diffrn_orient_matrix_UB_21      -0.0076277000
_diffrn_orient_matrix_UB_22      0.1814389000
_diffrn_orient_matrix_UB_23      -0.0268104000
_diffrn_orient_matrix_UB_31      0.0064464000
_diffrn_orient_matrix_UB_32      0.0516958000
_diffrn_orient_matrix_UB_33      0.0943376000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25191
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.178
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.86
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 1964 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4472
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0352P)^2^+0.3512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                4397
_reflns_number_total             4472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra07940k2.cif
_cod_data_source_block           lzd-14-1-4
_cod_database_code               7229383
_chemical_oxdiff_formula         'C1 H1 O1 N1'
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.06
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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:
 C14(H14), C27(H27), C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N4(H4), N25(H25), C23(H23), C10(H10), C20(H20), C8(H8), C7(H7),
 C9(H9), C22(H22), C21(H21)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C3(H3A,H3B,H3C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C15(H15A,H15B,H15C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.179
_oxdiff_exptl_absorpt_empirical_full_min 0.495