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_7229382
_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_compound_source        'Aspergillus versicolor'
_chemical_formula_moiety         'C26 H29 N5 O5, C H4 O'
_chemical_formula_sum            'C27 H33 N5 O6'
_chemical_formula_weight         523.58
_chemical_name_systematic        LZD-14-1-37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.58993(7)
_cell_length_b                   10.68072(7)
_cell_length_c                   28.6559(2)
_cell_measurement_reflns_used    19614
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.8230
_cell_measurement_theta_min      3.0740
_cell_volume                     2629.08(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.984
_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    -80.00  70.00   1.00    1.00    --    0.00  55.00  90.00  150
  2  \w   -135.00  16.00   1.00    1.00    --  -45.00  30.00   0.00  151
  3  \w   -135.00  13.00   1.00    1.00    --  -45.00  55.00 270.00  148
  4  \w   -100.00  40.00   1.00    1.00    --  -45.00  55.00  90.00  140
  5  \w   -164.00 -25.00   1.00    7.00    --  -90.00  30.00   0.00  139
  6  \w   -180.00 -45.00   1.00    7.00    --  -90.00  55.00 270.00  135
  7  \w   -180.00   0.00   1.00    7.00    --  -90.00   0.00   0.00  180
  8  \w   -180.00 -24.00   1.00    7.00    --  -90.00  55.00   0.00  156
  9  \w    -80.00  70.00   1.00    1.00    --    0.00  55.00  90.00  150
;
_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      0.0116822000
_diffrn_orient_matrix_UB_12      -0.1290388000
_diffrn_orient_matrix_UB_13      0.0237619000
_diffrn_orient_matrix_UB_21      -0.0611629000
_diffrn_orient_matrix_UB_22      -0.0629648000
_diffrn_orient_matrix_UB_23      -0.0447618000
_diffrn_orient_matrix_UB_31      0.1681647000
_diffrn_orient_matrix_UB_32      -0.0139089000
_diffrn_orient_matrix_UB_33      -0.0179453000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24101
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.684
_diffrn_reflns_theta_min         3.084
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82881
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1941 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0670P)^2^+0.3780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                4688
_reflns_number_total             4759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra07940k2.cif
_cod_data_source_block           lzd-14-1-9_
_cod_original_cell_volume        2629.09(3)
_cod_database_code               7229382
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.56
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C28(H28), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C16(H16A,H16B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N26(H26), N12(H12), C7(H7), C21(H21), C10(H10), C24(H24), C9(H9),
 C22(H22), C8(H8), C23(H23)
2.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C)
2.e Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_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 1.783
_oxdiff_exptl_absorpt_empirical_full_min 0.471