N-Arylated peptide: troponyl residue influences the structure and conformation of N-troponylated-(di/tri)-peptides
Palai, Bibhuti Bhusana; Sharma, Nagendra K.; CrystEngComm 23 (2021) 131–139; doi:10.1039/D0CE01386B

data_7241640
_publ_section_title
;
 N-Arylated peptide: troponyl residue influences the structure and
 conformation of N-troponylated-(di/tri)-peptides
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              131
_journal_page_last               139
_journal_paper_doi               10.1039/D0CE01386B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C20 H22 N2 O4'
_chemical_formula_sum            'C20 H22 N2 O4'
_chemical_formula_weight         354.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-07
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-01-07 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                72.921(3)
_cell_angle_beta                 79.751(3)
_cell_angle_gamma                68.981(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5709(3)
_cell_length_b                   9.7281(3)
_cell_length_c                   11.5654(3)
_cell_measurement_reflns_used    4851
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.0220
_cell_measurement_theta_min      3.9800
_cell_volume                     957.65(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_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_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_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    -63.00  27.00   0.50    2.00    --  -38.50  80.00-118.00  180
  2  \w    100.00 172.00   0.50    8.00    --  106.38  80.00-118.00  144
  3  \w     41.00 131.00   0.50    8.00    --  106.38 -80.00 118.00  180
  4  \w    -42.00  28.00   0.50    2.00    --  -38.50  37.00  90.00  140
  5  \w    -42.00  28.00   0.50    2.00    --  -38.50  37.00 150.00  140
  6  \w      2.00  85.00   0.50    2.00    --   49.31 -99.00 -90.00  166
  7  \w     38.00 112.00   0.50    2.00    --   49.31  57.00  30.00  148
  8  \w    -16.00  74.00   0.50    2.00    --   49.31 -80.00 118.00  180
  9  \w    -13.00  61.00   0.50    2.00    --   49.31 -57.00 -60.00  148
 10  \w    -17.00  53.00   0.50    2.00    --   49.31 -37.00-180.00  140
 11  \w     42.00 111.00   0.50    8.00    --  106.38 -45.00  90.00  138
 12  \w     98.00 175.00   0.50    8.00    --  106.38  15.00  90.00  154
 13  \w     98.00 175.00   0.50    8.00    --  106.38  15.00   0.00  154
 14  \w     38.00 109.00   0.50    8.00    --  106.38 -94.00  90.00  142
 15  \w    102.00 171.00   0.50    8.00    --  106.38  45.00  30.00  138
 16  \w     38.00 115.00   0.50    8.00    --  106.38 -15.00-120.00  154
 17  \w     42.00 122.00   0.50    8.00    --  106.38-125.00 150.00  160
 18  \w     93.00 169.00   0.50    8.00    --  106.38  61.00   0.00  152
 19  \w     44.00 120.00   0.50    8.00    --  106.38 -61.00-180.00  152
 20  \w     42.00 130.00   0.50    8.00    --  106.38 -77.00 -90.00  176
 21  \w     38.00 109.00   0.50    8.00    --  106.38 -94.00 -90.00  142
 22  \w     44.00 120.00   0.50    8.00    --  106.38 -61.00 -90.00  152
 23  \w     42.00 122.00   0.50    8.00    --  106.38-125.00-150.00  160
 24  \w     44.00 120.00   0.50    8.00    --  106.38 -61.00 -30.00  152
 25  \w     83.00 171.00   0.50    8.00    --  106.38  77.00  30.00  176
 26  \w    103.00 175.00   0.50    8.00    --  106.38  30.00 120.00  144
 27  \w     38.00 109.00   0.50    8.00    --  106.38 -94.00  30.00  142
 28  \w     26.00 114.00   0.50    2.00    --   49.31  77.00-150.00  176
 29  \w     38.00 112.00   0.50    2.00    --   49.31  57.00 120.00  148
 30  \w     26.00  82.00   0.50    2.00    --   49.31  77.00 150.00  112
 31  \w     26.00 114.00   0.50    2.00    --   49.31  77.00 -60.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0318920000
_diffrn_orient_matrix_UB_12      -0.1233862000
_diffrn_orient_matrix_UB_13      0.1201521000
_diffrn_orient_matrix_UB_21      0.1427189000
_diffrn_orient_matrix_UB_22      0.0355994000
_diffrn_orient_matrix_UB_23      0.0055338000
_diffrn_orient_matrix_UB_31      -0.0924479000
_diffrn_orient_matrix_UB_32      0.1192171000
_diffrn_orient_matrix_UB_33      0.0712764000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14809
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.457
_diffrn_reflns_theta_min         4.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       needle
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.002
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1232P)^2^+0.0584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2470
_reflns_number_total             3838
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 3.6639\% 
 around [0.01 0.03 -1.00] (reciprocal) or [0.09 0.33 -0.94] (direct)
;
_cod_data_source_file            d0ce01386b2.cif
_cod_data_source_block           4j
_cod_depositor_comments
;
Adding full bibliography for 7241635--7241640.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H44 N4 O8'
_cod_original_formula_weight         708.79
_cod_original_formula_moiety         '2(C20 H22 N2 O4)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        957.66(5)
_cod_database_code               7241640
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C42 H46 N10 '
_diffrn_oxdiff_ac3_digest_frames
;
017af7a8de20b329e83ecfb84e1404bd5604766fd68
;
_diffrn_oxdiff_ac3_digest_hkl
;
01103c27ccfa19bfc0a9e30fa1c608d1e1909e
;
_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
2.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C2(H2A), C5(H5), C3(H3), C4(H4), C11(H11), C15(H15),
 C12(H12), C13(H13), C14(H14)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_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 7.568
_oxdiff_exptl_absorpt_empirical_full_min 0.334
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2