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_7241636
_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         'C13 H16 N2 O4'
_chemical_formula_sum            'C13 H16 N2 O4'
_chemical_formula_weight         264.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-02-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-01-07 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.376(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8433(12)
_cell_length_b                   11.6707(8)
_cell_length_c                   8.3343(7)
_cell_measurement_reflns_used    2379
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.9380
_cell_measurement_theta_min      4.9630
_cell_volume                     1324.48(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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    -71.00  26.00   0.50    0.83    --  -38.50  94.00 -67.00  194
  2  \w     -4.00  82.00   0.50    0.83    --   49.31 -94.00-178.00  172
  3  \w    101.00 175.00   0.50    3.00    --  106.38  94.00 -67.00  148
  4  \w     38.00 109.00   0.50    3.00    --  106.38 -94.00-178.00  142
  5  \w   -105.00 -35.00   0.50    0.83    --  -38.50 -37.00  30.00  140
  6  \w    -17.00  53.00   0.50    0.83    --   49.31 -37.00 -90.00  140
  7  \w     46.00 116.00   0.50    0.83    --   49.31  37.00-180.00  140
  8  \w     46.00 116.00   0.50    0.83    --   49.31  37.00 -60.00  140
  9  \w     94.00 171.00   0.50    3.00    --  106.38 125.00-120.00  154
 10  \w    102.00 171.00   0.50    3.00    --  106.38  45.00-180.00  138
 11  \w     38.00 110.00   0.50    3.00    --  106.38 -30.00-120.00  144
 12  \w    103.00 175.00   0.50    3.00    --  106.38  30.00 120.00  144
 13  \w     44.00 120.00   0.50    3.00    --  106.38 -61.00 -60.00  152
 14  \w     38.00 110.00   0.50    3.00    --  106.38 -30.00  90.00  144
 15  \w     42.00 111.00   0.50    3.00    --  106.38 -45.00 150.00  138
 16  \w    103.00 169.00   0.50    3.00    --  106.38  30.00  60.00  132
 17  \w    103.00 171.00   0.50    3.00    --  106.38  30.00  30.00  136
;
_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      -0.0544759000
_diffrn_orient_matrix_UB_12      -0.0769095000
_diffrn_orient_matrix_UB_13      -0.1374374000
_diffrn_orient_matrix_UB_21      -0.0896406000
_diffrn_orient_matrix_UB_22      -0.0041605000
_diffrn_orient_matrix_UB_23      0.0858076000
_diffrn_orient_matrix_UB_31      -0.0424529000
_diffrn_orient_matrix_UB_32      0.1071697000
_diffrn_orient_matrix_UB_33      -0.0952036000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9030
_diffrn_reflns_theta_full        77.06
_diffrn_reflns_theta_max         77.06
_diffrn_reflns_theta_min         4.99
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1895P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2996
_reflns_number_gt                1639
_reflns_number_total             2695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce01386b2.cif
_cod_data_source_block           4f
_cod_depositor_comments
'Adding full bibliography for 7241635--7241640.cif.'
_cod_original_cell_volume        1324.48(18)
_cod_database_code               7241636
_chemical_oxdiff_formula         'C52 H64 N8 O16 '
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C7(H7), C6(H6), C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.153
_oxdiff_exptl_absorpt_empirical_full_min 0.367