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_7241635
_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         'C12 H14 N2 O4'
_chemical_formula_sum            'C12 H14 N2 O4'
_chemical_formula_weight         250.25
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 98.164(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8569(3)
_cell_length_b                   4.87510(10)
_cell_length_c                   18.1860(4)
_cell_measurement_reflns_used    5845
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.7890
_cell_measurement_theta_min      3.7650
_cell_volume                     1216.08(5)
_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    'ShelXT (Sheldrick, 2015)'
_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   -104.00 -35.00   0.50    1.29    --  -38.50 -39.00 -72.00  138
  2  \w    -42.00  28.00   0.50    1.29    --  -38.50  39.00  81.00  140
  3  \w    -17.00  53.00   0.50    1.29    --   49.06 -39.00 -72.00  140
  4  \w     46.00 115.00   0.50    1.29    --   49.06  39.00  81.00  138
  5  \w     41.00 110.00   0.50    7.21    --  106.38 -39.00 -72.00  138
  6  \w    103.00 172.00   0.50    7.21    --  106.38  39.00  81.00  138
  7  \w    -42.00  28.00   0.50    1.29    --  -38.50  37.00-120.00  140
  8  \w    -42.00  28.00   0.50    1.29    --  -38.50  37.00 150.00  140
  9  \w     46.00 116.00   0.50    1.29    --   49.06  37.00-180.00  140
 10  \w    103.00 175.00   0.50    7.21    --  106.38  30.00 -30.00  144
 11  \w     42.00 122.00   0.50    7.21    --  106.38-125.00 -30.00  160
 12  \w     38.00 109.00   0.50    7.21    --  106.38 -94.00  60.00  142
 13  \w    102.00 171.00   0.50    7.21    --  106.38  45.00-150.00  138
 14  \w     83.00 171.00   0.50    7.21    --  106.38  77.00-180.00  176
 15  \w    102.00 171.00   0.50    7.21    --  106.38  45.00 -60.00  138
 16  \w     44.00 120.00   0.50    7.21    --  106.38 -61.00  30.00  152
 17  \w     42.00 111.00   0.50    7.21    --  106.38 -45.00  90.00  138
 18  \w     26.00 114.00   0.50    1.29    --   49.06  77.00-120.00  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      0.0970269000
_diffrn_orient_matrix_UB_12      -0.1545366000
_diffrn_orient_matrix_UB_13      0.0207045000
_diffrn_orient_matrix_UB_21      0.0129887000
_diffrn_orient_matrix_UB_22      -0.0128092000
_diffrn_orient_matrix_UB_23      -0.0826651000
_diffrn_orient_matrix_UB_31      0.0550688000
_diffrn_orient_matrix_UB_32      0.2753473000
_diffrn_orient_matrix_UB_33      0.0078024000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9626
_diffrn_reflns_theta_full        77.29
_diffrn_reflns_theta_max         77.29
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54999
_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            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.039
_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     164
_refine_ls_number_reflns         2482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0669P)^2^+0.1373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                2189
_reflns_number_total             2482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce01386b2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7241635--7241640.cif.'
_cod_database_code               7241635
_chemical_oxdiff_formula         'C48 H56 N8 O16 '
_reflns_odcompleteness_completeness 100.00
_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)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C6(H6), C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_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 3.723
_oxdiff_exptl_absorpt_empirical_full_min 0.246