#------------------------------------------------------------------------------
#$Date: 2021-02-04 23:55:05 +0100 (jue 04 de feb de 2021) $
#$Revision: 261587 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/16/7241636.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7241636
loop_
_publ_author_name
'Palai, Bibhuti Bhusana'
'Sharma, Nagendra K.'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  26.00   0.50    0.83    --  -38.50  94.00 -67.00  194
  2  ω     -4.00  82.00   0.50    0.83    --   49.31 -94.00-178.00  172
  3  ω    101.00 175.00   0.50    3.00    --  106.38  94.00 -67.00  148
  4  ω     38.00 109.00   0.50    3.00    --  106.38 -94.00-178.00  142
  5  ω   -105.00 -35.00   0.50    0.83    --  -38.50 -37.00  30.00  140
  6  ω    -17.00  53.00   0.50    0.83    --   49.31 -37.00 -90.00  140
  7  ω     46.00 116.00   0.50    0.83    --   49.31  37.00-180.00  140
  8  ω     46.00 116.00   0.50    0.83    --   49.31  37.00 -60.00  140
  9  ω     94.00 171.00   0.50    3.00    --  106.38 125.00-120.00  154
 10  ω    102.00 171.00   0.50    3.00    --  106.38  45.00-180.00  138
 11  ω     38.00 110.00   0.50    3.00    --  106.38 -30.00-120.00  144
 12  ω    103.00 175.00   0.50    3.00    --  106.38  30.00 120.00  144
 13  ω     44.00 120.00   0.50    3.00    --  106.38 -61.00 -60.00  152
 14  ω     38.00 110.00   0.50    3.00    --  106.38 -30.00  90.00  144
 15  ω     42.00 111.00   0.50    3.00    --  106.38 -45.00 150.00  138
 16  ω    103.00 169.00   0.50    3.00    --  106.38  30.00  60.00  132
 17  ω    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       'ω 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/[σ²(Fo²)+(0.1895P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
O2 O 0.3905(2) 0.22021(19) 0.3690(3) 0.0737(8) Uani 1 d . . .
O1 O 0.6189(2) 0.1253(2) 0.1401(3) 0.0762(8) Uani 1 d . . .
O4 O 0.0846(2) 0.4795(2) 0.3632(3) 0.0779(8) Uani 1 d . . .
N1 N 0.5324(2) 0.3009(2) 0.2249(3) 0.0633(8) Uani 1 d . . .
H1 H 0.5187 0.2300 0.2378 0.076 Uiso 1 calc . . R
N2 N 0.3257(2) 0.3945(2) 0.4036(3) 0.0657(8) Uani 1 d . . .
H2 H 0.3268 0.4664 0.3811 0.079 Uiso 1 calc . . R
O3 O 0.0534(2) 0.3633(3) 0.1488(3) 0.0939(10) Uani 1 d . . .
C1 C 0.6117(2) 0.3236(3) 0.1574(4) 0.0559(8) Uani 1 d . . .
C9 C 0.3912(2) 0.3245(3) 0.3544(4) 0.0598(9) Uani 1 d . . .
C8 C 0.4690(2) 0.3842(3) 0.2769(4) 0.0626(8) Uani 1 d . . .
H8A H 0.4376 0.4292 0.1842 0.075 Uiso 1 calc . . R
H8B H 0.5070 0.4357 0.3554 0.075 Uiso 1 calc . . R
C2 C 0.6589(3) 0.2178(3) 0.1138(4) 0.0629(9) Uani 1 d . . .
C7 C 0.6385(3) 0.4360(3) 0.1328(4) 0.0644(9) Uani 1 d . . .
H7 H 0.5971 0.4914 0.1638 0.077 Uiso 1 calc . . R
C12 C 0.0965(2) 0.3823(3) 0.2852(4) 0.0647(9) Uani 1 d . . .
C10 C 0.2532(3) 0.3517(3) 0.4940(4) 0.0690(9) Uani 1 d . . .
H10A H 0.2323 0.4141 0.5567 0.083 Uiso 1 calc . . R
H10B H 0.2836 0.2940 0.5705 0.083 Uiso 1 calc . . R
C11 C 0.1634(3) 0.3000(3) 0.3873(4) 0.0695(9) Uani 1 d . . .
H11A H 0.1853 0.2440 0.3157 0.083 Uiso 1 calc . . R
H11B H 0.1259 0.2593 0.4571 0.083 Uiso 1 calc . . R
C6 C 0.7168(3) 0.4786(3) 0.0697(4) 0.0728(10) Uani 1 d . . .
H6 H 0.7194 0.5581 0.0637 0.087 Uiso 1 calc . . R
C3 C 0.7470(3) 0.2177(3) 0.0486(5) 0.0718(10) Uani 1 d . . .
H3 H 0.7705 0.1447 0.0321 0.086 Uiso 1 calc . . R
C5 C 0.7922(3) 0.4220(4) 0.0138(5) 0.0822(11) Uani 1 d . . .
H5 H 0.8394 0.4674 -0.0216 0.099 Uiso 1 calc . . R
C4 C 0.8041(3) 0.3045(4) 0.0056(5) 0.0798(11) Uani 1 d . . .
H4 H 0.8590 0.2809 -0.0354 0.096 Uiso 1 calc . . R
C13 C 0.0143(4) 0.5608(4) 0.2807(6) 0.0933(13) Uani 1 d . . .
H13A H 0.0288 0.5770 0.1745 0.140 Uiso 1 calc . . GR
H13B H 0.0180 0.6304 0.3430 0.140 Uiso 1 calc . . GR
H13C H -0.0506 0.5293 0.2696 0.140 Uiso 1 calc . . GR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 O4 C13 117.4(3) . . ?
C1 N1 H1 117.1 . . ?
C1 N1 C8 125.8(3) . . ?
C8 N1 H1 117.1 . . ?
C9 N2 H2 119.4 . . ?
C9 N2 C10 121.3(3) . . ?
C10 N2 H2 119.4 . . ?
N1 C1 C2 111.7(3) . . ?
N1 C1 C7 120.4(3) . . ?
C7 C1 C2 127.8(3) . . ?
O2 C9 N2 124.0(3) . . ?
O2 C9 C8 121.1(3) . . ?
N2 C9 C8 114.9(3) . . ?
N1 C8 C9 109.8(3) . . ?
N1 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O1 C2 C1 116.8(3) . . ?
O1 C2 C3 120.2(3) . . ?
C3 C2 C1 123.0(3) . . ?
C1 C7 H7 114.9 . . ?
C6 C7 C1 130.2(4) . . ?
C6 C7 H7 114.9 . . ?
O4 C12 C11 112.9(3) . . ?
O3 C12 O4 122.3(3) . . ?
O3 C12 C11 124.8(4) . . ?
N2 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
N2 C10 C11 113.8(3) . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
C12 C11 C10 115.9(3) . . ?
C12 C11 H11A 108.3 . . ?
C12 C11 H11B 108.3 . . ?
C10 C11 H11A 108.3 . . ?
C10 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C7 C6 H6 114.8 . . ?
C7 C6 C5 130.3(4) . . ?
C5 C6 H6 114.8 . . ?
C2 C3 H3 113.8 . . ?
C4 C3 C2 132.3(4) . . ?
C4 C3 H3 113.8 . . ?
C6 C5 H5 116.8 . . ?
C4 C5 C6 126.4(4) . . ?
C4 C5 H5 116.8 . . ?
C3 C4 C5 129.7(4) . . ?
C3 C4 H4 115.1 . . ?
C5 C4 H4 115.1 . . ?
O4 C13 H13A 109.5 . . ?
O4 C13 H13B 109.5 . . ?
O4 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C9 1.223(4) . ?
O1 C2 1.250(4) . ?
O4 C12 1.331(4) . ?
O4 C13 1.443(5) . ?
N1 H1 0.8600 . ?
N1 C1 1.347(5) . ?
N1 C8 1.429(4) . ?
N2 H2 0.8600 . ?
N2 C9 1.338(4) . ?
N2 C10 1.449(4) . ?
O3 C12 1.206(4) . ?
C1 C2 1.473(5) . ?
C1 C7 1.389(4) . ?
C9 C8 1.521(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 C3 1.422(6) . ?
C7 H7 0.9300 . ?
C7 C6 1.380(5) . ?
C12 C11 1.490(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.517(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C6 H6 0.9300 . ?
C6 C5 1.384(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.372(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.384(6) . ?
C4 H4 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
