#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:55:05 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261587 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/16/7241635.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_7241635
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         '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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -35.00   0.50    1.29    --  -38.50 -39.00 -72.00  138
  2  ω    -42.00  28.00   0.50    1.29    --  -38.50  39.00  81.00  140
  3  ω    -17.00  53.00   0.50    1.29    --   49.06 -39.00 -72.00  140
  4  ω     46.00 115.00   0.50    1.29    --   49.06  39.00  81.00  138
  5  ω     41.00 110.00   0.50    7.21    --  106.38 -39.00 -72.00  138
  6  ω    103.00 172.00   0.50    7.21    --  106.38  39.00  81.00  138
  7  ω    -42.00  28.00   0.50    1.29    --  -38.50  37.00-120.00  140
  8  ω    -42.00  28.00   0.50    1.29    --  -38.50  37.00 150.00  140
  9  ω     46.00 116.00   0.50    1.29    --   49.06  37.00-180.00  140
 10  ω    103.00 175.00   0.50    7.21    --  106.38  30.00 -30.00  144
 11  ω     42.00 122.00   0.50    7.21    --  106.38-125.00 -30.00  160
 12  ω     38.00 109.00   0.50    7.21    --  106.38 -94.00  60.00  142
 13  ω    102.00 171.00   0.50    7.21    --  106.38  45.00-150.00  138
 14  ω     83.00 171.00   0.50    7.21    --  106.38  77.00-180.00  176
 15  ω    102.00 171.00   0.50    7.21    --  106.38  45.00 -60.00  138
 16  ω     44.00 120.00   0.50    7.21    --  106.38 -61.00  30.00  152
 17  ω     42.00 111.00   0.50    7.21    --  106.38 -45.00  90.00  138
 18  ω     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       'ω 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/[σ²(Fo²)+(0.0669P)²+0.1373P] where P=(Fo²+2Fc²)/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
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -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 0.44657(7) 0.3252(2) 0.55574(5) 0.0508(3) Uani 1 d . . .
O1 O 0.84425(8) 0.4116(2) 0.74443(5) 0.0563(3) Uani 1 d . . .
O4 O 0.26070(7) 0.6317(2) 0.63022(7) 0.0618(3) Uani 1 d . . .
N1 N 0.69896(7) 0.3478(2) 0.64359(6) 0.0442(3) Uani 1 d . . .
H1 H 0.7081 0.2789 0.6876 0.053 Uiso 1 calc . . R
N2 N 0.51725(8) 0.6025(2) 0.64590(6) 0.0453(3) Uani 1 d . . .
H2 H 0.5686 0.6469 0.6759 0.054 Uiso 1 calc . . R
O3 O 0.35870(8) 0.3763(3) 0.71036(7) 0.0694(3) Uani 1 d . . .
C1 C 0.76406(8) 0.5346(2) 0.62764(6) 0.0383(3) Uani 1 d . . .
C9 C 0.51968(9) 0.3988(2) 0.59709(7) 0.0401(3) Uani 1 d . . .
C7 C 0.84730(9) 0.5580(3) 0.68782(7) 0.0432(3) Uani 1 d . . .
C11 C 0.34709(10) 0.5604(3) 0.66676(7) 0.0467(3) Uani 1 d . . .
C2 C 0.74925(10) 0.6822(3) 0.56165(7) 0.0466(3) Uani 1 d . . .
H2A H 0.6916 0.6412 0.5309 0.056 Uiso 1 calc . . R
C8 C 0.61518(9) 0.2511(3) 0.59427(8) 0.0474(3) Uani 1 d . . .
H8A H 0.6058 0.0589 0.6050 0.057 Uiso 1 calc . . R
H8B H 0.6301 0.2622 0.5438 0.057 Uiso 1 calc . . R
C10 C 0.42637(10) 0.7468(3) 0.64723(9) 0.0514(3) Uani 1 d . . .
H10A H 0.4057 0.8278 0.5988 0.062 Uiso 1 calc . . R
H10B H 0.4365 0.8943 0.6833 0.062 Uiso 1 calc . . R
C6 C 0.92779(10) 0.7341(3) 0.68419(9) 0.0564(4) Uani 1 d . . .
H6 H 0.9759 0.7224 0.7253 0.068 Uiso 1 calc . . R
C3 C 0.80651(12) 0.8817(3) 0.53392(9) 0.0576(4) Uani 1 d . . .
H3 H 0.7809 0.9528 0.4878 0.069 Uiso 1 calc . . R
C5 C 0.94824(12) 0.9180(4) 0.63181(11) 0.0669(4) Uani 1 d . . .
H5 H 1.0073 1.0098 0.6434 0.080 Uiso 1 calc . . R
C4 C 0.89481(13) 0.9895(4) 0.56405(10) 0.0667(4) Uani 1 d . . .
H4 H 0.9214 1.1232 0.5365 0.080 Uiso 1 calc . . R
C12 C 0.17918(12) 0.4705(5) 0.64695(12) 0.0792(5) Uani 1 d . . .
H12A H 0.1231 0.5085 0.6110 0.119 Uiso 1 calc . . GR
H12B H 0.1652 0.5168 0.6956 0.119 Uiso 1 calc . . GR
H12C H 0.1950 0.2792 0.6454 0.119 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
C11 O4 C12 115.34(14) . . ?
C1 N1 H1 116.8 . . ?
C1 N1 C8 126.43(11) . . ?
C8 N1 H1 116.8 . . ?
C9 N2 H2 120.8 . . ?
C9 N2 C10 118.49(11) . . ?
C10 N2 H2 120.8 . . ?
N1 C1 C7 111.74(11) . . ?
N1 C1 C2 121.12(11) . . ?
C2 C1 C7 127.14(12) . . ?
O2 C9 N2 121.90(12) . . ?
O2 C9 C8 119.34(12) . . ?
N2 C9 C8 118.74(11) . . ?
O1 C7 C1 116.67(12) . . ?
O1 C7 C6 120.00(12) . . ?
C6 C7 C1 123.33(12) . . ?
O4 C11 C10 111.05(12) . . ?
O3 C11 O4 123.74(13) . . ?
O3 C11 C10 125.19(13) . . ?
C1 C2 H2A 114.7 . . ?
C1 C2 C3 130.70(13) . . ?
C3 C2 H2A 114.7 . . ?
N1 C8 C9 117.01(11) . . ?
N1 C8 H8A 108.0 . . ?
N1 C8 H8B 108.0 . . ?
C9 C8 H8A 108.0 . . ?
C9 C8 H8B 108.0 . . ?
H8A C8 H8B 107.3 . . ?
N2 C10 C11 112.14(11) . . ?
N2 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C7 C6 H6 113.9 . . ?
C5 C6 C7 132.26(14) . . ?
C5 C6 H6 113.9 . . ?
C2 C3 H3 115.0 . . ?
C4 C3 C2 130.08(15) . . ?
C4 C3 H3 115.0 . . ?
C6 C5 H5 114.9 . . ?
C6 C5 C4 130.23(15) . . ?
C4 C5 H5 114.9 . . ?
C3 C4 C5 126.22(15) . . ?
C3 C4 H4 116.9 . . ?
C5 C4 H4 116.9 . . ?
O4 C12 H12A 109.5 . . ?
O4 C12 H12B 109.5 . . ?
O4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 1.2265(15) . ?
O1 C7 1.2583(16) . ?
O4 C11 1.3303(17) . ?
O4 C12 1.443(2) . ?
N1 H1 0.8600 . ?
N1 C1 1.3421(16) . ?
N1 C8 1.4416(16) . ?
N2 H2 0.8600 . ?
N2 C9 1.3357(17) . ?
N2 C10 1.4455(17) . ?
O3 C11 1.1934(17) . ?
C1 C7 1.4774(16) . ?
C1 C2 1.3896(17) . ?
C9 C8 1.5138(18) . ?
C7 C6 1.416(2) . ?
C11 C10 1.5065(19) . ?
C2 H2A 0.9300 . ?
C2 C3 1.394(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C6 H6 0.9300 . ?
C6 C5 1.367(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.372(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.389(3) . ?
C4 H4 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
