Polarization-dependent second harmonic generation in peptide crystals: effects of molecular packing.
Nandi, Sujay Kumar; Roy, Samrat; Pal, Bipul; Haldar, Debasish; Physical chemistry chemical physics : PCCP 25 (2023) 5849–5856; doi:10.1039/d2cp05462k

data_7246213
_publ_section_title
;
 Polarization-dependent second harmonic generation in peptide crystals:
 effects of molecular packing.
;
_journal_issue                   7
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              5849
_journal_page_last               5856
_journal_paper_doi               10.1039/d2cp05462k
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration s
_chemical_formula_moiety         'C17 H18 N2 O7'
_chemical_formula_sum            'C17 H18 N2 O7'
_chemical_formula_weight         362.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-05-26 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.252(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   58.3070(16)
_cell_length_b                   6.79340(10)
_cell_length_c                   9.0204(2)
_cell_measurement_reflns_used    5629
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.1130
_cell_measurement_theta_min      4.8720
_cell_volume                     3570.25(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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    -30.00  28.00   0.50    2.00    --  -41.21  25.00   0.00  116
  2  \w    -17.00  29.00   0.50    2.00    --  -41.21  12.00 -60.00   92
  3  \w    -41.00 -15.00   0.50   15.00    --  -82.50  42.00-120.00   52
  4  \w    -40.00 -15.00   0.50   15.00    --  -82.50  42.00 -90.00   50
  5  \w    -47.00 -15.00   0.50   15.00    --  -82.50  42.00-180.00   64
  6  \w    -77.00 -52.00   0.50   15.00    --  -82.50 129.00-138.00   50
  7  \w    -88.00 -41.00   0.50    2.00    --  -41.21 129.00-138.00   94
  8  \w    -87.00 -48.00   0.50    2.00    --  -41.21 141.00  33.00   78
  9  \w    -59.00 -30.00   0.50   15.00    --  -82.50 141.00  33.00   58
 10  \w    -45.00 -18.00   0.50   15.00    --  -82.50  42.00  60.00   54
 11  \w    -57.00 -27.00   0.50    2.00    --  -41.21 -25.00   0.00   60
 12  \w    -62.00 -36.00   0.50    2.00    --  -41.21 -77.00   0.00   52
 13  \w    -88.00 -62.00   0.50   15.00    --  -82.50-141.00 -23.00   52
 14  \w    -91.00 -65.00   0.50    2.00    --  -41.21-141.00 -23.00   52
 15  \w     65.00 107.00   0.50    2.00    --   41.21  64.00  90.00   84
 16  \w    116.00 160.00   0.50   15.00    --   96.67 141.00  33.00   88
 17  \w    129.00 154.00   0.50   15.00    --   96.67 117.00  30.00   50
 18  \w    113.00 153.00   0.50   15.00    --   96.67  96.00 -30.00   80
 19  \w    102.00 128.00   0.50   15.00    --   96.67 129.00-138.00   52
 20  \w    120.00 146.00   0.50   15.00    --   96.67 117.00-150.00   52
 21  \w    105.00 161.00   0.50   15.00    --   96.67  96.00-150.00  112
 22  \w    101.00 143.00   0.50   15.00    --   96.67 117.00 -60.00   84
 23  \w    101.00 127.00   0.50   15.00    --   96.67 117.00   0.00   52
 24  \w     86.00 151.00   0.50   15.00    --   96.67  77.00 -60.00  130
 25  \w     85.00 163.00   0.50   15.00    --   96.67  33.00  60.00  156
 26  \w    133.00 159.00   0.50   15.00    --   96.67  68.00 120.00   52
 27  \w    111.00 137.00   0.50   15.00    --   96.67 117.00 120.00   52
 28  \w     79.00 129.00   0.50   15.00    --   96.67  68.00 120.00  100
 29  \w     82.00 108.00   0.50   15.00    --   96.67 145.00  60.00   52
 30  \w     79.00 163.00   0.50   15.00    --   96.67  59.00   0.00  168
 31  \w     79.00 159.00   0.50   15.00    --   96.67  50.00 -90.00  160
 32  \w     35.00  69.00   0.50    2.00    --   41.21 -92.00-180.00   68
 33  \w     27.00  54.00   0.50    2.00    --   41.21 -50.00 -60.00   54
 34  \w     14.00  55.00   0.50    2.00    --   41.21 -50.00   0.00   82
 35  \w     31.00  57.00   0.50   15.00    --   96.67 -50.00   0.00   52
 36  \w     31.00  57.00   0.50   15.00    --   96.67 -50.00  30.00   52
 37  \w     31.00 104.00   0.50   15.00    --   96.67 -77.00   0.00  146
 38  \w     97.00 122.00   0.50   15.00    --   96.67-141.00 -23.00   50
 39  \w     87.00 127.00   0.50   15.00    --   96.67-145.00 -60.00   80
 40  \w     92.00 118.00   0.50   15.00    --   96.67-145.00-120.00   52
 41  \w     50.00  76.00   0.50   15.00    --   96.67-145.00 -60.00   52
 42  \w     30.00  93.00   0.50   15.00    --   96.67-117.00 -30.00  126
 43  \w     75.00 127.00   0.50   15.00    --   96.67-145.00  60.00  104
 44  \w     74.00 120.00   0.50   15.00    --   96.67-145.00 120.00   92
 45  \w     66.00  91.00   0.50    2.00    --   41.21-129.00 148.00   50
 46  \w     53.00 116.00   0.50   15.00    --   96.67-129.00 148.00  126
 47  \w     37.00  72.00   0.50   15.00    --   96.67 -68.00 120.00   70
 48  \w     39.00  75.00   0.50   15.00    --   96.67 -68.00 150.00   72
 49  \w     31.00  56.00   0.50   15.00    --   96.67 -50.00 120.00   50
 50  \w     29.00 115.00   0.50   15.00    --   96.67 -87.00 120.00  172
 51  \w     44.00  70.00   0.50    2.00    --   41.21-141.00 -23.00   52
 52  \w     32.00  68.00   0.50   15.00    --   96.67 -68.00   0.00   72
 53  \w     31.00  57.00   0.50   15.00    --   96.67 -50.00 -60.00   52
 54  \w     25.00 102.00   0.50   15.00    --   96.67 -96.00 -30.00  154
 55  \w     30.00  80.00   0.50   15.00    --   96.67 -68.00-150.00  100
 56  \w     36.00  71.00   0.50   15.00    --   96.67 -68.00-180.00   70
 57  \w     29.00  54.00   0.50   15.00    --   96.67 -59.00-150.00   50
 58  \w     -6.00  22.00   0.50    2.00    --   41.21 -50.00 -60.00   56
 59  \w     -8.00  29.00   0.50    2.00    --   41.21 -25.00-150.00   74
 60  \w    -17.00  29.00   0.50    2.00    --   41.21 -92.00-180.00   92
 61  \w     -1.00  24.00   0.50    2.00    --   41.21 -12.00-120.00   50
 62  \w    -32.00   2.00   0.50    2.00    --   41.21 -12.00-180.00   68
 63  \w     28.00 104.00   0.50    2.00    --   41.21  77.00-180.00  152
 64  \w    -24.00  10.00   0.50    2.00    --   41.21 -50.00   0.00   68
 65  \w     -9.00  18.00   0.50    2.00    --   41.21 -12.00  90.00   54
 66  \w     18.00  44.00   0.50    2.00    --   41.21  64.00  90.00   52
 67  \w    -97.00 -72.00   0.50    2.00    --  -41.21 -77.00   0.00   50
 68  \w   -103.00 -65.00   0.50    2.00    --  -41.21 -25.00   0.00   76
 69  \w   -120.00 -94.00   0.50   15.00    --  -82.50-129.00 148.00   52
 70  \w   -156.00 -99.00   0.50   15.00    --  -82.50 -96.00 -90.00  114
 71  \w   -149.00 -86.00   0.50   15.00    --  -82.50 -87.00-150.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0262746000
_diffrn_orient_matrix_UB_12      -0.0091288000
_diffrn_orient_matrix_UB_13      0.0119269000
_diffrn_orient_matrix_UB_21      -0.0027766000
_diffrn_orient_matrix_UB_22      0.1618464000
_diffrn_orient_matrix_UB_23      -0.1189141000
_diffrn_orient_matrix_UB_31      -0.0013167000
_diffrn_orient_matrix_UB_32      -0.1585090000
_diffrn_orient_matrix_UB_33      -0.1221390000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18281
_diffrn_reflns_point_group_measured_fraction_full 0.858
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.034
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.2478
_exptl_crystal_size_mid          0.2015
_exptl_crystal_size_min          0.1658
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 1168 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5410
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0981
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2909
_refine_ls_wR_factor_ref         0.3087
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.708
_reflns_Friedel_fraction_max     0.708
_reflns_number_gt                4253
_reflns_number_total             5410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp05462k2.cif
_cod_data_source_block           sn-couleu_1
_cod_depositor_comments
'Adding full bibliography for 7246211--7246213.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7246213
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O'
_reflns_odcompleteness_completeness 98.62
_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. Restrained distances
 C13-C15
 1.51 with sigma of 0.02
 C15-C13
 1.49 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C12) = Uanis(C14) = Uanis(C31) = Uanis(C32) = Uanis(C29) =
Uanis(C30) = Uanis(C13)
4.a Ternary CH refined with riding coordinates:
 C28(H28), C30(H30), C11(H11), C13(H13)
4.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C12(H12A,H12B)
4.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C5(H5), C24(H24), N2(H2), C7(H7), C22(H22), C2(H2A), C3(H3), C19(H19),
  C20(H20)
4.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C17(H17A,H17B,H17C), C31(H31A,H31B,H31C), C15(H15A,H15B,
 H15C), C32(H32A,H32B,H32C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              14639
_shelx_hkl_checksum              86455
_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 4.812
_oxdiff_exptl_absorpt_empirical_full_min 0.522