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_7246211
_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         'C20 H16 N2 O7'
_chemical_formula_sum            'C20 H16 N2 O7'
_chemical_formula_weight         396.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-01
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.22810(10)
_cell_length_b                   10.50560(10)
_cell_length_c                   21.3512(3)
_cell_measurement_reflns_used    7466
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.7230
_cell_measurement_theta_min      4.1280
_cell_volume                     1845.62(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -13.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.6472   57.0000 -120.0000 115

  2 omega  -13.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.6472   57.0000    0.0000 115

  3 omega    1.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.6472  -99.0000 -180.0000 81

  4 omega   27.00  145.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236   61.0000  -90.0000 118

  5 omega  100.00  153.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236  111.0000   90.0000 53

  6 omega   57.00  150.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236  178.0000  150.0000 93

  7 omega   17.00  148.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236   45.0000    0.0000 131

  8 omega  101.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   90.0000 77

  9 omega   86.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000 -150.0000 92

 10 omega  101.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  150.0000 77

 11 omega   20.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  -30.0000 93

 12 omega   68.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000    0.0000 110

 13 omega   70.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   65.0000  -30.0000 108

 14 omega  101.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  -60.0000 77

 15 omega   29.00  126.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -135.0000   -4.0000 97

 16 omega  -13.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.6472   57.0000  120.0000 115

 17 omega  -51.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.6472  -57.0000 -120.0000 115

 18 omega  -51.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.6472  -57.0000    0.0000 115

 19 omega   27.00  145.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236   61.0000 -150.0000 118

 20 omega   27.00  145.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236   61.0000   60.0000 118

 21 omega  100.00  153.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236  111.0000    0.0000 53

 22 omega   17.00  148.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236   45.0000  150.0000 131

 23 omega   20.00   46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236   81.0000  -73.6989 26

 24 omega  100.00  153.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.8236  111.0000  -90.0000 53

 25 omega   20.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  150.0000 93

 26 omega   56.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   43.0000  120.0000 122

 27 omega   33.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   32.0000 -150.0000 145

 28 omega   64.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 114

 29 omega   64.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -71.6175 114

 30 omega   56.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   43.0000  -90.0000 122

 31 omega   64.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0166042000
_diffrn_orient_matrix_UB_12      -0.1271665000
_diffrn_orient_matrix_UB_13      0.0353511000
_diffrn_orient_matrix_UB_21      0.0226850000
_diffrn_orient_matrix_UB_22      -0.0730252000
_diffrn_orient_matrix_UB_23      -0.0619977000
_diffrn_orient_matrix_UB_31      0.1850293000
_diffrn_orient_matrix_UB_32      -0.0024694000
_diffrn_orient_matrix_UB_33      0.0107498000
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14811
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        65.815
_diffrn_reflns_theta_max         65.815
_diffrn_reflns_theta_min         4.141
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.2547
_exptl_crystal_size_mid          0.2248
_exptl_crystal_size_min          0.1958
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 1128 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0473P)^2^+0.2294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                2981
_reflns_number_total             3182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp05462k2.cif
_cod_data_source_block           couphe
_cod_depositor_comments
'Adding full bibliography for 7246211--7246213.cif.'
_cod_database_code               7246211
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O'
_reflns_odcompleteness_completeness 97.20
_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 Ternary CH refined with riding coordinates:
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C5(H5), C2(H2A), C3(H3), C18(H18), C14(H14), C17(H17),
 C15(H15), C16(H16)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              33054
_shelx_hkl_checksum              7756
_olex2_date_sample_data_collection 2018-12-02
_olex2_submission_special_instructions 'No special instructions were received'