Deducing the conformational space for an octa-proline helix.
Waly, Sara M. A.; Benniston, Andrew C.; Harriman, Anthony; Chemical science 15 (2024) 1657–1671; doi:10.1039/d3sc05287g

data_1570591
_publ_section_title
;
 Deducing the conformational space for an octa-proline helix.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1657
_journal_page_last               1671
_journal_paper_doi               10.1039/d3sc05287g
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C31 H33 N3 O4'
_chemical_formula_sum            'C31 H33 N3 O4'
_chemical_formula_weight         511.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-22 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.498(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3503(2)
_cell_length_b                   8.7745(2)
_cell_length_c                   14.9164(3)
_cell_measurement_reflns_used    10914
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      77.4690
_cell_measurement_theta_min      3.0460
_cell_volume                     1311.55(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_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     70.00  96.00   0.50    1.64    --   48.76  28.00   8.00   52
  2  \w    -17.00   9.00   0.50    1.64    --   48.76 -28.00-153.00   52
  3  \w   -126.00 -26.00   0.50    1.64    --  -49.76 -28.00-153.00  200
  4  \w     -2.00  28.00   0.50    1.64    --  -49.76  28.00   8.00   60
  5  \w    -31.00  -6.00   0.50    1.64    --  -49.76  28.00   8.00   50
  6  \w   -105.00 -70.00   0.50    1.64    --  -92.01 -28.00-153.00   70
  7  \w     76.00 118.00   0.50    1.64    --   96.11  28.00   8.00   84
  8  \w     24.00  63.00   0.50    1.64    --   48.76  77.00  30.00   78
  9  \w    -30.00  27.00   0.50    1.64    --   48.76 -19.00  60.00  114
 10  \w     22.00  60.00   0.50    1.64    --   48.76  77.00  90.00   76
 11  \w    -84.00 -33.00   0.50    1.64    --  -49.76 -38.00 120.00  102
 12  \w     38.00  68.00   0.50    1.64    --   62.00  76.00 118.06   60
 13  \w    -83.00 -51.00   0.50    1.64    --  -62.00 -74.00  55.98   64
 14  \w    -78.00 -52.00   0.50    1.64    --  -74.00 -69.00 126.62   52
 15  \w    -85.00 -60.00   0.50    1.64    --  -82.00 -65.00 128.60   50
 16  \w    -87.00 -61.00   0.50    1.64    --  -86.00 -74.00 104.75   52
 17  \w   -124.00 -98.00   0.50    1.64    --  -86.00 -74.00 104.75   52
 18  \w    -88.00 -62.00   0.50    1.64    --  -86.00 -71.00  84.11   52
 19  \w   -154.00-104.00   0.50    1.64    --  -86.00 -56.00 145.33  100
 20  \w    -87.00 -62.00   0.50    1.64    --  -86.00 -72.00 106.37   50
 21  \w   -127.00 -66.00   0.50    1.64    --  -90.00 -72.00  82.80  122
 22  \w    -90.00 -65.00   0.50    1.64    --  -90.00 -73.00  75.05   50
 23  \w   -158.00-132.00   0.50    1.64    --  -90.00 -73.00  75.05   52
 24  \w   -110.00 -71.00   0.50    1.64    --  -92.01 -77.00-180.00   78
 25  \w   -159.00 -70.00   0.50    1.64    --  -92.01 -77.00  60.00  178
 26  \w    -85.00 -30.00   0.50    1.64    --  -92.01 125.00 120.00  110
 27  \w   -159.00 -68.00   0.50    1.64    --  -94.00 -77.00 133.88  182
 28  \w     19.00  50.00   0.50    1.64    --   96.11 -45.00 -30.00   62
 29  \w     23.00  49.00   0.50    1.64    --   96.11 -45.00-150.00   52
 30  \w     18.00  47.00   0.50    1.64    --   96.11 -45.00  60.00   58
 31  \w     26.00  51.00   0.50    1.64    --   96.11 -45.00  90.00   50
 32  \w     81.00 111.00   0.50    1.64    --   96.11-125.00-180.00   60
 33  \w     24.00  55.00   0.50    1.64    --   96.11-125.00-180.00   62
 34  \w     80.00 135.00   0.50    1.64    --   96.11  77.00 150.00  110
 35  \w     25.00  50.00   0.50    1.64    --   96.11 -45.00 -90.00   50
 36  \w     22.00  57.00   0.50    1.64    --   96.11 -61.00  30.00   70
 37  \w   -131.00 -75.00   0.50    1.64    --  -99.00 -74.00  75.49  112
 38  \w     43.00  83.00   0.50    1.64    --  108.00 -77.00 -90.00   80
 39  \w     41.00  66.00   0.50    1.64    --  108.00 -61.00-150.00   50
 40  \w     37.00  67.00   0.50    1.64    --  108.00 -61.00 120.00   60
 41  \w     39.00  71.00   0.50    1.64    --  108.00 -61.00  60.00   64
 42  \w    126.00 151.00   0.50    1.64    --  108.00  28.00   8.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0464037000
_diffrn_orient_matrix_UB_12      -0.0189745000
_diffrn_orient_matrix_UB_13      0.1058939000
_diffrn_orient_matrix_UB_21      0.1391624000
_diffrn_orient_matrix_UB_22      0.0605905000
_diffrn_orient_matrix_UB_23      -0.0015623000
_diffrn_orient_matrix_UB_31      -0.0460964000
_diffrn_orient_matrix_UB_32      0.1636498000
_diffrn_orient_matrix_UB_33      0.0128139000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15516
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.819
_diffrn_reflns_theta_min         3.060
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 1987 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(9)
_refine_ls_extinction_coef       0.0025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5086
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0430P)^2^+0.0709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                4720
_reflns_number_total             5086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05287g2.cif
_cod_data_source_block           acb220008_fa
_cod_depositor_comments          'Adding full bibliography for 1570591.cif.'
_cod_database_code               1570591
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H33 N3 O4'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.909
_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 Ternary CH refined with riding coordinates:
 C2(H2), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
 C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              67606
_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 1.616
_oxdiff_exptl_absorpt_empirical_full_min 0.538