A crystal-structural study of Pauling–Corey rippled sheets
Kuhn, Ariel J.; Ehlke, Beatriz; Johnstone, Timothy C.; Oliver, Scott R. J.; Raskatov, Jevgenij A.; Chemical Science 13 (2022) 671–680; doi:10.1039/D1SC05731F

data_1565601
_publ_section_title
;
 A crystal-structural study of Pauling--Corey rippled sheets
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              671
_journal_page_last               680
_journal_paper_doi               10.1039/D1SC05731F
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C27 H29 N3 O4'
_chemical_formula_sum            'C27 H29 N3 O4'
_chemical_formula_weight         459.53
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-28
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.483(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3563(5)
_cell_length_b                   16.7472(6)
_cell_length_c                   12.6545(6)
_cell_measurement_reflns_used    11046
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      76.0240
_cell_measurement_theta_min      3.9510
_cell_volume                     2358.54(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -77.00  24.00   0.50    9.66    --  -48.41  97.00 -62.00  202
  2  \w      7.00  69.00   0.50    9.66    --   48.41 -97.00-170.00  124
  3  \w   -135.00-107.00   0.50   38.63    --  -84.25 -97.00-170.00   56
  4  \w    -69.00 -43.00   0.50   38.63    --  -84.25  97.00 -62.00   52
  5  \w     58.00  85.00   0.50   38.63    --  105.75 -97.00-170.00   54
  6  \w    119.00 174.00   0.50   38.63    --  105.75  97.00 -62.00  110
  7  \w    -54.00 -11.00   0.50    9.66    --  -48.41  57.00 -90.00   86
  8  \w     -7.00  24.00   0.50    9.66    --  -48.41  57.00 -90.00   62
  9  \w   -116.00 -84.00   0.50    9.66    --  -48.41 -57.00-150.00   64
 10  \w   -115.00 -87.00   0.50    9.66    --  -48.41-125.00 -90.00   56
 11  \w   -118.00 -87.00   0.50    9.66    --  -48.41-125.00   0.00   62
 12  \w   -116.00 -86.00   0.50    9.66    --  -48.41 -57.00   0.00   60
 13  \w     82.00 115.00   0.50    9.66    --   48.41  57.00 -60.00   66
 14  \w     86.00 119.00   0.50    9.66    --   48.41  57.00   0.00   66
 15  \w     84.00 119.00   0.50    9.66    --   48.41  57.00 -30.00   70
 16  \w    -42.00 -15.00   0.50   38.63    --  -84.25  38.00 150.00   54
 17  \w    -41.00 -16.00   0.50   38.63    --  -84.25  38.00-120.00   50
 18  \w    -41.00 -15.00   0.50   38.63    --  -84.25  38.00 -60.00   52
 19  \w    -41.00 -13.00   0.50   38.63    --  -84.25  38.00 120.00   56
 20  \w    -42.00 -17.00   0.50   38.63    --  -84.25  38.00 -90.00   50
 21  \w   -137.00-110.00   0.50   38.63    --  -84.25 -99.00 120.00   54
 22  \w   -145.00-101.00   0.50   38.63    --  -84.25 -77.00   0.00   88
 23  \w     35.00  60.00   0.50   38.63    --  105.75 -57.00  90.00   50
 24  \w     35.00  66.00   0.50   38.63    --  105.75 -57.00 120.00   62
 25  \w     35.00  61.00   0.50   38.63    --  105.75 -99.00  90.00   52
 26  \w     99.00 176.00   0.50   38.63    --  105.75  38.00   0.00  154
 27  \w    101.00 173.00   0.50   38.63    --  105.75  38.00 -60.00  144
 28  \w     36.00 107.00   0.50   38.63    --  105.75-125.00  90.00  142
 29  \w     38.00  66.00   0.50   38.63    --  105.75 -57.00 -90.00   56
 30  \w     37.00  63.00   0.50   38.63    --  105.75 -57.00   0.00   52
 31  \w     79.00 106.00   0.50   38.63    --  105.75 -77.00-180.00   54
 32  \w     69.00 104.00   0.50   38.63    --  105.75 -99.00 -90.00   70
 33  \w     97.00 172.00   0.50   38.63    --  105.75  57.00  60.00  150
 34  \w     35.00  60.00   0.50   38.63    --  105.75 -77.00-180.00   50
 35  \w     38.00  64.00   0.50   38.63    --  105.75 -99.00 -60.00   52
 36  \w     78.00 106.00   0.50   38.63    --  105.75 -99.00 -60.00   56
 37  \w     41.00  66.00   0.50   38.63    --  105.75 -57.00  60.00   50
 38  \w     40.00  67.00   0.50   38.63    --  105.75 -99.00 -90.00   54
 39  \w     78.00 106.00   0.50   38.63    --  105.75 -99.00 150.00   56
 40  \w     34.00  68.00   0.50   38.63    --  105.75 -99.00 150.00   68
 41  \w     43.00 110.00   0.50   38.63    --  105.75-125.00  60.00  134
 42  \w    124.00 170.00   0.50   38.63    --  105.75  57.00   0.00   92
 43  \w     34.00  59.00   0.50   38.63    --  105.75 -57.00 -60.00   50
 44  \w     38.00 106.00   0.50   38.63    --  105.75 -99.00-150.00  136
 45  \w     34.00  66.00   0.50   38.63    --  105.75 -57.00-150.00   64
 46  \w     70.00 106.00   0.50   38.63    --  105.75 -99.00  90.00   72
 47  \w     39.00  66.00   0.50   38.63    --  105.75 -57.00 -30.00   54
 48  \w     79.00 104.00   0.50   38.63    --  105.75 -77.00  60.00   50
 49  \w     99.00 168.00   0.50   38.63    --  105.75  38.00  30.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1020083000
_diffrn_orient_matrix_UB_12      0.0379729000
_diffrn_orient_matrix_UB_13      0.0834681000
_diffrn_orient_matrix_UB_21      -0.0119451000
_diffrn_orient_matrix_UB_22      0.0776222000
_diffrn_orient_matrix_UB_23      -0.0664952000
_diffrn_orient_matrix_UB_31      -0.0926262000
_diffrn_orient_matrix_UB_32      0.0316124000
_diffrn_orient_matrix_UB_33      0.0637063000
_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  0.0500
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23314
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.064
_diffrn_reflns_theta_max         67.064
_diffrn_reflns_theta_min         4.436
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4187
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0708P)^2^+0.5612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3438
_reflns_number_total             4187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05731f2.cif
_cod_data_source_block           be_134_fff_man
_cod_depositor_comments          'Adding full bibliography for 1565601.cif.'
_cod_database_code               1565601
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H29 N3 O4'
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.932
_reflns_odcompleteness_completeness 99.59
_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 N(H,H,H) groups
2. Restrained distances
 N1-H1A = N1-H1B = N1-H1C
 0.91 with sigma of 0.02
 N2-H2 = N3-H3
 0.88 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C12(H12), C22(H22), C32(H32)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C23(H23A,H23B), C33(H33A,H33B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
;
_shelx_res_checksum              1617
_shelx_hkl_checksum              85960
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.915
_oxdiff_exptl_absorpt_empirical_full_min 0.699