Structural origins of two-dimensional elastic bending in a nonaromatic organic molecular crystal.
Lin, Jiawei; Cao, Yuechao; Liu, Yanbo; Li, Maolin; Chen, Yifu; Zhou, Jianmin; Wu, Songgu; Gong, Junbo; Chemical communications (Cambridge, England) 59 (2023) 619–622; doi:10.1039/d2cc05169a

data_7131129
_publ_section_title
;
 Structural origins of two-dimensional elastic bending in a nonaromatic
 organic molecular crystal.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              619
_journal_page_last               622
_journal_paper_doi               10.1039/d2cc05169a
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H9 N O6'
_chemical_formula_sum            'C6 H9 N O6'
_chemical_formula_weight         191.14
_chemical_name_systematic        'Isosorbide mononitrate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-18 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.86558(18)
_cell_length_b                   15.86558(18)
_cell_length_c                   6.49312(13)
_cell_measurement_reflns_used    11168
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      76.2690
_cell_measurement_theta_min      2.7730
_cell_volume                     1634.43(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_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    -96.00 -67.00   0.50    1.00    --  -47.23 -17.00 111.00   58
  2  \w     55.00  80.00   0.50    1.00    --   47.23  17.00 -79.00   50
  3  \w     23.00  86.00   0.50    1.00    --   47.23-125.00  47.00  126
  4  \w   -149.00-117.00   0.50    4.00    -- -100.00 -17.00 111.00   64
  5  \w   -147.00-122.00   0.50    4.00    -- -100.00-125.00  47.00   50
  6  \w   -104.00 -42.00   0.50    4.00    -- -100.00 110.00  42.00  124
  7  \w     90.00 124.00   0.50    4.00    --  103.33-146.00-118.00   68
  8  \w    111.00 136.00   0.50    4.00    --  103.33  17.00 -79.00   50
  9  \w    111.00 137.00   0.50    4.00    --  103.33 146.00 -68.00   52
 10  \w    121.00 156.00   0.50    4.00    --  103.33 110.00  42.00   70
 11  \w   -117.00 -33.00   0.50    1.00    --  -47.23 -57.00 -30.00  168
 12  \w     33.00  70.00   0.50    1.00    --   47.23  57.00   0.00   74
 13  \w     44.00  69.00   0.50    1.00    --   47.23  19.00   0.00   50
 14  \w     29.00  56.00   0.50    1.00    --   47.23  77.00  30.00   54
 15  \w     41.00  67.00   0.50    1.00    --   47.23  37.00   0.00   52
 16  \w   -116.00 -82.00   0.50    4.00    -- -100.00 -69.00  -7.91   68
 17  \w   -167.00 -82.00   0.50    4.00    -- -100.00 -68.00  13.99  170
 18  \w   -105.00 -80.00   0.50    4.00    -- -100.00 -74.00   5.05   50
 19  \w   -172.00 -82.00   0.50    4.00    -- -100.00 -68.00   8.48  180
 20  \w   -106.00 -80.00   0.50    4.00    -- -100.00 -74.00  33.48   52
 21  \w   -105.00 -79.00   0.50    4.00    -- -100.00 -77.00  30.00   52
 22  \w   -132.00 -82.00   0.50    4.00    -- -100.00 -67.00  30.65  100
 23  \w   -113.00 -80.00   0.50    4.00    -- -100.00 -77.00  60.00   66
 24  \w   -107.00 -82.00   0.50    4.00    -- -100.00 -73.00  10.99   50
 25  \w   -112.00 -81.00   0.50    4.00    -- -100.00 -74.00  47.96   62
 26  \w   -172.00 -80.00   0.50    4.00    -- -100.00 -81.00  78.61  184
 27  \w   -103.00 -78.00   0.50    4.00    -- -100.00 -77.00   0.00   50
 28  \w   -107.00 -82.00   0.50    4.00    -- -100.00 -70.00 -13.26   50
 29  \w   -154.00 -80.00   0.50    4.00    -- -100.00 -73.00  27.80  148
 30  \w     49.00  74.00   0.50    4.00    --  103.33 -61.00 -60.00   50
 31  \w     34.00  66.00   0.50    4.00    --  103.33 -61.00   0.00   64
 32  \w     36.00  74.00   0.50    4.00    --  103.33 -61.00  90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0948155000
_diffrn_orient_matrix_UB_12      0.0064672000
_diffrn_orient_matrix_UB_13      -0.0482077000
_diffrn_orient_matrix_UB_21      0.0077644000
_diffrn_orient_matrix_UB_22      0.0966118000
_diffrn_orient_matrix_UB_23      -0.0142819000
_diffrn_orient_matrix_UB_31      0.0191672000
_diffrn_orient_matrix_UB_32      -0.0072725000
_diffrn_orient_matrix_UB_33      -0.2320136000
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            15280
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.521
_diffrn_reflns_theta_min         2.785
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
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    1.554
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.123
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 1249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3159
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0385P)^2^+0.1723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                3034
_reflns_number_total             3159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05169a2.cif
_cod_data_source_block           IMN
_cod_depositor_comments
'Adding full bibliography for 7131129--7131130.cif.'
_cod_original_cell_volume        1634.43(5)
_cod_database_code               7131129
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C1(H1), C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C35(H35A,H35B), C15(H15A,H15B), C18(H18A,H18B)
2.c Idealised tetrahedral OH refined as rotating group:
 O33(H33)
;
_shelx_res_checksum              7122
_shelx_hkl_checksum              8710
_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 1.789
_oxdiff_exptl_absorpt_empirical_full_min 0.570