Structural Origins of Elastic and 2D Plastic Flexibility of Molecular Crystals Investigated with Two Polymorphs of Conformationally Rigid Coumarin
Zhang, Keke; Sun, Changquan Calvin; Liu, Yu; Wang, Chenguang; Shi, Peng; Xu, Jun; Wu, Songgu; Gong, Junbo; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.0c04560

data_4003856
_publ_section_title
;
 Structural Origins of Elastic and 2D Plastic Flexibility of Molecular
 Crystals Investigated with Two Polymorphs of Conformationally Rigid
 Coumarin
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c04560
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H6 O2'
_chemical_formula_sum            'C9 H6 O2'
_chemical_formula_weight         146.14
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-26
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.608(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.87010(10)
_cell_length_b                   15.2836(5)
_cell_length_c                   5.8211(2)
_cell_measurement_reflns_used    1528
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      76.4580
_cell_measurement_theta_min      5.7630
_cell_volume                     343.630(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.943
_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    -74.00  27.00   0.50    0.05    --  -46.12  87.00 166.00  202
  2  \w    -26.00  75.00   0.50    0.05    --   46.12 -87.00  49.00  202
  3  \w   -128.00 -27.00   0.50    0.20    -- -100.00  87.00 166.00  202
  4  \w     78.00 178.00   0.50    0.20    --  106.36  87.00 166.00  200
  5  \w     73.00 118.00   0.50    0.05    --   46.12 125.00  30.00   90
  6  \w     30.00 118.00   0.50    0.05    --   46.12  57.00  60.00  176
  7  \w   -174.00 -85.00   0.50    0.20    -- -100.00 -37.00 120.00  178
  8  \w   -173.00 -84.00   0.50    0.20    -- -100.00 -57.00  90.00  178
  9  \w   -124.00 -27.00   0.50    0.20    -- -100.00  77.00 -90.00  194
 10  \w   -173.00 -84.00   0.50    0.20    -- -100.00 -57.00 120.00  178
 11  \w     34.00 110.00   0.50    0.20    --  106.36 -99.00   0.00  152
 12  \w     34.00 135.00   0.50    0.20    --  106.36 -87.00  49.00  202
 13  \w     30.00 118.00   0.50    0.05    --   46.12  57.00 -60.00  176
 14  \w     23.00 118.00   0.50    0.05    --   46.12  77.00 -30.00  190
 15  \w     30.00 118.00   0.50    0.05    --   46.12  57.00-180.00  176
 16  \w     91.00 150.00   0.50    0.20    --  106.36  19.00 -90.00  118
;
_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      -0.3807684000
_diffrn_orient_matrix_UB_12      -0.0281295000
_diffrn_orient_matrix_UB_13      0.0126480000
_diffrn_orient_matrix_UB_21      -0.1188338000
_diffrn_orient_matrix_UB_22      0.0859403000
_diffrn_orient_matrix_UB_23      -0.1184900000
_diffrn_orient_matrix_UB_31      0.0113218000
_diffrn_orient_matrix_UB_32      -0.0445399000
_diffrn_orient_matrix_UB_33      -0.2367403000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3334
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.775
_diffrn_reflns_theta_min         5.790
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
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    1.412
_exptl_crystal_description       plate
_exptl_crystal_F_000             152
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.121
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 399 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1186
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0493P)^2^+0.0293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.678
_reflns_Friedel_fraction_full    0.767
_reflns_Friedel_fraction_max     0.689
_reflns_number_gt                1060
_reflns_number_total             1186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c04560_si_008.cif
_cod_data_source_block           031885_zkkxds_ra
_cod_database_code               4003856
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.937
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C2(H2), C7(H7), C6(H6), C8(H8)
;
_shelx_res_checksum              18187
_shelx_hkl_checksum              29821
_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.697