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_4003857
_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      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-03
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5258(15)
_cell_length_b                   5.6690(4)
_cell_length_c                   7.9119(6)
_cell_measurement_reflns_used    1363
_cell_measurement_temperature    303.20(10)
_cell_measurement_theta_max      76.3590
_cell_measurement_theta_min      5.6680
_cell_volume                     696.37(10)
_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      air
_diffrn_ambient_temperature      303.20(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.918
_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    -22.00  59.00   0.50    0.08    --   45.12 -56.00-154.00  162
  2  \w     31.00 118.00   0.50    0.08    --   45.12  56.00 -12.00  174
  3  \w   -116.00 -79.00   0.50    0.30    -- -100.00  65.00 146.00   74
  4  \w   -111.00 -39.00   0.50    0.30    -- -100.00 116.00-138.00  144
  5  \w     95.00 166.00   0.50    0.30    --  107.61  56.00 -12.00  142
  6  \w    -92.00 -65.00   0.50    0.08    --  -45.12 125.00-180.00   54
  7  \w     93.00 118.00   0.50    0.08    --   45.12 125.00-150.00   50
  8  \w   -106.00 -71.00   0.50    0.30    -- -100.00  37.00-180.00   70
  9  \w   -117.00 -79.00   0.50    0.30    -- -100.00-125.00-180.00   76
 10  \w   -171.00-129.00   0.50    0.30    -- -100.00-125.00-180.00   84
 11  \w    -68.00 -35.00   0.50    0.30    -- -100.00  37.00-180.00   66
 12  \w     96.00 162.00   0.50    0.30    --  107.61  37.00  30.00  132
 13  \w     42.00 116.00   0.50    0.30    --  107.61-125.00-120.00  148
 14  \w     54.00 109.00   0.50    0.30    --  107.61 -99.00  30.00  110
;
_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      0.2681953000
_diffrn_orient_matrix_UB_12      -0.0085633000
_diffrn_orient_matrix_UB_13      -0.0274135000
_diffrn_orient_matrix_UB_21      -0.0130456000
_diffrn_orient_matrix_UB_22      0.0663718000
_diffrn_orient_matrix_UB_23      -0.1442825000
_diffrn_orient_matrix_UB_31      0.0430322000
_diffrn_orient_matrix_UB_32      0.0731222000
_diffrn_orient_matrix_UB_33      0.1279495000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2850
_diffrn_reflns_point_group_measured_fraction_full 0.755
_diffrn_reflns_point_group_measured_fraction_max 0.701
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.115
_diffrn_reflns_theta_min         5.699
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73178
_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            colorless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.5(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1032
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1998
_reflns_Friedel_coverage         0.418
_reflns_Friedel_fraction_full    0.499
_reflns_Friedel_fraction_max     0.448
_reflns_number_gt                935
_reflns_number_total             1032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c04560_si_006.cif
_cod_data_source_block           032328_zkkform1bentroom_rb
_cod_database_code               4003857
_shelx_shelxl_version_number     2018/1
_reflns_odcompleteness_completeness 95.97
_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), C2(H2), C6(H6), C7(H7), C9(H9), C8(H8)
;
_shelx_res_checksum              13794
_shelx_hkl_checksum              6280
_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 1.626
_oxdiff_exptl_absorpt_empirical_full_min 0.378