Structure–Thermomechanical Property Correlation in Polymorphic Molecular Crystals Probed by the Nanoindentation Technique
Su, Yuan; Bhunia, Surojit; Xu, Shuyuan; Chen, An; Reddy, C. Malla; Cai, Ting; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.1c00584

data_4003940
_publ_section_title
;
 Structure--Thermomechanical Property Correlation in Polymorphic Molecular
 Crystals Probed by the Nanoindentation Technique
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c00584
_journal_year                    2021
_chemical_formula_moiety         'C2 H3 O2, C30 H35 N2 O3'
_chemical_formula_sum            'C32 H38 N2 O5'
_chemical_formula_weight         530.64
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.3834(16)
_cell_length_b                   10.3834(16)
_cell_length_c                   44.399(6)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.328
_cell_measurement_theta_min      2.265
_cell_volume                     4145.6(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            10406
_diffrn_reflns_point_group_measured_fraction_full 0.886
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.362
_diffrn_reflns_theta_min         2.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0874 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.8999. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 1120 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.1(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4882
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.4311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.771
_reflns_Friedel_fraction_max     0.732
_reflns_number_gt                3264
_reflns_number_total             4882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c00584_si_004.cif
_cod_data_source_block           22019370298k_0m
_cod_original_cell_volume        4145.6(14)
_cod_database_code               4003940
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.083) H5(0.1) H2A(0.053) H17(0.055) H20(0.054) H29(0.058)
 H10(0.059) H30(0.055) H13(0.053) H27(0.055) H11(0.056) H26(0.053) H23A(0.081)
 H23B(0.081) H23C(0.081) H15A(0.054) H15B(0.054) H6A(0.066) H6B(0.066)
 H14(0.059) H8A(0.076) H8B(0.076) H1A(0.069) H1B(0.069) H18(0.062) H5A(0.083)
 H5B(0.083) H7A(0.071) H7B(0.071) H31A(0.106) H31B(0.106) H31C(0.106)
 H2B(0.085) H2C(0.085) H3A(0.108) H3B(0.108) H4A(0.111) H4B(0.111)
 Fixed X: H2(0.293985) H5(1.084815) H2A(1.070058) H17(0.690029) H20(1.014917)
 H29(0.217594) H10(0.920026) H30(0.379718) H13(0.428913) H27(0.545526)
 H11(0.807272) H26(0.707464) H23A(0.869626) H23B(0.79763) H23C(0.955849)
 H15A(0.455817) H15B(0.481016) H6A(1.069366) H6B(1.221138) H14(0.53886)
 H8A(0.706781) H8B(0.841916) H1A(1.105399) H1B(1.115718) H18(0.877612)
 H5A(1.199756) H5B(1.143463) H7A(0.899091) H7B(0.871765) H31A(0.607618)
 H31B(0.627522) H31C(0.507034) H2B(1.339517) H2C(1.345673) H3A(1.348958)
 H3B(1.49162) H4A(1.403746) H4B(1.418925)
 Fixed Y: H2(0.010783) H5(-0.46799) H2A(0.300289) H17(-0.438142) H20(-
 0.301906) H29(-0.328949) H10(0.118585) H30(-0.388473) H13(-0.247474)
 H27(0.092724) H11(-0.056252) H26(0.03154) H23A(-0.236227) H23B(-0.134763)
 H23C(-0.074947) H15A(-0.28144) H15B(-0.390118) H6A(0.087226) H6B(0.222126)
 H14(-0.072126) H8A(0.025608) H8B(0.004628) H1A(0.490973) H1B(0.414944) H18(-
 0.497347) H5A(0.10598) H5B(0.214125) H7A(0.15983) H7B(0.270891) H31A(0.430003)
 H31B(0.516262) H31C(0.49955) H2B(0.489725) H2C(0.620081) H3A(0.495208)
 H3B(0.549762) H4A(0.309666) H4B(0.316181)
 Fixed Z: H2(0.619727) H5(0.518043) H2A(0.406643) H17(0.491899) H20(0.574179)
 H29(0.603234) H10(0.475279) H30(0.58014) H13(0.466668) H27(0.610752)
 H11(0.513269) H26(0.587848) H23A(0.619326) H23B(0.620108) H23C(0.605984)
 H15A(0.526448) H15B(0.50614) H6A(0.384527) H6B(0.394803) H14(0.428725)
 H8A(0.389184) H8B(0.398093) H1A(0.377873) H1B(0.348251) H18(0.493331)
 H5A(0.344554) H5B(0.334481) H7A(0.355697) H7B(0.374754) H31A(0.596962)
 H31B(0.627161) H31C(0.603761) H2B(0.390731) H2C(0.371798) H3A(0.327294)
 H3B(0.347082) H4A(0.327948) H4B(0.363022)
;
_olex2_submission_special_instructions 'No special instructions were received'