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_4003927
_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         'C30 H35 N2 O3, C2 H3 O2'
_chemical_formula_sum            'C32 H38 N2 O5'
_chemical_formula_weight         530.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 104.8630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7099(4)
_cell_length_b                   14.7709(5)
_cell_length_c                   15.4936(5)
_cell_measurement_reflns_used    9357
_cell_measurement_temperature    269
_cell_measurement_theta_max      26.899
_cell_measurement_theta_min      2.312
_cell_volume                     2811.40(16)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      269.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34259
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.311
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1154 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.9264. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+1.3860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4332
_reflns_number_total             6415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c00584_si_003.cif
_cod_data_source_block           22019278269k_0m
_cod_database_code               4003927
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: H28A(0.75) H28B(0.75) H28C(0.25) H28D(0.25) C29(0.75) H29A(0.75)
 H29B(0.75) H30A(0.75) H30B(0.75) H30C(0.25) H30D(0.25) C0AA(0.25) H0AA(0.25)
 H0AB(0.25)
5.a Ternary CH refined with riding coordinates:
 N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C18(H18A,H18B), C26(H26A,H26B), C32(H32A,H32B), C27(H27A,
 H27B), C28(H28A,H28B), C28(H28C,H28D), C31(H31A,H31B), C29(H29A,H29B),
 C30(H30A,H30B), C30(H30C,H30D), C0AA(H0AA,H0AB)
5.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C3(H3), C2(H2A), C20(H20), C5(H5), C6(H6), C24(H24), C11(H11),
 C14(H14), C23(H23), C13(H13)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C9(H9A,H9B,H9C)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'