Solid-state behaviors of imines: colossal biaxial positive thermal expansion, motion capability, and phase transitions
Juneja, Navkiran; Zahid, Ethan; Unruh, Daniel K.; Hutchins, Kristin M.; CrystEngComm 23 (2021) 4439–4443; doi:10.1039/D1CE00706H

data_7243006
_publ_section_title
;
 Solid-state behaviors of imines: colossal biaxial positive thermal
 expansion, motion capability, and phase transitions
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              4439
_journal_page_last               4443
_journal_paper_doi               10.1039/D1CE00706H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C12 H11 N3'
_chemical_formula_sum            'C12 H11 N3'
_chemical_formula_weight         197.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-02-04
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-05-28 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.85010(6)
_cell_length_b                   7.36978(7)
_cell_length_c                   23.4676(2)
_cell_measurement_reflns_used    12345
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      77.216
_cell_measurement_theta_min      3.743
_cell_volume                     1011.781(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      229.95
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19324
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.377
_diffrn_reflns_theta_min         3.767
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       irregular
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.115
_refine_diff_density_min         -0.095
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 785 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_coef       0.0054(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2107
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0420P)^2^+0.0768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.659
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                2009
_reflns_number_total             2107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00706h2.cif
_cod_data_source_block           PI_230_2
_cod_depositor_comments
'Adding full bibliography for 7242993--7243020.cif.'
_cod_original_cell_volume        1011.783(16)
_cod_database_code               7243006
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 N2A-C7A = N2B-C7B
 1.27754 with sigma of 0.02
 C7A-C8A = C7B-C8B
 1.49168 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2A \\sim N2B \\sim C7A \\sim C7B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N3A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim N3B \\sim C8B
\\sim C9B \\sim C10B \\sim C11B \\sim C12B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(N2B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(H10B)=
 Sof(N3B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(H12B)=1-FVAR(1)
 Sof(N2A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=
 Sof(N3A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C7B(H7B), C2(H2), C3(H3), C5(H5), C6(H6), C9A(H9A), C10A(H10A),
 C11A(H11A), C12A(H12A), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B)
5.b Fitted hexagon refined as free rotating group:
 C8B(C9B,C10B,N3B,C11B,C12B)
;
_shelx_res_checksum              72912
_olex2_submission_special_instructions 'No special instructions were received'